SLUDGE BATCH 7B QUALIFICATION ACTIVITIES WITH SRS TANK FARM SLUDGE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pareizs, J.; Click, D.; Lambert, D.

2011-11-16

Waste Solidification Engineering (WSE) has requested that characterization and a radioactive demonstration of the next batch of sludge slurry - Sludge Batch 7b (SB7b) - be completed in the Shielded Cells Facility of the Savannah River National Laboratory (SRNL) via a Technical Task Request (TTR). This characterization and demonstration, or sludge batch qualification process, is required prior to transfer of the sludge from Tank 51 to the Defense Waste Processing Facility (DWPF) feed tank (Tank 40). The current WSE practice is to prepare sludge batches in Tank 51 by transferring sludge from other tanks. Discharges of nuclear materials from Hmore » Canyon are often added to Tank 51 during sludge batch preparation. The sludge is washed and transferred to Tank 40, the current DWPF feed tank. Prior to transfer of Tank 51 to Tank 40, SRNL typically simulates the Tank Farm and DWPF processes with a Tank 51 sample (referred to as the qualification sample). With the tight schedule constraints for SB7b and the potential need for caustic addition to allow for an acceptable glass processing window, the qualification for SB7b was approached differently than past batches. For SB7b, SRNL prepared a Tank 51 and a Tank 40 sample for qualification. SRNL did not receive the qualification sample from Tank 51 nor did it simulate all of the Tank Farm washing and decanting operations. Instead, SRNL prepared a Tank 51 SB7b sample from samples of Tank 7 and Tank 51, along with a wash solution to adjust the supernatant composition to the final SB7b Tank 51 Tank Farm projections. SRNL then prepared a sample to represent SB7b in Tank 40 by combining portions of the SRNL-prepared Tank 51 SB7b sample and a Tank 40 Sludge Batch 7a (SB7a) sample. The blended sample was 71% Tank 40 (SB7a) and 29% Tank 7/Tank 51 on an insoluble solids basis. This sample is referred to as the SB7b Qualification Sample. The blend represented the highest projected Tank 40 heel (as of May 25, 2011), and thus, the highest projected noble metals content for SB7b. Characterization was performed on the Tank 51 SB7b samples and SRNL performed DWPF simulations using the Tank 40 SB7b material. This report documents: (1) The preparation and characterization of the Tank 51 SB7b and Tank 40 SB7b samples. (2) The performance of a DWPF Chemical Process Cell (CPC) simulation using the SB7b Tank 40 sample. The simulation included a Sludge Receipt and Adjustment Tank (SRAT) cycle, where acid was added to the sludge to destroy nitrite and reduce mercury, and a Slurry Mix Evaporator (SME) cycle, where glass frit was added to the sludge in preparation for vitrification. The SME cycle also included replication of five canister decontamination additions and concentrations. Processing parameters were based on work with a nonradioactive simulant. (3) Vitrification of a portion of the SME product and characterization and durability testing (as measured by the Product Consistency Test (PCT)) of the resulting glass. (4) Rheology measurements of the SRAT receipt, SRAT product, and SME product. This program was controlled by a Task Technical and Quality Assurance Plan (TTQAP), and analyses were guided by an Analytical Study Plan. This work is Technical Baseline Research and Development (R&D) for the DWPF. It should be noted that much of the data in this document has been published in interoffice memoranda. The intent of this technical report is bring all of the SB7b related data together in a single permanent record and to discuss the overall aspects of SB7b processing.« less

Solvent hold tank sample results for MCU-16-1317-1318-1319: September 2016 monthly sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Jones, D. H.

Savannah River National Laboratory (SRNL) received one set of three Solvent Hold Tank (SHT) samples (MCU-16-1317-1318-1319), pulled on 09/12/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-1317-1318-1319 indicated the Isopar™L concentration is above its nominal level (102%). The extractant (MaxCalix) and the modifier (CS-7SB) are 5% and 9% below their nominal concentrations. The suppressor (TiDG) is 76% below its nominal concentration. A summary of the concentration of the relevant solvent components is shown below.

Solvent hold tank sample results for MCU-16-1363-1364-1365: November 2016 monthly sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Jones, D. H.

Savannah River National Laboratory (SRNL) received one set of three Solvent Hold Tank (SHT) samples (MCU-16-1363-1364-1365), pulled on 11/15/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-1363-1364-1365 indicated the Isopar™L concentration is at its nominal level (100%). The extractant (MaxCalix) and the modifier (CS- 7SB) are 8% and 2 % below their nominal concentrations. The suppressor (TiDG) is 7% below its nominal concentration. A summary of the concentration of the relevant solvent components is shown below.

Results From The Salt Disposition Project Next Generation Solvent Demonstration Plan

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.; Fondeur, F. F.; Taylor-Pashow, K. M.L.

2014-04-02

Strip Effluent Hold Tank (SEHT), Decontaminated Salt Solution Hold Tank (DSSHT), Caustic Wash Tank (CWT) and Solvent Hold Tank (SHT) samples were taken throughout the Next Generation Solvent (NGS) Demonstration Plan. These samples were analyzed and the results are reported. SHT: The solvent behaved as expected, with no bulk changes in the composition over time, with the exception of the TOA and TiDG. The TiDG depletion is higher than expected, and consideration must be taken on the required rate of replenishment. Monthly sampling of the SHT is warranted. If possible, additional SHT samples for TiDG analysis (only) would help SRNLmore » refine the TiDG degradation model. CWT: The CWT samples show the expected behavior in terms of bulk chemistry. The 137Cs deposited into the CWT varies somewhat, but generally appears to be lower than during operations with the BOBCalix solvent. While a few minor organic components were noted to be present in the Preliminary sample, at this time these are thought to be artifacts of the sample preparation or may be due to the preceding solvent superwash. DSSHT: The DSSHT samples show the predicted bulk chemistry, although they point towards significant dilution at the front end of the Demonstration. The 137Cs levels in the DSSHT are much lower than during the BOBCalix operations, which is the expected observation. SEHT: The SEHT samples represent the most different output of all four of the outputs from MCU. While the bulk chemistry is as expected, something is causing the pH of the SEHT to be higher than what would be predicted from a pure stream of 0.01 M boric acid. There are several possible different reasons for this, and SRNL is in the process of investigating. Other than the pH issue, the SEHT is as predicted. In summary, the NGS Demonstration Plan samples indicate that the MCU system, with the Blend Solvent, is operating as expected. The only issue of concern regards the pH of the SEHT, and SRNL is in the process of investigating this. SRNL results support the transition to routine operations.« less

Results from the interim salt disposition program macrobatch 10 tank 21H qualification samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.; Bannochie, C. J.

2017-02-23

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Macrobatch (Salt Batch) 10 for the Interim Salt Disposition Program (ISDP). This document reports characterization data on the samples of Tank 21H and fulfills the requirements of Deliverable 3 of the Technical Task Request (TTR). Further work will report the results of the Extraction-Scrub-Strip (ESS) testing (Task 5 of the TTR) using the Tank 21H material. Task 4 of the TTR (MST Strike) will not be completed for Salt Batch 10.

Results of Hg speciation testing on tank 39 and 1Q16 tank 50 samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.

2016-03-07

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team.i,ii The seventeenth shipment of samples was designated to include two Tank 39 samples and the 1Q16 Tank 50 Quarterly WAC sample. The surface Tank 39 sample was pulled at 262.1” from the tank bottom, and the depth Tank 39 sample was pulled at 95” from the tank bottom. The 1Q16 Tank 50 WAC sample was drawn from the 1-L variable depth sample received bymore » SRNL.« less

Characterization of solids deposited on the modular caustic-side solvent extraction unit (MCU) coalescer media removed in May and October 2014

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.

During routine maintenance, the coalescers utilized in the Modular Caustic-Side Solvent Extraction Unit (MCU) processing of Salt Batch 6 and a portion of Salt Batch 7 were sampled and submitted to the Savannah River National Laboratory (SRNL) for characterization, for the purpose of identifying solid phase constituents that may be accumulating in these coalescers. Specifically, two samples were received and characterized: A decontaminated salt solution (DSS) coalescer sample and a strip effluent (SE) coalescer sample. Aliquots of the samples were analyzed by XRD, Fourier Transform Infrared (FTIR) Spectroscopy, SEM, and EDS. Other aliquots of the samples were leached in acidmore » solution, and the leachates were analyzed by ICP-AES. In addition, modeling was performed to provide a basis for comparison of the analytical results.« less

EVALUATION OF ARG-1 SAMPLES PREPARED BY CESIUM CARBONATE DISSOLUTION DURING THE ISOLOK SME ACCEPTABILITY TESTING

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edwards, T.; Hera, K.; Coleman, C.

2011-12-05

Evaluation of Defense Waste Processing Facility (DWPF) Chemical Process Cell (CPC) cycle time identified several opportunities to improve the CPC processing time. The Mechanical Systems & Custom Equipment Development (MS&CED) Section of the Savannah River National Laboratory (SRNL) recently completed the evaluation of one of these opportunities - the possibility of using an Isolok sampling valve as an alternative to the Hydragard valve for taking DWPF process samples at the Slurry Mix Evaporator (SME). The use of an Isolok for SME sampling has the potential to improve operability, reduce maintenance time, and decrease CPC cycle time. The SME acceptability testingmore » for the Isolok was requested in Task Technical Request (TTR) HLW-DWPF-TTR-2010-0036 and was conducted as outlined in Task Technical and Quality Assurance Plan (TTQAP) SRNLRP-2011-00145. RW-0333P QA requirements applied to the task, and the results from the investigation were documented in SRNL-STI-2011-00693. Measurement of the chemical composition of study samples was a critical component of the SME acceptability testing of the Isolok. A sampling and analytical plan supported the investigation with the analytical plan directing that the study samples be prepared by a cesium carbonate (Cs{sub 2}CO{sub 3}) fusion dissolution method and analyzed by Inductively Coupled Plasma - Optical Emission Spectroscopy (ICP-OES). The use of the cesium carbonate preparation method for the Isolok testing provided an opportunity for an additional assessment of this dissolution method, which is being investigated as a potential replacement for the two methods (i.e., sodium peroxide fusion and mixed acid dissolution) that have been used at the DWPF for the analysis of SME samples. Earlier testing of the Cs{sub 2}CO{sub 3} method yielded promising results which led to a TTR from Savannah River Remediation, LLC (SRR) to SRNL for additional support and an associated TTQAP to direct the SRNL efforts. A technical report resulting from this work was issued that recommended that the mixed acid method be replaced by the Cs{sub 2}CO{sub 3} method for the measurement of magnesium (Mg), sodium (Na), and zirconium (Zr) with additional testing of the method by DWPF Laboratory being needed before further implementation of the Cs{sub 2}CO{sub 3} method at that laboratory. While the SME acceptability testing of the Isolok does not address any of the open issues remaining after the publication of the recommendation for the replacement of the mixed acid method by the Cs{sub 2}CO{sub 3} method (since those issues are to be addressed by the DWPF Laboratory), the Cs{sub 2}CO{sub 3} testing associated with the Isolok testing does provide additional insight into the performance of the method as conducted by SRNL. The performance is to be investigated by looking to the composition measurement data generated by the samples of a standard glass, the Analytical Reference Glass - 1 (ARG-1), that were prepared by the Cs{sub 2}CO{sub 3} method and included in the SME acceptability testing of the Isolok. The measurements of these samples were presented as part of the study results, but no statistical analysis of these measurements was conducted as part of those results. It is the purpose of this report to provide that analysis, which was supported using JMP Version 7.0.2.« less

Solvent Hold Tank Sample Results for MCU-15-129-130-131: January 2015 Monthly Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Taylor-Pashow, K. M. L.

2015-02-19

SRNL received one set of SHT samples (MCU-15-129, MCU-15-130, and MCU-15-131), pulled on 01/25/2015 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-15-129-130-131 indicated low concentrations of the suppressor (TiDG), of the extractant (MaxCalix), and of the modifier (CS-7SB) in the solvent relative to their nominal values. This analysis confirms a downward trend of these components. No impurities were found in this solvent. The laboratory will continue to monitor the quality of the solvent in particular for any new impurity or degradation of the solvent components.

Analysis of Waste Isolation Pilot Plant Samples: Integrated Summary Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Britt, Phillip F

2015-03-01

Analysis of Waste Isolation Pilot Plant Samples: Integrated Summary Report. Summaries of conclusions, analytical processes, and analytical results. Analysis of samples taken from the Waste Isolation Pilot Plant (WIPP) near Carlsbad, New Mexico in support of the WIPP Technical Assessment Team (TAT) activities to determine to the extent feasible the mechanisms and chemical reactions that may have resulted in the breach of at least one waste drum and release of waste material in WIPP Panel 7 Room 7 on February 14, 2014. This report integrates and summarizes the results contained in three separate reports, described below, and draws conclusions basedmore » on those results. Chemical and Radiochemical Analyses of WIPP Samples R-15 C5 SWB and R16 C-4 Lip; PNNL-24003, Pacific Northwest National Laboratory, December 2014 Analysis of Waste Isolation Pilot Plant (WIPP) Underground and MgO Samples by the Savannah River National Laboratory (SRNL); SRNL-STI-2014-00617; Savannah River National Laboratory, December 2014 Report for WIPP UG Sample #3, R15C5 (9/3/14); LLNL-TR-667015; Lawrence Livermore National Laboratory, January 2015 This report is also contained in the Waste Isolation Pilot Plant Technical Assessment Team Report; SRNL-RP-2015-01198; Savannah River National Laboratory, March 17, 2015, as Appendix C: Analysis Integrated Summary Report.« less

Characterization of the March 2017 Tank 15 Waste Removal Slurry Sample (Combination of Slurry Samples HTF-15-17-28 and HTF-15-17-29)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Reboul, S. H.; King, W. D.; Coleman, C. J.

2017-05-09

Two March 2017 Tank 15 slurry samples (HTF-15-17-28 and HTF-15-17-29) were collected during the second bulk waste removal campaign and submitted to SRNL for characterization. At SRNL, the two samples were combined and then characterized by a series of physical, elemental, radiological, and ionic analysis methods. Sludge settling as a function of time was also quantified. The characterization results reported in this document are consistent with expectations based upon waste type, process knowledge, comparisons between alternate analysis techniques, and comparisons with the characterization results obtained for the November 2016 Tank 15 slurry sample (the sample collected during the first bulkmore » waste removal campaign).« less

SOLVENT HOLD TANK SAMPLE RESULTS FOR MCU-14-259/260/261 AND MCU-14-315/316/317: APRIL AND MAY 2014 MONTHLY SAMPLES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F.; Taylor-Pashow, K.

2014-08-05

SRNL received two sets of SHT samples (MCU-14-259/260/261 in April 2014 and MCU-14- 315/316/317 in May 2014) for analysis. The samples were analyzed for composition. Both samples have similar chemical composition. As with the previous solvent sample results, these analyses indicate that the solvent does not require Isopar® L trimming at this time. Since an addition of TiDG and MaxCalix to the SHT was added in early July 2014, the solvent does not require TiDG addition at this time. The current TiDG level (1.5 mM) is above the minimum recommended operating level of 1 mM.

Characterization of the March 2017 tank 10 surface sample (combination of HTF-10-17-30 AND HTF-10-17-31) and variable depth sample (combination of HTF-10-17-32 and HTF-10-17-33)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Reboul, S. H.

Two surface samples (HTF-10-17-30 and HTF-10-17-31) and two variable depth samples (HTF-10-17-32 and HTF-10-17-33) were collected from SRS Tank 10 during March 2017 and submitted to SRNL for characterization. At SRNL, the two surface samples were combined in one container, the two variable depth samples (VDSs) were combined in another container, and then the two composite samples were each characterized by a series of physical, ionic, radiological, and elemental analysis methods. The surface sample composite was characterized primarily for Tank Farm corrosion control purposes, while the VDS composite was characterized primarily for Tank Closure Cesium Removal (TCCR) purposes.

Analysis Of 2H-Evaporator Scale Pot Bottom Sample [HTF-13-11-28H

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oji, L. N.

2013-07-15

Savannah River Remediation (SRR) is planning to remove a buildup of sodium aluminosilicate scale from the 2H-evaporator pot by loading and soaking the pot with heated 1.5 M nitric acid solution. Sampling and analysis of the scale material from the 2H evaporator has been performed so that the evaporator can be chemically cleaned beginning July of 2013. Historically, since the operation of the Defense Waste Processing Facility (DWPF), silicon in the DWPF recycle stream combines with aluminum in the typical tank farm supernate to form sodium aluminosilicate scale mineral deposits in the 2H-evaporator pot and gravity drain line. The 2H-evaporatormore » scale samples analyzed by Savannah River National Laboratory (SRNL) came from the bottom cone sections of the 2H-evaporator pot. The sample holder from the 2H-evaporator wall was virtually empty and was not included in the analysis. It is worth noting that after the delivery of these 2H-evaporator scale samples to SRNL for the analyses, the plant customer determined that the 2H evaporator could be operated for additional period prior to requiring cleaning. Therefore, there was no need for expedited sample analysis as was presented in the Technical Task Request. However, a second set of 2H evaporator scale samples were expected in May of 2013, which would need expedited sample analysis. X-ray diffraction analysis (XRD) confirmed the bottom cone section sample from the 2H-evaporator pot consisted of nitrated cancrinite, (a crystalline sodium aluminosilicate solid), clarkeite and uranium oxide. There were also mercury compound XRD peaks which could not be matched and further X-ray fluorescence (XRF) analysis of the sample confirmed the existence of elemental mercury or mercuric oxide. On ''as received'' basis, the scale contained an average of 7.09E+00 wt % total uranium (n = 3; st.dev. = 8.31E-01 wt %) with a U-235 enrichment of 5.80E-01 % (n = 3; st.dev. = 3.96E-02 %). The measured U-238 concentration was 7.05E+00 wt % (n=3, st. dev. = 8.25E-01 wt %). Analyses results for Pu-238 and Pu-239, and Pu-241 are 7.06E-05 {+-} 7.63E-06 wt %, 9.45E-04 {+-} 3.52E-05 wt %, and <2.24E-06 wt %, respectively. These results are provided so that SRR can calculate the equivalent uranium-235 concentrations for the NCSA. Because this 2H evaporator pot bottom scale sample contained a significant amount of elemental mercury (11.7 wt % average), it is recommended that analysis for mercury be included in future Technical Task Requests on 2H evaporator sample analysis at SRNL. Results confirm that the uranium contained in the scale remains depleted with respect to natural uranium. SRNL did not calculate an equivalent U-235 enrichment, which takes into account other fissionable isotopes U-233, Pu-239 and Pu-241.« less

Results of initial analyses of the salt (macro) batch 9 tank 21H qualification samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.

2015-10-01

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Interim Salt Disposition Project (ISDP) Salt (Macro) Batch 9 for processing through the Actinide Removal Process (ARP) and the Modular Caustic-Side Solvent Extraction Unit (MCU). This document reports the initial results of the analyses of samples of Tank 21H. Analysis of the Tank 21H Salt (Macro) Batch 9 composite sample indicates that the material does not display any unusual characteristics or observations, such as floating solids, the presence of large amount of solids, or unusual colors. Further results on the chemistry and other tests willmore » be issued in the future.« less

Sludge batch 9 (SB9) acceptance evaluation. Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.; Diprete, D. P.; Pareizs, J. M.

Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tankmore » 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a composition expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.« less

Sludge batch 9 (SB9) accepance evaluation: Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C.; Diprete, D.; Pareizs, J.

Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tankmore » 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a compositioniv expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.« less

Results of initial analyses of the salt (macro) batch 10 tank 21H qualification samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.

2017-01-01

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Interim Salt Disposition Project (ISDP) Salt (Macro) Batch 10 for processing through the Actinide Removal Process (ARP) and the Modular Caustic-Side Solvent Extraction Unit (MCU). This document reports the initial results of the analyses of samples of Tank 21H. Analysis of the Tank 21H Salt (Macro) Batch 10 composite sample indicates that the material does not display any unusual characteristics or observations, such as floating solids, the presence of large amount of solids, or unusual colors. Further sample results will be reported in a futuremore » document. This memo satisfies part of Deliverable 3 of the Technical Task Request (TTR).« less

Results of initial analyses of the salt (macro) batch 11 Tank 21H qualification samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Interim Salt Disposition Project (ISDP) Salt (Macro) Batch 11 for processing through the Actinide Removal Process (ARP) and the Modular Caustic-Side Solvent Extraction Unit (MCU). This document reports the initial results of the analyses of samples of Tank 21H. Analysis of the Tank 21H Salt (Macro) Batch 11 composite sample indicates that the material does not display any unusual characteristics or observations, such as floating solids, the presence of large amounts of solids, or unusual colors. Further sample results will be reported in a futuremore » document. This memo satisfies part of Deliverable 3 of the Technical Task Request (TTR).« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F.; Taylor-Pashow, K.

SRNL received two sets of SHT samples (MCU-14-667-672, pulled 8/27/2014 and MCU-14-846-847, pulled on 9/22/2014) for analysis. The samples were analyzed for composition. It is recommended that the solvent receives Isopar® L and TiDG trimming at this time. Analysis of sample MCU-14-846-847 indicates the solvent has evaporated Isopar®L and has lost TiDG to a level below the recommended minimum 1 mM level. Since the addition of MaxCalix to the SHT in early July 2014, the MaxCalix concentration in the solvent has reached nominal values. The laboratory will continue to monitor the quality of the solvent in particular for any newmore » impurity or degradation of the solvent components.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

King, W. D.

In order to appropriately model and predict the chemical integrity and performance of cementitious materials used for waste immobilization at the Savannah River Site (SRS), it is critical to understand the I-129 solubility and distribution within the tank farm. Iodine in radioactive waste and in environmental media is typically highly mobile and long lived. Iodine is ubiquitous in SRS tank waste and waste forms. The iodine is assumed to be soluble and present at low levels in Performance Assessments (PAs) for SRS Tank Farms, and is one of the dose drivers in the PAs for both the SRS Salt Disposalmore » Facility (SDF) and the H-Area Tank Farm (HTF). Analysis of tank waste samples is critical to understanding the Tank Farm iodine inventory and reducing disposal uncertainty. Higher than expected iodine levels have recently been observed in residual solids isolated from some SRS tanks prior to closure, indicating uncertainty regarding the chemical species involved. If the iodine inventory uncertainty is larger than anticipated, future work may be necessary to reduce the uncertainty. This memorandum satisfies a portion of the work scope identified in Task Plan SRNL-RP-2016-00651. A separate memorandum issued previously, reported historical unpublished I-129 data, a significant portion of which was below detectable analytical limits. This memorandum includes iodine and general chemical analysis results for six archived SRNL samples which were previously reported to have I-129 concentrations below detectable limits. Lower sample dilution factors were used for the current analyses in order to obtain concentrations above detection. The samples analyzed included surface and depth samples from SRS tanks 30, 32, and 39.« less

Tank 40 Final Sludge Batch 8 Chemical Characterization Results

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, Christopher J.

2013-09-19

A sample of Sludge Batch 8 (SB8) was pulled from Tank 40 in order to obtain radionuclide inventory analyses necessary for compliance with the Waste Acceptance Product Specifications (WAPS). The SB8 WAPS sample was also analyzed for chemical composition, including noble metals, and fissile constituents, and these results are reported here. These analyses along with the WAPS radionuclide analyses will help define the composition of the sludge in Tank 40 that is currently being fed to the Defense Waste Processing Facility (DWPF) as SB8. At SRNL, the 3-L Tank 40 SB8 sample was transferred from the shipping container into amore » 4-L high density polyethylene bottle and solids were allowed to settle. Supernate was then siphoned off and circulated through the shipping container to complete the transfer of the sample. Following thorough mixing of the 3-L sample, a 553 g sub-sample was removed. This sub-sample was then utilized for all subsequent slurry sample preparations. Eight separate aliquots of the slurry were digested, four with HNO{sub 3}/HCl (aqua regia) in sealed Teflon(r) vessels and four with NaOH/Na{sub 2}O{sub 2} (alkali or peroxide fusion) using Zr crucibles. Two Analytical Reference Glass - 1 (ARG-1) standards were digested along with a blank for each preparation. Each aqua regia digestion and blank was diluted to 1:100 mL with deionized water and submitted to Analytical Development (AD) for inductively coupled plasma - atomic emission spectroscopy (ICP-AES) analysis, inductively coupled plasma - mass spectrometry (ICP-MS) analysis, atomic absorption spectroscopy (AA) for As and Se, and cold vapor atomic absorption spectroscopy (CV-AA) for Hg. Equivalent dilutions of the alkali fusion digestions and blank were submitted to AD for ICP-AES analysis. Tank 40 SB8 supernate was collected from a mixed slurry sample in the SRNL Shielded Cells and submitted to AD for ICP-AES, ion chromatography (IC), total base/free OH-/other base, total inorganic carbon/total organic carbon (TIC/TOC) analyses. Weighted dilutions of slurry were submitted for IC, TIC/TOC, and total base/free OH-/other base analyses. Activities for U-233, U-235, and Pu-239 were determined from the ICP-MS data for the aqua regia digestions of the Tank 40 WAPS slurry using the specific activity of each isotope. The Pu-241 value was determined from a Pu-238/-241 method developed by SRNL AD and previously described.« less

Tank 40 final sludge batch 9 chemical and fissile radionuclide characterization results

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.; Kubilius, W. P.; Pareizs, J. M.

A sample of Sludge Batch (SB) 9 was pulled from Tank 40 in order to obtain radionuclide inventory analyses necessary for compliance with the Waste Acceptance Product Specifications (WAPS)i. The SB9 WAPS sample was also analyzed for chemical composition, including noble metals, and fissile constituents, and these results are reported here. These analyses along with the WAPS radionuclide analyses will help define the composition of the sludge in Tank 40 that is fed to the Defense Waste Processing Facility (DWPF) as SB9. At the Savannah River National Laboratory (SRNL), the 3-L Tank 40 SB9 sample was transferred from the shippingmore » container into a 4-L high density polyethylene bottle and solids were allowed to settle. Supernate was then siphoned off and circulated through the shipping container to complete the transfer of the sample. Following thorough mixing of the 3-L sample, a 547 g sub-sample was removed. This sub-sample was then utilized for all subsequent slurry sample preparations. Eight separate aliquots of the slurry were digested, four with HNO3/HCl (aqua regiaii) in sealed Teflon® vessels and four with NaOH/Na2O2 (alkali or peroxide fusioniii) using Zr crucibles. Three Analytical Reference Glass – 1iv (ARG-1) standards were digested along with a blank for each preparation. Each aqua regia digestion and blank was diluted to 1:100 with deionized water and submitted to Analytical Development (AD) for inductively coupled plasma – atomic emission spectroscopy (ICP-AES) analysis, inductively coupled plasma – mass spectrometry (ICP-MS) analysis, atomic absorption spectroscopy (AA) for As and Se, and cold vapor atomic absorption spectroscopy (CV-AA) for Hg. Equivalent dilutions of the alkali fusion digestions and blank were submitted to AD for ICP-AES analysis. Tank 40 SB9 supernate was collected from a mixed slurry sample in the SRNL Shielded Cells and submitted to AD for ICP-AES, ion chromatography (IC), total base/free OH-/other base, total inorganic carbon/total organic carbon (TIC/TOC) analyses. Weighted dilutions of slurry were submitted for IC, TIC/TOC, and total base/free OH-/other base analyses. Activities for U-233, U-235, and Pu-239 were determined from the ICP-MS data for the aqua regia digestions of the SB9 WAPS slurry using the specific activity of each isotope. The Pu-241 value was determined from a Pu-238/-241 method developed by SRNL AD and previously described.v« less

ANALYSIS OF SAMPLES FROM TANK 5F CHEMICAL CLEANING

DOE Office of Scientific and Technical Information (OSTI.GOV)

Poirier, M.; Fink, S.

2011-03-07

The Savannah River Site (SRS) is preparing Tank 5F for closure. The first step in preparing the tank for closure is mechanical sludge removal. Following mechanical sludge removal, SRS performed chemical cleaning with oxalic acid to remove the sludge heel. Personnel are currently assessing the effectiveness of the chemical cleaning. SRS personnel collected liquid samples during chemical cleaning and submitted them to Savannah River National Laboratory (SRNL) for analysis. Following chemical cleaning, they collected a solid sample (also known as 'process sample') and submitted it to SRNL for analysis. The authors analyzed these samples to assess the effectiveness of themore » chemical cleaning process. The conclusions from this work are: (1) With the exception of iron, the dissolution of sludge components from Tank 5F agreed with results from the actual waste demonstration performed in 2007. The fraction of iron removed from Tank 5F by chemical cleaning was significantly less than the fraction removed in the SRNL demonstrations. The likely cause of this difference is the high pH following the first oxalic acid strike. (2) Most of the sludge mass remaining in the tank is iron and nickel. (3) The remaining sludge contains approximately 26 kg of barium, 37 kg of chromium, and 37 kg of mercury. (4) Most of the radioactivity remaining in the residual material is beta emitters and {sup 90}Sr. (5) The chemical cleaning removed more than {approx} 90% of the uranium isotopes and {sup 137}Cs. (6) The chemical cleaning removed {approx} 70% of the neptunium, {approx} 83% of the {sup 90}Sr, and {approx} 21% of the {sup 60}Co. (7) The chemical cleaning removed less than 10% of the plutonium, americium, and curium isotopes. (8) The chemical cleaning removed more than 90% of the aluminium, calcium, and sodium from the tank. (9) The cleaning operations removed 61% of lithium, 88% of non-radioactive strontium, and 65% of zirconium. The {sup 90}Sr and non-radioactive strontium were measured by different methods, and the differences in the fraction removed are not statistically significant. (10) Chemical cleaning removed 10-50% of the barium, chromium, iron, magnesium, manganese, and silicon. (11) Chemical cleaning removed only {approx}1% of the nickel.« less

TANK 26F SUPERNATANT AND 2F EVAPORATOR EDUCTOR PUMP SAMPLE CHARACTERIZATION RESULTS

DOE Office of Scientific and Technical Information (OSTI.GOV)

King, W.; Hay, M.; Coleman, C.

2011-08-23

In an effort to understand the reasons for system plugging problems in the SRS 2F evaporator, supernatant samples were retrieved from the evaporator feed tank (Tank 26F) and solids were collected from the evaporator eductor feed pump for characterization. The variable depth supernatant samples were retrieved from Tank 26F in early December of 2010 and samples were provided to SRNL and the F/H Area laboratories for analysis. Inspection and analysis of the samples at SRNL was initiated in early March of 2011. During the interim period, samples were frequently exposed to temperatures as low as 12 C with daily temperaturemore » fluctuations as high as 10 C. The temperature at the time of sample collection from the waste tank was 51 C. Upon opening the supernatant bottles at SRNL, many brown solids were observed in both of the Tank 26F supernatant samples. In contrast, no solids were observed in the supernatant samples sent to the F/H Area laboratories, where the analysis was completed within a few days after receipt. Based on these results, it is believed that the original Tank 26F supernatant samples did not contain solids, but solids formed during the interim period while samples were stored at ambient temperature in the SRNL shielded cells without direct climate control. Many insoluble solids (>11 wt. % for one sample) were observed in the Tank 26F supernatant samples after three months of storage at SRNL which would not dissolve in the supernatant solution in two days at 51 C. Characterization of these solids along with the eductor pump solids revealed the presence of sodium oxalate and clarkeite (uranyl oxyhydroxide) as major crystalline phases. Sodium nitrate was the dominant crystalline phase present in the unwashed Eductor Pump solids. Crystalline sodium nitrate may have formed during the drying of the solids after filtration or may have been formed in the Tank 26F supernatant during storage since the solution was found to be very concentrated (9-12 M Na{sup +}). Concentrated mineral acids and elevated temperature were required to dissolve all of these solids. The refractory nature of some of the solids is consistent with the presence of metal oxides such as aluminosilicates (observed as a minor phase by XRD). Characterization of the water wash solutions and the digested solids confirmed the presence of oxalate salts in both solid samples. Sulfate enrichment was also observed in the Tank 26F solids wash solution, indicating the presence of sulfate precipitates such as burkeite. OLI modeling of the Tank 26F filtered supernatant composition revealed that sodium oxalate has a very low solubility in this solution. The model predicts that the sodium oxalate solubility in the Tank 26F supernatant is only 0.0011 M at 50 C. The results indicate that the highly concentrated nature of the evaporator feed solution and the addition of oxalate anion to the waste stream each contribute to the formation of insoluble solids in the 2F evaporator system.« less

Solvent hold tank sample results for MCU-16-1317-1318-1319. September 2016 monthly sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Jones, D. H.

2017-01-01

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-1317-1318-1319), pulled on 09/12/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-1317-1318-1319 indicated the Isopar™L concentration is above its nominal level (102%). The extractant (MaxCalix) and the modifier (CS-7SB) are 5% and 10 % below their nominal concentrations. The suppressor (TiDG) is 77% below its nominal concentration. A summary of the concentration of the relevant solvent components is shown below. This analysis confirms the Isopar™ addition to the solvent in August. This analysis also indicates the solvent maymore » require the addition of TiDG, and possibly of modifier to restore them to nominal levels.« less

Sulfur Solubility Testing and Characterization of LAW Phase 1 Matrix Glasses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fox, K.

In this report, the Savannah River National Laboratory (SRNL) provides chemical analysis results for a series of simulated low-activity waste (LAW) glass compositions. These data will be used in the development of improved sulfur solubility models for LAW glass. A procedure developed at Pacific Northwest National Laboratory (PNNL) for producing sulfur saturated melts (SSMs) was carried out at both SRNL and PNNL to fabricate the glasses characterized in this report. This method includes triplicate melting steps with excess sodium sulfate, followed by grinding and washing to remove unincorporated sulfur salts. The wash solutions were also analyzed as part of thismore » study.« less

Characterization Of The As-Received Sludge Batch 9 Qualification Sample (Htf-51-15-81)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pareizs, J.

Savannah River National Laboratory (SRNL) personnel have been requested to qualify the next sludge batch (Sludge Batch 9 – SB9) for processing at the Defense Waste Processing Facility (DWPF). To accomplish this task, Savannah River Remediation (SRR) has sent SRNL a 3-L slurried sample of Tank 51H (HTF-51-15-81) to be characterized, washed, and then used in a lab-scale demonstration of the DWPF flowsheet (potentially after combining with Tank 40H sludge). This report documents the first steps of the qualification process – characterization of the as-received Tank 51H qualification sample. These results will be used to support a reprojection of SB9more » by SRR from which final Tank 51H washing, frit development, and Chemical Processing Cell (CPC) activities will be based.« less

SNL/SRNL Joint Project on degradation of mechanical properties in structural metals and welds for GTS reservoirs.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ronevich, Joseph Allen; Balch, Dorian K.; San Marchi, Christopher W.

2015-12-01

This project was intended to enable SNL-CA to produce appropriate specimens of relevant stainless steels for testing and perform baseline testing of weld heat-affected zone and weld fusion zone. One of the key deliverables in this project was to establish a procedure for fracture testing stainless steel weld fusion zone and heat affected zones that were pre-charged with hydrogen. Following the establishment of the procedure, a round robin was planned between SNL-CA and SRNL to ensure testing consistency between laboratories. SNL-CA and SRNL would then develop a comprehensive test plan, which would include tritium exposures of several years at SRNLmore » on samples delivered by SNL-CA. Testing would follow the procedures developed at SNL-CA. SRNL will also purchase tritium charging vessels to perform the tritium exposures. Although comprehensive understanding of isotope-induced fracture in GTS reservoir materials is a several year effort, the FY15 work would enabled us to jump-start the tests and initiate long-term tritium exposures to aid comprehensive future investigations. Development of a procedure and laboratory testing consistency between SNL-CA and SNRL ensures reliability in results as future evaluations are performed on aluminum alloys and potentially additively-manufactured components.« less

Solvent Hold Tank Sample Results for MCU-16-596-597-598: April 2016 Monthly Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Jones, D. H.

2016-07-12

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-596-597-598), pulled on 04/30/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-596-597-598 indicated the Isopar™L concentration is above its nominal level (102%). The modifier (CS-7SB) is 14% below its nominal concentration, while the TiDG and MaxCalix concentrations are at and above their nominal concentrations, respectively. This analysis confirms the solvent may require the addition of modifier. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expectedmore » to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Boggess, A.

Existing models and simulants of tank disposition media at SRS have presumed the presence of high concentrations of inorganic mercury. However, recent quarterly tank analyses show that mercury is present as organomercurial species at concentrations that may present challenges to remediation and disposition and may exceed the Saltstone Waste Acceptance Criteria (WAC). To-date, methylmercury analysis for Savannah River Remediation (SRR) has been performed off-site by Eurofins Scientific (Lancaster, PA). A series of optimization and validation experiments has been performed at SRNL, which has resulted in the development of on-site organomercury speciation capabilities using purge and trap gas chromatography coupled withmore » thermal desorption cold vapor atomic fluorescence spectroscopy (P&T GC/CVAFS). Speciation has been achieved for methylmercury, with a method reporting limit (MRL) values of 1.42 pg for methylmercury. Results obtained by SRNL from the analysis of past quarterly samples from tanks 21, 40, and 50 have demonstrated statistically indistinguishable concentration values compared with the concentration data obtained from Eurofins, while the data from SRNL has demonstrated significantly improved precision and processing time.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

King, W. D.; Restivo, M. L.; Martino, C. J.

Radioactive waste samples retrieved from Savannah River Site (SRS) Tanks 38H and 43H (concentrate receipt and feed tanks, respectively, for the 2H Evaporator system) were evaluated with regard to their tendency to form foams during air sparging. This work was conducted due to recent processing issues and outages in the evaporator that were believed to have resulted from sample foaming. The samples evaluated for foam formation included supernate collected in April of 2014 (near the time of the evaporator outage) as well as historical samples available within the SRNL shielded cells facility. The April samples included one Tank 43H surfacemore » sample (HTF-43-14-42), one Tank 43H sub-surface sample (HTF-43-14-43), and one Tank 38H (HTF-38-14-41) surface sample. In addition, two Tank 43H samples (HTF-43-14-8 and HTF-43-14-9) and one Tank 38H sample (HTF-38-14-6) were also evaluated along with a blended sample of various historical Tank 38H and 43H samples. Characterization results for the April samples are also provided. The composition of the samples was similar to historical evaporator system samples received at SRNL.« less

Sample Results From Tank 48H Samples HTF-48-14-158, -159, -169, and -170

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T.; Hang, T.

2015-04-28

Savannah River National Laboratory (SRNL) analyzed samples from Tank 48H in support of determining the cause for the unusually high dose rates at the sampling points for this tank. A set of two samples was taken from the quiescent tank, and two additional samples were taken after the contents of the tank were mixed. The results of the analyses of all the samples show that the contents of the tank have changed very little since the analysis of the previous sample in 2012. The solids are almost exclusively composed of tetraphenylborate (TPB) salts, and there is no indication of accelerationmore » in the TPB decomposition. The filtrate composition shows a moderate increase in salt concentration and density, which is attributable to the addition of NaOH for the purposes of corrosion control. An older modeling simulation of the TPB degradation was updated, and the supernate results from a 2012 sample were run in the model. This result was compared to the results from the 2014 recent sample results reported in this document. The model indicates there is no change in the TPB degradation from 2012 to 2014. SRNL measured the buoyancy of the TPB solids in Tank 48H simulant solutions. It was determined that a solution of density 1.279 g/mL (~6.5M sodium) was capable of indefinitely suspending the TPB solids evenly throughout the solution. A solution of density 1.296 g/mL (~7M sodium) caused a significant fraction of the solids to float on the solution surface. As the experiments could not include the effect of additional buoyancy elements such as benzene or hydrogen generation, the buoyancy measurements provide an upper bound estimate of the density in Tank 48H required to float the solids.« less

Sulfur Solubility Testing and Characterization of Hanford LAW Phase 2, Inner Layer Matrix Glasses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fox, K. M.; Edwards, T. B.; Caldwell, M. E.

In this report, the Savannah River National Laboratory (SRNL) provides chemical analyses and Product Consistency Test (PCT) results for a series of simulated low activity waste (LAW) glass compositions. A procedure developed at the Pacific Northwest National Laboratory (PNNL) for producing sulfur saturated melts (SSMs) was carried out at both SRNL and PNNL to fabricate the glasses characterized in this report. This method includes triplicate melting steps with excess sodium sulfate, followed by grinding and washing to remove unincorporated sulfur salts. The wash solutions were also analyzed as part of this study. These data will be used in the developmentmore » of improved sulfur solubility models for LAW glass.« less

Gum-compliant uncertainty propagations for Pu and U concentration measurements using the 1st-prototype XOS/LANL hiRX instrument; an SRNL H-Canyon Test Bed performance evaluation project

DOE Office of Scientific and Technical Information (OSTI.GOV)

Holland, Michael K.; O'Rourke, Patrick E.

An SRNL H-Canyon Test Bed performance evaluation project was completed jointly by SRNL and LANL on a prototype monochromatic energy dispersive x-ray fluorescence instrument, the hiRX. A series of uncertainty propagations were generated based upon plutonium and uranium measurements performed using the alpha-prototype hiRX instrument. Data reduction and uncertainty modeling provided in this report were performed by the SRNL authors. Observations and lessons learned from this evaluation were also used to predict the expected uncertainties that should be achievable at multiple plutonium and uranium concentration levels provided instrument hardware and software upgrades being recommended by LANL and SRNL are performed.

Rapid determination of 226Ra in emergency urine samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, Sherrod L.; Culligan, Brian K.; Hutchison, Jay B.

2014-02-27

A new method has been developed at the Savannah River National Laboratory (SRNL) that can be used for the rapid determination of 226Ra in emergency urine samples following a radiological incident. If a radiological dispersive device event or a nuclear accident occurs, there will be an urgent need for rapid analyses of radionuclides in urine samples to ensure the safety of the public. Large numbers of urine samples will have to be analyzed very quickly. This new SRNL method was applied to 100 mL urine aliquots, however this method can be applied to smaller or larger sample aliquots as needed.more » The method was optimized for rapid turnaround times; urine samples may be prepared for counting in <3 h. A rapid calcium phosphate precipitation method was used to pre-concentrate 226Ra from the urine sample matrix, followed by removal of calcium by cation exchange separation. A stacked elution method using DGA Resin was used to purify the 226Ra during the cation exchange elution step. This approach combines the cation resin elution step with the simultaneous purification of 226Ra with DGA Resin, saving time. 133Ba was used instead of 225Ra as tracer to allow immediate counting; however, 225Ra can still be used as an option. The rapid purification of 226Ra to remove interferences using DGA Resin was compared with a slightly longer Ln Resin approach. A final barium sulfate micro-precipitation step was used with isopropanol present to reduce solubility; producing alpha spectrometry sources with peaks typically <40 keV FWHM (full width half max). This new rapid method is fast, has very high tracer yield (>90 %), and removes interferences effectively. The sample preparation method can also be adapted to ICP-MS measurement of 226Ra, with rapid removal of isobaric interferences.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Jones, D. H.

Savannah River National Laboratory (SRNL) received one set of three Solvent Hold Tank (SHT) samples (MCU-16-1363-1364-1365), pulled on 11/15/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-1363-1364-1365 indicated the Isopar™L concentration is at its nominal level (100%). The extractant (MaxCalix) and the modifier (CS- 7SB) are 8% and 2 % below their nominal concentrations. The suppressor (TiDG) is 7% below its nominal concentration. This analysis confirms the trim and Isopar™ additions to the solvent in November. This analysis also indicates the solvent did not require further additions. Based on the current monthlymore » sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.« less

Analytical Results from Routine DSSHT and SEHT Monthly Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.

2016-08-17

Strip Effluent Hold Tank (SEHT) and Decontaminated Salt Solution Hold Tank (DSSHT) samples from several of the “microbatches” of Integrated Salt Disposition Project (ISDP) Salt Batch (“Macrobatch”) 8B have been analyzed for 238Pu, 90Sr, 137Cs, cations (Inductively Coupled Plasma Emission Spectroscopy - ICPES), and anions (Ion Chromatography Anions - IC-A). The analytical results from the current microbatch samples are similar to those from previous macrobatch samples. The Actinide Removal Process (ARP) and the Modular Caustic-Side Solvent Extraction Unit (MCU) continue to show more than adequate Pu and Sr removal for times when monosodium titanate (MST) is used. Even with nomore » MST strike being performed there exists some small Pu and Sr removal, likely from filtration of fines containing these elements. The Cs removal continues to be excellent, with decontamination factors (DF) averaging 16,400. The bulk chemistry of the DSSHT and SEHT samples do not show any signs of unusual behavior. SRNL recommends that a sample of the strip feed be analyzed for cation and anion content if a further decline in boron concentration is noted in future SEHT samples.« less

Analysis of Tank 38H (HTF-38-16-80, 81) and Tank 43H (HTF-43-16-82, 83) Samples for Support of the Enrichment Control and Corrosion Control Programs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hay, M.

2016-10-24

SRNL analyzed samples from Tank 38H and Tank 43H to support ECP and CCP. The total uranium in the Tank 38H surface sample was 57.6 mg/L, while the sub-surface sample was 106 mg/L. The Tank 43H samples ranged from 50.0 to 51.9 mg/L total uranium. The U-235 percentage was consistent for all four samples at 0.62%. The total uranium and percent U-235 results appear consistent with recent Tank 38H and Tank 43H uranium measurements. The Tank 38H plutonium results show a large difference between the surface and sub-surface sample concentrations and somewhat higher concentrations than previous samples. The Pu-238 concentrationmore » is more than forty times higher in the Tank 38H sub-surface sample than the surface sample. The surface and sub-surface Tank 43H samples contain similar plutonium concentrations and are within the range of values measured on previous samples. The four samples analyzed show silicon concentrations somewhat higher than the previous sample with values ranging from 104 to 213 mg/L.« less

Gray QB-sing-faced version 2 (SF2) open environment test report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Plummer, J.; Immel, D.; Bobbitt, J.

This report details the design upgrades incorporated into the new version of the GrayQbTM SF2 device and the characterization testing of this upgraded device. Results from controlled characterization testing in the Savannah River National Laboratory (SRNL) R&D Engineering Imaging and Radiation Lab (IRL) and the Savannah River Site (SRS) Health Physics Instrument Calibration Laboratory (HPICL) is presented, as well as results from the open environment field testing performed in the E-Area Low Level Waste Storage Area. Resultant images presented in this report were generated using the SRNL developed Radiation Analyzer (RAzerTM) software program which overlays the radiation contour images ontomore » the visual image of the location being surveyed.« less

Results of Hg speciation testing on MCU strip effluent hold tank (SEHT) and decontaminated salt solution hold tank (DSSHT) materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.

2015-09-17

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team.i,ii The tenth shipment of samples was designated to include Modular Caustic Side Solvent Extraction Unit (MCU) Strip Effluent Hold Tank (SEHT) and MCU Decontaminated Salt Solution Hold Tank (DSSHT) materials from processing Salt Batch 7b. The MCU SEHT (MCU-15-722) and DSSHT (MCU-15-709) samples were pulled on June 15, 2015. All MCU samples were received at SRNL on June 16, 2015. The DSSHT sample wasmore » moved the same day to refrigeration, while the SEHT sample was placed in the Shielded Cells. On July 9, 2015 it was opened and an aliquot diluted 1:100 with Eurofins deionized water and a portion of the diluted sample transferred to a Teflon® bottle prior to moving it to refrigeration that same day. All samples were kept in the dark and refrigerated until final dilutions were prepared for shipment to Eurofins.« less

Results of Hg speciation testing on DWPF SMECT-8, OGCT-1, AND OGCT-2 samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C.

2016-02-22

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team. The sixteenth shipment of samples was designated to include a Defense Waste Processing Facility (DWPF) Slurry Mix Evaporator Condensate Tank (SMECT) sample from Sludge Receipt and Adjustment Tank (SRAT) Batch 738 processing and two Off-Gas Condensate Tank (OGCT) samples, one following Batch 736 and one following Batch 738. The DWPF sample designations for the three samples analyzed are provided. The Batch 738 ‘End ofmore » SME Cycle’ SMECT sample was taken at the conclusion of Slurry Mix Evaporator (SME) operations for this batch and represents the fourth SMECT sample examined from Batch 738. Batch 738 experienced a sludge slurry carryover event, which introduced sludge solids to the SMECT that were particularly evident in the SMECT-5 sample, but less evident in the ‘End of SME Cycle’ SMECT-8 sample.« less

Characterization of the tank 51 alternate reductant sludge batch 9 slurry sample (HTF-51-15-130)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Reboul, S. H.

Tank 51 slurry sample HTF-51-15-130 was collected following sludge washing at the Tank Farm. The sample was received at SRNL and then characterized in preparation for qualification of the alternate reductant Sludge Batch 9 (SB9) flowsheet. In this characterization, densities, solids distribution, elemental constituents, anionic constituents, carbon content, and select radioisotopes were quantified.

DOE Office of Scientific and Technical Information (OSTI.GOV)

French, T

I am pleased to present the fiscal year 2007 Laboratory Directed Research and Development (LDRD) annual report. This represents the first year that SRNL has been eligible for LDRD participation and our results to date demonstrate we are off to an excellent start. SRNL became a National Laboratory in 2004, and was designated the 'Corporate Laboratory' for the DOE Office of Environmental Management (EM) in 2006. As you will see, we have made great progress since these designations. The LDRD program is one of the tools SRNL is using to enable achievement of our strategic goals for the DOE. Themore » LDRD program allows the laboratory to blend a strong basic science component into our applied technical portfolio. This blending of science with applied technology provides opportunities for our scientists to strengthen our capabilities and delivery. The LDRD program is vital to help SRNL attract and retain leading scientists and engineers who will help build SRNL's future and achieve DOE mission objectives. This program has stimulated our research staff creativity, while realizing benefits from their participation. This investment will yield long term dividends to the DOE in its Environmental Management, Energy, and National Security missions.« less

NEUTRON MULTIPLICITY AND ACTIVE WELL NEUTRON COINCIDENCE VERIFICATION MEASUREMENTS PERFORMED FOR MARCH 2009 SEMI-ANNUAL DOE INVENTORY

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dewberry, R.; Ayers, J.; Tietze, F.

The Analytical Development (AD) Section field nuclear measurement group performed six 'best available technique' verification measurements to satisfy a DOE requirement instituted for the March 2009 semi-annual inventory. The requirement of (1) yielded the need for SRNL Research Operations Department Material Control & Accountability (MC&A) group to measure the Pu content of five items and the highly enrich uranium (HEU) content of two. No 14Q-qualified measurement equipment was available to satisfy the requirement. The AD field nuclear group has routinely performed the required Confirmatory Measurements for the semi-annual inventories for fifteen years using sodium iodide and high purity germanium (HpGe)more » {gamma}-ray pulse height analysis nondestructive assay (NDA) instruments. With appropriate {gamma}-ray acquisition modeling, the HpGe spectrometers can be used to perform verification-type quantitative assay for Pu-isotopics and HEU content. The AD nuclear NDA group is widely experienced with this type of measurement and reports content for these species in requested process control, MC&A booking, and holdup measurements assays Site-wide. However none of the AD HpGe {gamma}-ray spectrometers have been 14Q-qualified, and the requirement of reference 1 specifically excluded a {gamma}-ray PHA measurement from those it would accept for the required verification measurements. The requirement of reference 1 was a new requirement for which the Savannah River National Laboratory (SRNL) Research Operations Department (ROD) MC&A group was unprepared. The criteria for exemption from verification were: (1) isotope content below 50 grams; (2) intrinsically tamper indicating or TID sealed items which contain a Category IV quantity of material; (3) assembled components; and (4) laboratory samples. Therefore all (SRNL) Material Balance Area (MBA) items with greater than 50 grams total Pu or greater than 50 grams HEU were subject to a verification measurement. The pass/fail criteria of reference 7 stated 'The facility will report measured values, book values, and statistical control limits for the selected items to DOE SR...', and 'The site/facility operator must develop, document, and maintain measurement methods for all nuclear material on inventory'. These new requirements exceeded SRNL's experience with prior semi-annual inventory expectations, but allowed the AD nuclear field measurement group to demonstrate its excellent adaptability and superior flexibility to respond to unpredicted expectations from the DOE customer. The requirements yielded five SRNL items subject to Pu verification and two SRNL items subject to HEU verification. These items are listed and described in Table 1.« less

SLUDGE WASHING AND DEMONSTRATION OF THE DWPF FLOWSHEET IN THE SRNL SHIELDED CELLS FOR SLUDGE BATCH 7A QUALIFICATION

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pareizs, J.; Billings, A.; Click, D.

2011-07-08

Waste Solidification Engineering (WSE) has requested that characterization and a radioactive demonstration of the next batch of sludge slurry (Sludge Batch 7a*) be completed in the Shielded Cells Facility of the Savannah River National Laboratory (SRNL) via a Technical Task Request (TTR). This characterization and demonstration, or sludge batch qualification process, is required prior to transfer of the sludge from Tank 51 to the Defense Waste Processing Facility (DWPF) feed tank (Tank 40). The current WSE practice is to prepare sludge batches in Tank 51 by transferring sludge from other tanks. Discharges of nuclear materials from H Canyon are oftenmore » added to Tank 51 during sludge batch preparation. The sludge is washed and transferred to Tank 40, the current DWPF feed tank. Prior to transfer of Tank 51 to Tank 40, SRNL simulates the Tank Farm and DWPF processes with a Tank 51 sample (referred to as the qualification sample). Sludge Batch 7a (SB7a) is composed of portions of Tanks 4, 7, and 12; the Sludge Batch 6 heel in Tank 51; and a plutonium stream from H Canyon. SRNL received the Tank 51 qualification sample (sample ID HTF-51-10-125) following sludge additions to Tank 51. This report documents: (1) The washing (addition of water to dilute the sludge supernate) and concentration (decanting of supernate) of the SB7a - Tank 51 qualification sample to adjust sodium content and weight percent insoluble solids to Tank Farm projections. (2) The performance of a DWPF Chemical Process Cell (CPC) simulation using the washed Tank 51 sample. The simulation included a Sludge Receipt and Adjustment Tank (SRAT) cycle, where acid was added to the sludge to destroy nitrite and reduce mercury, and a Slurry Mix Evaporator (SME) cycle, where glass frit was added to the sludge in preparation for vitrification. The SME cycle also included replication of five canister decontamination additions and concentrations. Processing parameters were based on work with a non-radioactive simulant. (3) Vitrification of a portion of the SME product and characterization and durability testing (as measured by the Product Consistency Test (PCT)) of the resulting glass. (4) Rheology measurements of the initial slurry samples and samples after each phase of CPC processing. This program was controlled by a Task Technical and Quality Assurance Plan (TTQAP), and analyses were guided by an Analytical Study Plan. This work is Technical Baseline Research and Development (R&D) for the DWPF. It should be noted that much of the data in this document has been published in interoffice memoranda. The intent of this technical report is bring all of the SB7a related data together in a single permanent record and to discuss the overall aspects of SB7a processing.« less

Innovative approach to reduction of waste streams for cutting operations in remote environments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Skibo, A.

SRNL proposes to develop and demonstrate an approach using the SRNL rotary microfilter (RMF) technology for reducing waste streams in remote cutting operations during decontamination operations. SRNL offers to collaborate with Tokyo Electric Power Company (TEPCO) in evaluation, testing, and utilization of SRNL’s radiation-hardened rotary microfilter in the deactivation and decommissioning (D&D) operations of the Fukushima Daiichi Nuclear Power Station (NPS). Refinement of the scope and associated costs will be conducted in consultation with TEPCO.

A Next Generation Digital Counting System For Low-Level Tritium Studies (Project Report)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bowman, P.

2016-10-03

Since the early seventies, SRNL has pioneered low-level tritium analysis using various nuclear counting technologies and techniques. Since 1999, SRNL has successfully performed routine low-level tritium analyses with counting systems based on digital signal processor (DSP) modules developed in the late 1990s. Each of these counting systems are complex, unique to SRNL, and fully dedicated to performing routine tritium analyses of low-level environmental samples. It is time to modernize these systems due to a variety of issues including (1) age, (2) lack of direct replacement electronics modules and (3) advances in digital signal processing and computer technology. There has beenmore » considerable development in many areas associated with the enterprise of performing low-level tritium analyses. The objective of this LDRD project was to design, build, and demonstrate a Next Generation Tritium Counting System (NGTCS), while not disrupting the routine low-level tritium analyses underway in the facility on the legacy counting systems. The work involved (1) developing a test bed for building and testing new counting system hardware that does not interfere with our routine analyses, (2) testing a new counting system based on a modern state of the art DSP module, and (3) evolving the low-level tritium counter design to reflect the state of the science.« less

Extraction, -scrub, -strip test results from the interim salt disposition program macrobatch 10 tank 21H qualification samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.

Savannah River National Laboratory (SRNL) analyzed samples from Tank 21H in support of qualification of Macrobatch (Salt Batch) 10 for the Interim Salt Disposition Program (ISDP). The Salt Batch 10 characterization results were previously reported.ii,iii An Extraction, -Scrub, -Strip (ESS) test was performed to determine cesium distribution ratios (D(Cs)) and cesium concentration in the strip effluent (SE) and decontaminated salt solution (DSS) streams; this data will be used by Tank Farm Engineering to project a cesium decontamination factor (DF). This test used actual Tank 21H material, and a sample of the NGS Blend solvent currently being used at the Modularmore » Caustic-Side Solvent Extraction Unit (MCU). The ESS test showed acceptable performance with an extraction D(Cs) value of 110. This value is consistent with results from previous salt batch ESS tests using similar solvent formulations. This is better than the predicted value of 39.8 from a recently created D(Cs) model.« less

DEVELOPMENT OF A CERAMIC TAMPER INDICATING SEAL: SRNL CONTRIBUTIONS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Krementz, D.; Brinkman, K.; Martinez-Rodriguez, M.

2013-06-03

Savannah River National Laboratory (SRNL) and Sandia National Laboratories (SNL) are collaborating on development of a Ceramic Seal, also sometimes designated the Intrinsically Tamper Indicating Ceramic Seal (ITICS), which is a tamper indicating seal for international safeguards applications. The Ceramic Seal is designed to be a replacement for metal loop seals that are currently used by the IAEA and other safeguards organizations. The Ceramic Seal has numerous features that enhance the security of the seal, including a frangible ceramic body, protective and tamper indicating coatings, an intrinsic unique identifier using Laser Surface Authentication, electronics incorporated into the seal that providemore » cryptographic seal authentication, and user-friendly seal wire capture. A second generation prototype of the seal is currently under development whose seal body is of Low Temperature Co-fired Ceramic (LTCC) construction. SRNL has developed the mechanical design of the seal in an iterative process incorporating comments from the SNL vulnerability review team. SRNL is developing fluorescent tamper indicating coatings, with recent development focusing on optimizing the durability of the coatings and working with a vendor to develop a method to apply coatings on a 3-D surface. SRNL performed a study on the effects of radiation on the electronics of the seal and possible radiation shielding techniques to minimize the effects. SRNL is also investigating implementation of Laser Surface Authentication (LSA) as a means of unique identification of each seal and the effects of the surface coatings on the LSA signature.« less

NITRATE CONVERSION OF HB-LINE REILLEXTM HPQ RESIN

DOE Office of Scientific and Technical Information (OSTI.GOV)

Steimke, J.; Williams, M.; Steeper, T.

Reillex{trademark} HPQ ion exchange resin is used by HB Line to remove plutonium from aqueous streams. Reillex{trademark} HPQ resin currently available from Vertellus Specialties LLC is a chloride ionic form, which can cause stress corrosion cracking in stainless steels. Therefore, HB Line Engineering requested that Savannah River National Laboratory (SRNL) convert resin from chloride form to nitrate form in the Engineering Development Laboratory (EDL). To perform this task, SRNL treated two batches of resin in 2012. The first batch of resin from Reilly Industries Batch 80302MA was initially treated at SRNL in 2001 to remove chloride. This batch of resin,more » nominally 30 liters, has been stored wet in carboys since that time until being retreated in 2012. The second batch of resin from Batch 23408 consisted of 50 kg of new resin purchased from Vertellus Specialties in 2012. Both batches were treated in a column designed to convert resin using downflow of 1.0 M sodium nitrate solution through the resin bed followed by rinsing with deionized water. Both batches were analyzed for chloride concentration, before and after treatment, using Neutron Activation Analysis (NAA). The resin specification [Werling, 2003] states the total chlorine and chloride concentration shall be less than 250 ppm. The resin condition for measuring this concentration is not specified; however, in service the resin would always be fully wet. Measurements in SRNL showed that changing from oven dry resin to fully wet resin, with liquid in the particle interstices but no supernatant, increases the total weight by a factor of at least three. Therefore, concentration of chlorine or chloride expressed as parts per million (ppm) decreases by a factor of three. Therefore, SRNL recommends measuring chlorine concentration on an oven dry basis, then dividing by three to estimate chloride concentration in the fully wet condition. Chloride concentration in the first batch (No.80302MA) was nearly the same before the current treatment (759 ppm dry) and after treatment (745 ppm dry or {approx}248 ppm wet). Treatment of the second batch of resin (No.23408) was very successful. Chloride concentration decreased from 120,000 ppm dry to an average of 44 ppm dry or {approx}15ppm wet, which easily passes the 250 ppm wet criterion. Per guidance from HB Line Engineering, SRNL blended Batch 80302 resin with Batch P9059 resin which had been treated previously by ResinTech to remove chloride. The chloride concentrations for the two drums of Batch P9059 were 248 ppm dry ({approx}83 ppm wet) {+-}22.8% and 583 ppm dry ({approx}194 ppm wet) {+-} 11.8%. The blended resin was packaged in five gallon buckets.« less

MEASUREMENT OF WIND SPEED FROM COOLING LAKE THERMAL IMAGERY

DOE Office of Scientific and Technical Information (OSTI.GOV)

Garrett, A; Robert Kurzeja, R; Eliel Villa-Aleman, E

2009-01-20

The Savannah River National Laboratory (SRNL) collected thermal imagery and ground truth data at two commercial power plant cooling lakes to investigate the applicability of laboratory empirical correlations between surface heat flux and wind speed, and statistics derived from thermal imagery. SRNL demonstrated in a previous paper [1] that a linear relationship exists between the standard deviation of image temperature and surface heat flux. In this paper, SRNL will show that the skewness of the temperature distribution derived from cooling lake thermal images correlates with instantaneous wind speed measured at the same location. SRNL collected thermal imagery, surface meteorology andmore » water temperatures from helicopters and boats at the Comanche Peak and H. B. Robinson nuclear power plant cooling lakes. SRNL found that decreasing skewness correlated with increasing wind speed, as was the case for the laboratory experiments. Simple linear and orthogonal regression models both explained about 50% of the variance in the skewness - wind speed plots. A nonlinear (logistic) regression model produced a better fit to the data, apparently because the thermal convection and resulting skewness are related to wind speed in a highly nonlinear way in nearly calm and in windy conditions.« less

Analysis of 2H-Evaporator Acid Cleaning Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hay, M.; Diprete, D.; Edwards, T.

The 2H-Evaporator acid cleaning solution samples were analyzed by SRNL to determine a composition for the scale present in the evaporator before recent acid cleaning. Composite samples were formed from the solution samples from the two acid cleaning cycles. The solution composition was converted to a weight percent scale solids basis under an assumed chemical composition. The scale composition produced from the acid cleaning solution samples indicates a concentration of 6.85 wt% uranium. An upper bound, onesided 95% confidence interval on the weight percent uranium value may be given as 6.9 wt% + 1.645 × 0.596 wt% = 7.9 wt%.more » The comparison of the composition from the current acid cleaning solutions with the composition of recent scale samples along with the thermodynamic modeling results provides reasonable assurance that the sample results provide a good representation of the overall scale composition in the evaporator prior to acid cleaning. The small amount of scale solids dissolved in the 1.5 M nitric acid during the evaporator cleaning process likely produced only a small amount of precipitation based on modeling results and the visual appearance of the samples.« less

Results for the Fourth Quarter Calendar Year 2015 Tank 50H Salt Solution Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Crawford, C.

In this memorandum, the chemical and radionuclide contaminant results from the Fourth Quarter Calendar Year 2015 (CY15) sample of Tank 50H salt solution are presented in tabulated form. The Fourth Quarter CY15 Tank 50H samples were obtained on October 29, 2015 and received at Savannah River National Laboratory (SRNL) on October 30, 2015. The information from this characterization will be used by Defense Waste Processing Facility (DWPF) & Saltstone Facility Engineering for the transfer of aqueous waste from Tank 50H to the Salt Feed Tank in the Saltstone Production Facility, where the waste will be treated and disposed of inmore » the Saltstone Disposal Facility. This memorandum compares results, where applicable, to Saltstone Waste Acceptance Criteria (WAC) limits and targets. Data pertaining to the regulatory limits for Resource Conservation and Recovery Act (RCRA) metals will be documented at a later time per the Task Technical and Quality Assurance Plan (TTQAP) for the Tank 50H saltstone task. The chemical and radionuclide contaminant results from the characterization of the Fourth Quarter Calendar Year 2015 (CY15) sampling of Tank 50H were requested by SRR personnel and details of the testing are presented in the SRNL Task Technical and Quality Assurance Plan.« less

Tank 40 Final SB7b Chemical Characterization Results

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.

2012-11-06

A sample of Sludge Batch 7b (SB7b) was taken from Tank 40 in order to obtain radionuclide inventory analyses necessary for compliance with the Waste Acceptance Product Specifications (WAPS). The SB7b WAPS sample was also analyzed for chemical composition including noble metals and fissile constituents. At the Savannah River National Laboratory (SRNL) the 3-L Tank 40 SB7b sample was transferred from the shipping container into a 4-L high density polyethylene bottle and solids were allowed to settle over the weekend. Supernate was then siphoned off and circulated through the shipping container to complete the transfer of the sample. Following thoroughmore » mixing of the 3-L sample, a 558 g sub-sample was removed. This sub-sample was then utilized for all subsequent analytical samples. Eight separate aliquots of the slurry were digested, four with HNO{sub 3}/HCl (aqua regia) in sealed Teflon vessels and four with NaOH/Na{sub 2}O{sub 2} (alkali or peroxide fusion) using Zr crucibles. Two Analytical Reference Glass ? 1 (ARG-1) standards were digested along with a blank for each preparation. Each aqua regia digestion and blank was diluted to 1:100 mL with deionized water and submitted to Analytical Development (AD) for inductively coupled plasma ? atomic emission spectroscopy (ICP-AES) analysis, inductively coupled plasma ? mass spectrometry (ICP-MS) analysis, atomic absorption spectroscopy (AA) for As and Se, and cold vapor atomic absorption spectroscopy (CV-AA) for Hg. Equivalent dilutions of the alkali fusion digestions and blank were submitted to AD for ICP-AES analysis. Tank 40 SB7b supernate was collected from a mixed slurry sample in the SRNL Shielded Cells and submitted to AD for ICP-AES, ion chromatography (IC), total base/free OH{sup -}/other base, total inorganic carbon/total organic carbon (TIC/TOC) analyses, and Cs-137 gamma scan. Weighted dilutions of slurry were submitted for IC, TIC/TOC, and total base/free OH-/other base analyses. Activities for U-233, U-235, and Pu-239 were determined from the ICP-MS data for the aqua regia digestions of the Tank 40 WAPS slurry using the specific activity of each isotope. The Pu-241 value was determined from a Pu-238/-241 method.« less

ELIMINATION OF THE CHARACTERIZATION OF DWPF POUR STREAM SAMPLE AND THE GLASS FABRICATION AND TESTING OF THE DWPF SLUDGE BATCH QUALIFICATION SAMPLE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Amoroso, J.; Peeler, D.; Edwards, T.

2012-05-11

A recommendation to eliminate all characterization of pour stream glass samples and the glass fabrication and Product Consistency Test (PCT) of the sludge batch qualification sample was made by a Six-Sigma team chartered to eliminate non-value-added activities for the Defense Waste Processing Facility (DWPF) sludge batch qualification program and is documented in the report SS-PIP-2006-00030. That recommendation was supported through a technical data review by the Savannah River National Laboratory (SRNL) and is documented in the memorandums SRNL-PSE-2007-00079 and SRNL-PSE-2007-00080. At the time of writing those memorandums, the DWPF was processing sludge-only waste but, has since transitioned to a coupledmore » operation (sludge and salt). The SRNL was recently tasked to perform a similar data review relevant to coupled operations and re-evaluate the previous recommendations. This report evaluates the validity of eliminating the characterization of pour stream glass samples and the glass fabrication and Product Consistency Test (PCT) of the sludge batch qualification samples based on sludge-only and coupled operations. The pour stream sample has confirmed the DWPF's ability to produce an acceptable waste form from Slurry Mix Evaporator (SME) blending and product composition/durability predictions for the previous sixteen years but, ultimately the pour stream analysis has added minimal value to the DWPF's waste qualification strategy. Similarly, the information gained from the glass fabrication and PCT of the sludge batch qualification sample was determined to add minimal value to the waste qualification strategy since that sample is routinely not representative of the waste composition ultimately processed at the DWPF due to blending and salt processing considerations. Moreover, the qualification process has repeatedly confirmed minimal differences in glass behavior from actual radioactive waste to glasses fabricated from simulants or batch chemicals. In contrast, the variability study has significantly added value to the DWPF's qualification strategy. The variability study has evolved to become the primary aspect of the DWPF's compliance strategy as it has been shown to be versatile and capable of adapting to the DWPF's various and diverse waste streams and blending strategies. The variability study, which aims to ensure durability requirements and the PCT and chemical composition correlations are valid for the compositional region to be processed at the DWPF, must continue to be performed. Due to the importance of the variability study and its place in the DWPF's qualification strategy, it will also be discussed in this report. An analysis of historical data and Production Records indicated that the recommendation of the Six Sigma team to eliminate all characterization of pour stream glass samples and the glass fabrication and PCT performed with the qualification glass does not compromise the DWPF's current compliance plan. Furthermore, the DWPF should continue to produce an acceptable waste form following the remaining elements of the Glass Product Control Program; regardless of a sludge-only or coupled operations strategy. If the DWPF does decide to eliminate the characterization of pour stream samples, pour stream samples should continue to be collected for archival reasons, which would allow testing to be performed should any issues arise or new repository test methods be developed.« less

SRNL Tagging and Tracking Video

DOE Office of Scientific and Technical Information (OSTI.GOV)

None

SRNL generates a next generation satellite base tracking system. The tagging and tracking system can work in remote wilderness areas, inside buildings, underground and other areas not well served by traditional GPS. It’s a perfect response to customer needs and market demand.

DOE Office of Scientific and Technical Information (OSTI.GOV)

French, T

The Laboratory Director is pleased to have the opportunity to present the 2008 Laboratory Directed Research and Development (LDRD) annual report. This is my first opportunity to do so, and only the second such report that has been issued. As will be obvious, SRNL has built upon the excellent start that was made with the LDRD program last year, and researchers have broken new ground in some important areas. In reviewing the output of this program this year, it is clear that the researchers implemented their ideas with creativity, skill and enthusiasm. It is gratifying to see this level ofmore » participation, because the LDRD program remains a key part of meeting SRNL's and DOE's strategic goals, and helps lay a solid scientific foundation for SRNL as the premier applied science laboratory. I also believe that the LDRD program's results this year have demonstrated SRNL's value as the EM Corporate Laboratory, having advanced knowledge in a spectrum of areas, including reduction of the technical risks of cleanup, separations science, packaging and transportation of nuclear materials, and many others. The research in support of Energy Security and National and Homeland Security has been no less notable. SRNL' s researchers have shown again that the nascent LDRD program is a sound investment for DOE that will pay off handsomely for the nation as time goes on.« less

Characterization Results for the January 2017 H-Tank Farm 2H Evaporator Overhead Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Truong, T.; Nicholson, J.

2017-04-11

This report contains the radioanalytical results of the 2H evaporator overhead sample received at SRNL on January 19, 2017. Specifically, concentrations of 137Cs, 90Sr, and 129I are reported and compared to the corresponding Waste Acceptance Criteria (WAC) limits of the Effluent Treatment Project (ETP) Waste Water Collection Tank (WWCT) (rev. 6). All of the radionuclide concentrations in the sample were found to be in compliance with the ETP WAC limits.

Characterization Results for the March 2016 H-Tank Farm 2H Evaporator Overhead Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nicholson, J. C.

2016-05-09

This report contains the radioanalytical results of the 2H evaporator overhead sample received at SRNL on March 16, 2016. Specifically, concentrations of 137Cs, 90Sr, and 129I are reported and compared to the corresponding Waste Acceptance Criteria (WAC) limits of the Effluent Treatment Project (ETP) Waste Water Collection Tank (WWCT) (rev. 6). All of the radionuclide concentrations in the sample were found to be in compliance with the ETP WAC limits.

Antifoam Degradation Products in Off Gas and Condensate of Sludge Batch 9 Simulant Nitric-Formic Flowsheet Testing for the Defense Waste Processing Facility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, T.

Ten chemical processing cell (CPC) experiments were performed using simulant to evaluate Sludge Batch 9 for sludge-only and coupled processing using the nitric-formic flowsheet in the Defense Waste Processing Facility (DWPF). Sludge Receipt and Adjustment Tank (SRAT) and Slurry Mix Evaporator (SME) cycles were performed on eight of the ten. The other two were SRAT cycles only. Samples of the condensate, sludge, and off gas were taken to monitor the chemistry of the CPC experiments. The Savannah River National Laboratory (SRNL) has previously shown antifoam decomposes to form flammable organic products, (hexamethyldisiloxane (HMDSO), trimethylsilanol (TMS), and propanal), that are presentmore » in the vapor phase and condensate of the CPC vessels. To minimize antifoam degradation product formation, a new antifoam addition strategy was implemented at SRNL and DWPF to add antifoam undiluted.« less

REACTOR PHYSICS MODELING OF SPENT RESEARCH REACTOR FUEL FOR TECHNICAL NUCLEAR FORENSICS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nichols, T.; Beals, D.; Sternat, M.

2011-07-18

Technical nuclear forensics (TNF) refers to the collection, analysis and evaluation of pre- and post-detonation radiological or nuclear materials, devices, and/or debris. TNF is an integral component, complementing traditional forensics and investigative work, to help enable the attribution of discovered radiological or nuclear material. Research is needed to improve the capabilities of TNF. One research area of interest is determining the isotopic signatures of research reactors. Research reactors are a potential source of both radiological and nuclear material. Research reactors are often the least safeguarded type of reactor; they vary greatly in size, fuel type, enrichment, power, and burn-up. Manymore » research reactors are fueled with highly-enriched uranium (HEU), up to {approx}93% {sup 235}U, which could potentially be used as weapons material. All of them have significant amounts of radiological material with which a radioactive dispersal device (RDD) could be built. Therefore, the ability to attribute if material originated from or was produced in a specific research reactor is an important tool in providing for the security of the United States. Currently there are approximately 237 operating research reactors worldwide, another 12 are in temporary shutdown and 224 research reactors are reported as shut down. Little is currently known about the isotopic signatures of spent research reactor fuel. An effort is underway at Savannah River National Laboratory (SRNL) to analyze spent research reactor fuel to determine these signatures. Computer models, using reactor physics codes, are being compared to the measured analytes in the spent fuel. This allows for improving the reactor physics codes in modeling research reactors for the purpose of nuclear forensics. Currently the Oak Ridge Research reactor (ORR) is being modeled and fuel samples are being analyzed for comparison. Samples of an ORR spent fuel assembly were taken by SRNL for analytical and radiochemical analysis. The fuel assembly was modeled using MONTEBURNS(MCNP5/ ORIGEN2.2) and MCNPX/CINDER90. The results from the models have been compared to each other and to the measured data.« less

Solvent Hold Tank Sample Results for MCU-16-1247-1248-1249: August 2016 Monthly Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Jones, D. H.

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-1247-1248-1249), pulled on 08/22/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-1247-1248-1249 indicated the Isopar™L concentration is above its nominal level (101%). The extractant (MaxCalix) and the modifier (CS-7SB) are 7% and 9 % below their nominal concentrations. The suppressor (TiDG) is 63% below its nominal concentration. This analysis confirms the solvent may require the addition of TiDG, and possibly of modifier and MaxCalix to restore then to nominal levels. Based on the current monthly sample, the levelsmore » of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended. At the time of writing this report, A solvent trim batch containing TiDG, modifier and MaxCalix, was added to the SHT (October 2016) and expect the concentration of these components to be at their nominal values.« less

SRNL Tagging and Tracking Video

ScienceCinema

None

2018-01-16

SRNL generates a next generation satellite base tracking system. The tagging and tracking system can work in remote wilderness areas, inside buildings, underground and other areas not well served by traditional GPS. It’s a perfect response to customer needs and market demand.

Edwards nXDS15iC Vacuum Scroll Pump Pressure Testing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sessions, H.; Morgan, G. A.

2013-07-17

The SRNL High Pressure Laboratory performed testing on an Edwards Model nXDS15iC Vacuum Scroll Pump on July 10th and 11th of 2013 at 723-A. This testing was done in an attempt to obtain initial compression ratio information for the nXDS15iC pump, with compression ratio defined as discharge pressure of the pump divided by suction pressure. Pressure burst testing was also done on the pump to determine its design pressure for pressure safety reasons. The Edwards nXDS15iC pump is being evaluated by SRNL for use part of the SHINE project being executed by SRNL.

Results for the DWPF Slurry Mix Evaporator Condensate Tank, Off Gas Condensate Tank, And Recycle Collection Tank Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

TERRI, FELLINGER

2004-12-21

The Defense Waste Processing Facility, DWPF, currently generates approximately 1.4 million gallons of recycle water per year during Sludge-Only operations. DWPF has minimized condensate generation to 1.4 million gallons by not operating the Steam Atomized Scrubbers, SASs, for the melter off gas system. By not operating the SASs, DWPF has reduced the total volume by approximately 800,000 gallons of condensate per year. Currently, the recycle stream is sent to back to the Tank Farm and processed through the 2H Evaporator system. To alleviate the load on the 2H Evaporator system, an acid evaporator design is being considered as an alternatemore » processing and/or concentration method for the DWPF recycle stream. In order to support this alternate processing option, the DWPF has requested that the chemical and radionuclide compositions of the Off Gas Condensate Tank, OGCT, Slurry Mix Evaporator Condensate Tank, SMECT, Recycle Collection Tank, RCT, and the Decontamination Waste Treatment Tank, DWTT, be determined as a part of the process development work for the acid evaporator design. Samples have been retrieved from the OGCT, RCT, and SMECT and have been sent to the Savannah River National Laboratory, SRNL for this characterization. The DWTT samples have been recently shipped to SRNL. The results for the DWTT samples will be issued at later date.« less

Results For The Third Quarter Calendar Year 2016 Tank 50H Salt Solution Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Crawford, C.

2016-10-13

In this memorandum, the chemical and radionuclide contaminant results from the Third Quarter Calendar Year 2016 (CY16) sample of Tank 50H salt solution are presented in tabulated form. The Third Quarter CY16 Tank 50H samples (a 200 mL sample obtained 6” below the surface (HTF-5-16-63) and a 1 L sample obtained 66” from the tank bottom (HTF-50-16-64)) were obtained on July 14, 2016 and received at Savannah River National Laboratory (SRNL) on the same day. Prior to obtaining the samples from Tank 50H, a single pump was run at least 4.4 hours, and the samples were pulled immediately after pumpmore » shut down. The information from this characterization will be used by Defense Waste Processing Facility (DWPF) & Saltstone Facility Engineering for the transfer of aqueous waste from Tank 50H to the Saltstone Production Facility, where the waste will be treated and disposed of in the Saltstone Disposal Facility. This memorandum compares results, where applicable, to Saltstone Waste Acceptance Criteria (WAC) limits and targets. Data pertaining to the regulatory limits for Resource Conservation and Recovery Act (RCRA) metals will be documented at a later time per the Task Technical and Quality Assurance Plan (TTQAP) for the Tank 50H saltstone task. The chemical and radionuclide contaminant results from the characterization of the Third Quarter CY16 sampling of Tank 50H were requested by Savannah River Remediation (SRR) personnel and details of the testing are presented in the SRNL TTQAP.« less

VERIFICATION OF THE DEFENSE WASTE PROCESSING FACILITY PROCESS DIGESTION METHOD FOR THE SLUDGE BATCH 6 QUALIFICATION SAMPLE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Click, D.; Jones, M.; Edwards, T.

2010-06-09

For each sludge batch that is processed in the Defense Waste Processing Facility (DWPF), the Savannah River National Laboratory (SRNL) confirms applicability of the digestion method to be used by the DWPF lab for elemental analysis of Sludge Receipt and Adjustment Tank (SRAT) receipt samples and SRAT product process control samples.1 DWPF SRAT samples are typically dissolved using a room temperature HF-HNO3 acid dissolution (i.e., DWPF Cold Chem (CC) Method, see DWPF Procedure SW4-15.201) and then analyzed by inductively coupled plasma - atomic emission spectroscopy (ICPAES). In addition to the CC method confirmation, the DWPF lab's mercury (Hg) digestion methodmore » was also evaluated for applicability to SB6 (see DWPF procedure 'Mercury System Operating Manual', Manual: SW4-15.204. Section 6.1, Revision 5, Effective date: 12-04-03). This report contains the results and comparison of data generated from performing the Aqua Regia (AR), Sodium Peroxide/Hydroxide Fusion (PF) and DWPF Cold Chem (CC) method digestion of Sludge Batch 6 (SB6) SRAT Receipt and SB6 SRAT Product samples. For validation of the DWPF lab's Hg method, only SRAT receipt material was used and compared to AR digestion results. The SB6 SRAT Receipt and SB6 SRAT Product samples were prepared in the SRNL Shielded Cells, and the SRAT Receipt material is representative of the sludge that constitutes the SB6 Batch or qualification composition. This is the sludge in Tank 51 that is to be transferred into Tank 40, which will contain the heel of Sludge Batch 5 (SB5), to form the SB6 Blend composition. In addition to the 16 elements currently measured by the DWPF, this report includes Hg and thorium (Th) data (Th comprising {approx}2.5 - 3 Wt% of the total solids in SRAT Receipt and SRAT Product, respectively) and provides specific details of ICP-AES analysis of Th. Thorium was found to interfere with the U 367.007 nm emission line, and an inter-element correction (IEC) had to be applied to U data, which is also discussed. The results for any one particular element should not be used in any way to identify the form or speciation of a particular element without support from XRD analysis or used to estimate ratios of compounds in the sludge.« less

Results for the first quarter calendar year 2017 tank 50H salt solution sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Crawford, C. L.

2017-04-12

In this memorandum, the chemical and radionuclide contaminant results from the First Quarter Calendar Year 2017 (CY17) sample of Tank 50H salt solution are presented in tabulated form. The First Quarter CY17 Tank 50H samples [a 200 mL sample obtained 6” below the surface (HTF-50-17-7) and a 1 L sample obtained 66” from the tank bottom (HTF-50-17-8)] were obtained on January 15, 2017 and received at Savannah River National Laboratory (SRNL) on January 16, 2017. Prior to obtaining the samples from Tank 50H, a single pump was run at least 4.4 hours and the samples were pulled immediately after pumpmore » shut down. All volatile organic analysis (VOA) and semi-volatile organic analysis (SVOA) were performed on the surface sample and all other analyses were performed on the variable depth sample. The information from this characterization will be used by Savannah River Remediation (SRR) for the transfer of aqueous waste from Tank 50H to the Saltstone Production Facility, where the waste will be treated and disposed of in the Saltstone Disposal Facility. This memorandum compares results, where applicable, to Saltstone Waste Acceptance Criteria (WAC) limits and targets. The chemical and radionuclide contaminant results from the characterization of the First Quarter CY17 sampling of Tank 50H were requested by SRR personnel and details of the testing are presented in the SRNL Task Technical and Quality Assurance Plan (TTQAP). This memorandum is part of Deliverable 2 from SRR request. Data pertaining to the regulatory limits for Resource Conservation and Recovery Act (RCRA) metals will be documented at a later time per the TTQAP for the Tank 50H saltstone task.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Martino, C

The Department of Energy (DOE) recognizes the need for the characterization of High-Level Waste (HLW) saltcake in the Savannah River Site (SRS) F- and H-area tank farms to support upcoming salt processing activities. As part of the enhanced characterization efforts, Tank 25F will be sampled and the samples analyzed at the Savannah River National Laboratory (SRNL). This Task Technical and Quality Assurance Plan documents the planned activities for the physical, chemical, and radiological analysis of the Tank 25F saltcake core samples. This plan does not cover other characterization activities that do not involve core sample analysis and it does notmore » address issues regarding sampling or sample transportation. The objectives of this report are: (1) Provide information useful in projecting the composition of dissolved salt batches by quantifying important components (such as actinides, {sup 137}Cs, and {sup 90}Sr) on a per batch basis. This will assist in process selection for the treatment of salt batches and provide data for the validation of dissolution modeling. (2) Determine the properties of the heel resulting from dissolution of the bulk saltcake. Also note tendencies toward post-mixing precipitation. (3) Provide a basis for determining the number of samples needed for the characterization of future saltcake tanks. Gather information useful towards performing characterization in a manner that is more cost and time effective.« less

Argon Collection And Purification For Proliferation Detection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Achey, R.; Hunter, D.

2015-10-09

In order to determine whether a seismic event was a declared/undeclared underground nuclear weapon test, environmental samples must be taken and analyzed for signatures that are unique to a nuclear explosion. These signatures are either particles or gases. Particle samples are routinely taken and analyzed under the Comprehensive Nuclear-Test-Ban Treaty Organization (CTBTO) verification regime as well as by individual countries. Gas samples are analyzed for signature gases, especially radioactive xenon. Underground nuclear tests also produce radioactive argon, but that signature is not well monitored. A radioactive argon signature, along with other signatures, can more conclusively determine whether an event wasmore » a nuclear test. This project has developed capabilities for collecting and purifying argon samples for ultra-low-background proportional counting. SRNL has developed a continuous gas enrichment system that produces an output stream containing 97% argon from whole air using adsorbent separation technology (the flow diagram for the system is shown in the figure). The vacuum swing adsorption (VSA) enrichment system is easily scalable to produce ten liters or more of 97% argon within twelve hours. A gas chromatographic separation using a column of modified hydrogen mordenite molecular sieve has been developed that can further purify the sample to better than 99% purity after separation from the helium carrier gas. The combination of these concentration and purification systems has the capability of being used for a field-deployable system for collecting argon samples suitable for ultra-low-background proportional counting for detecting nuclear detonations under the On-Site Inspection program of the CTBTO verification regime. The technology also has applications for the bulk argon separation from air for industrial purposes such as the semi-conductor industry.« less

Fluidized bed steam reformed mineral waste form performance testing to support Hanford Supplemental Low Activity Waste Immobilization Technology Selection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jantzen, C. M.; Pierce, E. M.; Bannochie, C. J.

This report describes the benchscale testing with simulant and radioactive Hanford Tank Blends, mineral product characterization and testing, and monolith testing and characterization. These projects were funded by DOE EM-31 Technology Development & Deployment (TDD) Program Technical Task Plan WP-5.2.1-2010-001 and are entitled “Fluidized Bed Steam Reformer Low-Level Waste Form Qualification”, Inter-Entity Work Order (IEWO) M0SRV00054 with Washington River Protection Solutions (WRPS) entitled “Fluidized Bed Steam Reforming Treatability Studies Using Savannah River Site (SRS) Low Activity Waste and Hanford Low Activity Waste Tank Samples”, and IEWO M0SRV00080, “Fluidized Bed Steam Reforming Waste Form Qualification Testing Using SRS Low Activity Wastemore » and Hanford Low Activity Waste Tank Samples”. This was a multi-organizational program that included Savannah River National Laboratory (SRNL), THOR® Treatment Technologies (TTT), Pacific Northwest National Laboratory (PNNL), Oak Ridge National Laboratory (ORNL), Office of River Protection (ORP), and Washington River Protection Solutions (WRPS). The SRNL testing of the non-radioactive pilot-scale Fluidized Bed Steam Reformer (FBSR) products made by TTT, subsequent SRNL monolith formulation and testing and studies of these products, and SRNL Waste Treatment Plant Secondary Waste (WTP-SW) radioactive campaign were funded by DOE Advanced Remediation Technologies (ART) Phase 2 Project in connection with a Work-For-Others (WFO) between SRNL and TTT.« less

Characterization results for the October 2015-Tank for farm 3H evaporator overhead examples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nicholson, J. C.

2016-01-28

This report contains the radioanalytical results of the 3H evaporator overhead sample received at SRNL on October 13, 2015. Specifically, concentrations of 137Cs, 90Sr, and 129I are reported and compared to the corresponding Waste Acceptance Criteria (WAC) limits of the Effluent Treatment Project (ETP) Waste Water Collection Tank (WWCT) (rev. 6). All of the radionuclide concentrations in the sample were found to be in compliance with the ETP WAC limits.

Results of Hg speciation testing on DWPF SMECT-4, SMECT-6, and RCT-2 samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.

2016-02-04

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team.i,ii The fifteenth shipment of samples was designated to include Defense Waste Processing Facility (DWPF) Slurry Mix Evaporator Condensate Tank (SMECT) samples from Sludge Receipt and Adjustment Tank (SRAT) Batch 738 and a Recycle Condensate Tank (RCT) sample from SRAT Batch 736. The DWPF sample designations for the three samples analyzed are provided in Table 1. The Batch 738 ‘Baseline’ SMECT sample was taken priormore » to Precipitate Reactor Feed Tank (PRFT) addition and concentration and therefore, precedes the SMECT-5 sample reported previously. iii The Batch 738 ‘End of SRAT Cycle’ SMECT sample was taken at the conclusion of SRAT operations for this batch (PRFT addition/concentration, acid additions, initial concentration, MCU addition, and steam stripping). Batch 738 experienced a sludge slurry carryover event, which introduced sludge solids to the SMECT that were particularly evident in the SMECT-5 sample, but less evident in the ‘End of SRAT Cycle’ SMECT-6 sample. The Batch 736 ‘After SME’ RCT sample was taken after completion of SMECT transfers at the end of the SME cycle.« less

Rapid determination of 226Ra in environmental samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, Sherrod L.; Culligan, Brian K.

A new rapid method for the determination of {sup 228}Ra in natural water samples has been developed at the SRNL/EBL (Savannah River National Lab/ Environmental Bioassay Laboratory) that can be used for emergency response or routine samples. While gamma spectrometry can be employed with sufficient detection limits to determine {sup 228}Ra in solid samples (via {sup 228}Ac) , radiochemical methods that employ gas flow proportional counting techniques typically provide lower MDA (Minimal Detectable Activity) levels for the determination of {sup 228}Ra in water samples. Most radiochemical methods for {sup 228}Ra collect and purify {sup 228}Ra and allow for {sup 228}Acmore » daughter ingrowth for ~36 hours. In this new SRNL/EBL approach, {sup 228}Ac is collected and purified from the water sample without waiting to eliminate this delay. The sample preparation requires only about 4 hours so that {sup 228}Ra assay results on water samples can be achieved in < 6 hours. The method uses a rapid calcium carbonate precipitation enhanced with a small amount of phosphate added to enhance chemical yields (typically >90%), followed by rapid cation exchange removal of calcium. Lead, bismuth, uranium, thorium and protactinium isotopes are also removed by the cation exchange separation. {sup 228}Ac is eluted from the cation resin directly onto a DGA Resin cartridge attached to the bottom of the cation column to purify {sup 228}Ac. DGA Resin also removes lead and bismuth isotopes, along with Sr isotopes and {sup 90}Y. La is used to determine {sup 228}Ac chemical yield via ICP-MS, but {sup 133}Ba can also be used instead if ICP-MS assay is not available. Unlike some older methods, no lead or strontium holdback carriers or continual readjustment of sample pH is required.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Campbell, Sam; Dam, Wiliam

In 2012, the U.S.Department of Energy (DOE) began reassessing the former Riverton, Wyoming, Processing Site area for potential contaminant sources impacting groundwater. A flood in 2010 along the Little Wind River resulted in increases in groundwater contamination (DOE 2013).This investigation is a small part of continued efforts by DOE and other stakeholders to update human health and ecological risk assessments, to make a comprehensive examination of all exposure pathways to ensure that the site remains protective through established institutional controls. During field inspections at the Riverton Site in 2013, a white evaporitic mineral deposit was identified along the bank ofmore » the Little Wind River within the discharge zone of the groundwater contamination plume. In December 2013, Savannah River National Laboratory (SRNL) personnel collected a sample for analysis by X-ray fluorescence (Figure 1 shows the type of material sampled). The sample had a uranium concentration of approximately 64 to 73 parts per million. Although the uranium in this mineral deposit is within the expected range for evaporatic minerals in the western United States (SRNL 2014), DOE determined that additional assessment of the mineral deposit was warranted. In response to the initial collection and analysis of a sample of the mineral deposit, DOE developed a work plan (Work Plan to Sample Mineral Deposits Along the Little Wind River, Riverton, Wyoming, Processing Site [DOE 2014]) to further define the extent of these mineral deposits and the concentration of the associated contaminants (Appendix A). The work plan addressed field reconnaissance, mapping, sampling, and the assessment of risk associated with the mineral deposits adjacent to the Little Wind River.« less

FY16 Annual Accomplishments - Waste Form Development and Performance: Evaluation Of Ceramic Waste Forms - Comparison Of Hot Isostatic Pressed And Melt Processed Fabrication Methods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Amoroso, J.; Dandeneau, C.

FY16 efforts were focused on direct comparison of multi-phase ceramic waste forms produced via melt processing and HIP methods. Based on promising waste form compositions previously devised at SRNL, simulant material was prepared at SRNL and a portion was sent to the Australian Nuclear Science and Technology Organization (ANSTO) for HIP treatments, while the remainder of the material was melt processed at SRNL. The microstructure, phase formation, elemental speciation, and leach behavior, and radiation stability of the fabricated ceramics was performed. In addition, melt-processed ceramics designed with different fractions of hollandite, zirconolite, perovskite, and pyrochlore phases were investigated. for performancemore » and properties.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F.; Taylor-Pashow, K.

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-15-556, MCU-15-557, and MCU-15-558), pulled on 03/16/2015 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-15-556-557-558 indicated a low concentration (~ 78 % of nominal) of the suppressor (TiDG) and concentrations of the extractant (MaxCalix), and of the modifier (CS-7SB) in the solvent that were slightly lower than nominal. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent in February 2015. Based on the current monthly sample, the levels of TiDG, MaxCalix, and modifier aremore » sufficient for continuing operation without adding a trim at this time. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). However, the p-nut vials that delivered the samples contained small (1 mm) droplets of oxidized modifier and amides (as detected by the FTIR analysis). In addition, up to 21 microgram of mercury per gram of solvent (or 17.4 µg/mL) was detected in this sample. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.« less

TRACE ELEMENT ANALYSES OF URANIUM MATERIALS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Beals, D; Charles Shick, C

The Savannah River National Laboratory (SRNL) has developed an analytical method to measure many trace elements in a variety of uranium materials at the high part-per-billion (ppb) to low part-per-million (ppm) levels using matrix removal and analysis by quadrapole ICP-MS. Over 35 elements were measured in uranium oxides, acetate, ore and metal. Replicate analyses of samples did provide precise results however none of the materials was certified for trace element content thus no measure of the accuracy could be made. The DOE New Brunswick Laboratory (NBL) does provide a Certified Reference Material (CRM) that has provisional values for a seriesmore » of trace elements. The NBL CRM were purchased and analyzed to determine the accuracy of the method for the analysis of trace elements in uranium oxide. These results are presented and discussed in the following paper.« less

ISOLOK VALVE ACCEPTANCE TESTING FOR DWPF SME SAMPLING PROCESS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edwards, T.; Hera, K.; Coleman, C.

2011-12-05

Evaluation of the Defense Waste Processing Facility (DWPF) Chemical Process Cell (CPC) cycle time identified several opportunities to improve the CPC processing time. Of the opportunities, a focus area related to optimizing the equipment and efficiency of the sample turnaround time for DWPF Analytical Laboratory was identified. The Mechanical Systems & Custom Equipment Development (MS&CED) Section of the Savannah River National Laboratory (SRNL) evaluated the possibility of using an Isolok{reg_sign} sampling valve as an alternative to the Hydragard{reg_sign} valve for taking process samples. Previous viability testing was conducted with favorable results using the Isolok sampler and reported in SRNL-STI-2010-00749 (1).more » This task has the potential to improve operability, reduce maintenance time and decrease CPC cycle time. This report summarizes the results from acceptance testing which was requested in Task Technical Request (TTR) HLW-DWPF-TTR-2010-0036 (2) and which was conducted as outlined in Task Technical and Quality Assurance Plan (TTQAP) SRNL-RP-2011-00145 (3). The Isolok to be tested is the same model which was tested, qualified, and installed in the Sludge Receipt Adjustment Tank (SRAT) sample system. RW-0333P QA requirements apply to this task. This task was to qualify the Isolok sampler for use in the DWPF Slurry Mix Evaporator (SME) sampling process. The Hydragard, which is the current baseline sampling method, was used for comparison to the Isolok sampling data. The Isolok sampler is an air powered grab sampler used to 'pull' a sample volume from a process line. The operation of the sampler is shown in Figure 1. The image on the left shows the Isolok's spool extended into the process line and the image on the right shows the sampler retracted and then dispensing the liquid into the sampling container. To determine tank homogeneity, a Coliwasa sampler was used to grab samples at a high and low location within the mixing tank. Data from the two locations were compared to determine if the contents of the tank were well mixed. The Coliwasa sampler is a tube with a stopper at the bottom and is designed to obtain grab samples from specific locations within the drum contents. A position paper (4) was issued to address the prototypic flow loop issues and simulant selections. A statistically designed plan (5) was issued to address the total number of samples each sampler needed to pull, to provide the random order in which samples were pulled and to group samples for elemental analysis. The TTR required that the Isolok sampler perform as well as the Hydragard sampler during these tests to ensure the acceptability of the Isolok sampler for use in the DWPF sampling cells. Procedure No.L9.4-5015 was used to document the sample parameters and process steps. Completed procedures are located in R&D Engineering job folder 23269.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Skibo, A.

SRNL has considerable experience in designing, engineering, and operating systems for removing iodine-129 (I-129) and ruthenium-106 (Ru-106) from waste streams that are directly analogous to the Advanced Liquid Processing System (ALPS) waste streams. SRNL proposes to provide the technical background and design and engineering support for an improved I-129 and Ru-106 removal system for application to ALPS on the Fukushima Daiichi Nuclear Power Station (NPS).

SRNL Development of Recovery Processes for Mark-18A Heavy Actinide Targets

DOE Office of Scientific and Technical Information (OSTI.GOV)

Allender, Jeffrey S.; Bridges, Nicholas J.; Loftin, Bradley M.

2015-07-14

Savannah River National Laboratory (SRNL) and Oak Ridge National Laboratory (ORNL) are developing plans for the recovery of rare and unique isotopes contained within heavy-actinide target assemblies, specifically the Mark-18A. Mark-18A assemblies were irradiated in Savannah River Site (SRS) reactors in the 1970s under extremely high neutron-flux conditions and produced, virtually, the world's supply of plutonium-244, an isotope of key importance to high-precision actinide measurement and other scientific and nonproliferation uses; and curium highly enriched in heavy isotopes (e.g., curium-246 and curium-248). In 2015 and 2016, SRNL is pursuing tasks that would reduce program risk and budget requirements, including furthermore » characterization of unprocessed targets; engineering studies for the use of the SRNL Shielded Cells Facility (SCF) for recovery; and development of onsite and offsite shipping methods including a replacement for the heavy (70 ton) cask previously used for onsite transfer of irradiated items at SRS. A status update is provided for the characterization, including modeling using the Monte Carlo N-Particle Transport Code (MCNP); direct non-destructive assay measurements; and cask design.« less

2004 Savannah River Cooling Tower Collection (U)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Garrett, Alfred; Parker, Matthew J.; Villa-Aleman, E.

2005-05-01

The Savannah River National Laboratory (SRNL) collected ground truth in and around the Savannah River Site (SRS) F-Area cooling tower during the spring and summer of 2004. The ground truth data consisted of air temperatures and humidity inside and around the cooling tower, wind speed and direction, cooling water temperatures entering; inside adn leaving the cooling tower, cooling tower fan exhaust velocities and thermal images taken from helicopters. The F-Area cooling tower had six cells, some of which were operated with fans off during long periods of the collection. The operating status (fan on or off) for each of themore » six cells was derived from operations logbooks and added to the collection database. SRNL collected the F-Area cooling tower data to produce a database suitable for validation of a cooling tower model used by one of SRNL's customer agencies. SRNL considers the data to be accurate enough for use in a model validation effort. Also, the thermal images of the cooling tower decks and throats combined with the temperature measurements inside the tower provide valuable information about the appearance of cooling towers as a function of fan operating status and time of day.« less

Rapid Radiochemical Analyses in Support of Fukushima Nuclear Accident - 13196

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, Sherrod L.; Culligan, Brian K.; Hutchison, Jay B.

There is an increasing need to develop faster analytical methods for emergency response, including emergency soil and air filter samples [1, 2]. The Savannah River National Laboratory (SRNL) performed analyses on samples received from Japan in April, 2011 as part of a U.S. Department of Energy effort to provide assistance to the government of Japan, following the nuclear event at Fukushima Daiichi, resulting from the earthquake and tsunami on March 11, 2011. Of particular concern was whether it was safe to plant rice in certain areas (prefectures) near Fukushima. The primary objectives of the sample collection, sample analysis, and datamore » assessment teams were to evaluate personnel exposure hazards, identify the nuclear power plant radiological source term and plume deposition, and assist the government of Japan in assessing any environmental and agricultural impacts associated with the nuclear event. SRNL analyzed approximately 250 samples and reported approximately 500 analytical method determinations. Samples included soil from farmland surrounding the Fukushima reactors and air monitoring samples of national interest, including those collected at the U.S. Embassy and American military bases. Samples were analyzed for a wide range of radionuclides, including strontium-89, strontium-90, gamma-emitting radionuclides, and plutonium, uranium, americium and curium isotopes. Technical aspects of the rapid soil and air filter analyses will be described. The extent of radiostrontium contamination was a significant concern. For {sup 89,90}Sr analyses on soil samples, a rapid fusion technique using 1.5 gram soil aliquots to enable a Minimum Detectable Activity (MDA) of <1 pCi {sup 89,90}Sr /g of soil was employed. This sequential technique has been published recently by this laboratory for actinides and radiostrontium in soil and vegetation [3, 4]. It consists of a rapid sodium hydroxide fusion, pre-concentration steps using iron hydroxide and calcium fluoride precipitations, followed by Sr-Resin separation and gas flow proportional counting. To achieve a lower detection limit for analysis of some of the Japanese soil samples, a 10 gram aliquot of soil was taken, acid-leached and processed with similar preconcentration chemistry. The MDA using this approach was ∼0.03 pCi/g (1.1 mBq/g)/, which is less than the 0.05-0.10 pCi/g {sup 90}Sr levels found in soil as a result of global fallout. The chemical yields observed for the Japanese soil samples was typically 75-80% and the laboratory control sample (LCS) and matrix spike (MS) results looked very good for this work Individual QC results were well within the ± 25% acceptable range and the average of these results does not show significant bias. Additional data for a radiostrontium in soil method for 50 gram samples will also be presented, which appears to be a significant step forward based on looking at the current literature, with higher chemical yields for even larger sample aliquots and lower MDA [5, 6, 7] Hou et al surveyed a wide range of separation methods for Pu in waters and environmental solid samples [8]. While there are many actinide methods in the scientific literature, few would be considered rapid due to the tedious and time-consuming steps involved. For actinide analyses in soil, a new rapid method for the determination of actinide isotopes in soil samples using both alpha spectrometry and inductively-coupled plasma mass spectrometry was employed. The new rapid soil method utilizes an acid leaching method, iron/titanium hydroxide precipitation, a lanthanum fluoride soil matrix removal step, and a rapid column separation process with TEVA Resin. The large soil matrix is removed easily and rapidly using these two simple precipitations with high chemical recoveries and effective removal of interferences. [9, 10] Vacuum box technology and rapid flow rates were used to reduce analytical time. Challenges associated with the mineral content in the volcanic soil will be discussed. Air filter samples were reported within twenty-four (24) hours of receipt using rapid techniques published previously. [11] The rapid reporting of high quality analytical data arranged through the U.S. Department of Energy Consequence Management Home Team was critical to allow the government of Japan to readily evaluate radiological impacts from the nuclear reactor incident to both personnel and the environment. SRNL employed unique rapid methods capability for radionuclides to support Japan that can also be applied to environmental, bioassay and waste management samples. New rapid radiochemical techniques for radionuclides in soil and other environmental matrices as well as some of the unique challenges associated with this work will be presented that can be used for application to environmental monitoring, environmental remediation, decommissioning and decontamination activities. (authors)« less

RAPID RADIOCHEMICAL ANALYSES IN SUPPORT OF FUKUSHIMA NUCLEAR ACCIDENT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, S.

2012-11-07

There is an increasing need to develop faster analytical methods for emergency response, including emergency soil and air filter samples. The Savannah River National Laboratory (SRNL) performed analyses on samples received from Japan in April, 2011 as part of a U.S. Department of Energy effort to provide assistance to the government of Japan, following the nuclear event at Fukushima Daiichi, resulting from the earthquake and tsunami on March 11, 2011. Of particular concern was whether it was safe to plant rice in certain areas (prefectures) near Fukushima. The primary objectives of the sample collection, sample analysis, and data assessment teamsmore » were to evaluate personnel exposure hazards, identify the nuclear power plant radiological source term and plume deposition, and assist the government of Japan in assessing any environmental and agricultural impacts associated with the nuclear event. SRNL analyzed approximately 250 samples and reported approximately 500 analytical method determinations. Samples included soil from farmland surrounding the Fukushima reactors and air monitoring samples of national interest, including those collected at the U.S. Embassy and American military bases. Samples were analyzed for a wide range of radionuclides, including strontium-89, strontium-90, gamma-emitting radionuclides, and plutonium, uranium, americium and curium isotopes. Technical aspects of the rapid soil and air filter analyses will be described. The extent of radiostrontium contamination was a significant concern. For {sup 89,90}Sr analyses on soil samples, a rapid fusion technique using 1.5 gram soil aliquots to enable a Minimum Detectable Activity (MDA) of <1 pCi {sup 89,90} Sr /g of soil was employed. This sequential technique has been published recently by this laboratory for actinides and radiostrontium in soil and vegetation. It consists of a rapid sodium hydroxide fusion, pre-concentration steps using iron hydroxide and calcium fluoride precipitations, followed by Sr-Resin separation and gas flow proportional counting. To achieve a lower detection limit for analysis of some of the Japanese soil samples, a 10 gram aliquot of soil was taken, acid-leached and processed with similar preconcentration chemistry. The MDA using this approach was ~0.03 pCi/g (1.1 mBq/g)/, which is less than the 0.05-0.10 pCi/g {sup 90}Sr levels found in soil as a result of global fallout. The chemical yields observed for the Japanese soil samples was typically 75-80% and the laboratory control sample (LCS) and matrix spike (MS) results looked very good for this work Individual QC results were well within the ± 25% acceptable range and the average of these results does not show significant bias. Additional data for a radiostrontium in soil method for 50 gram samples will also be presented, which appears to be a significant step forward based on looking at the current literature, with higher chemical yields for even larger sample aliquots and lower MDA. Hou et al surveyed a wide range of separation methods for Pu in waters and environmental solid samples. While there are many actinide methods in the scientific literature, few would be considered rapid due to the tedious and time-consuming steps involved. For actinide analyses in soil, a new rapid method for the determination of actinide isotopes in soil samples using both alpha spectrometry and inductively-coupled plasma mass spectrometry was employed. The new rapid soil method utilizes an acid leaching method, iron/titanium hydroxide precipitation, a lanthanum fluoride soil matrix removal step, and a rapid column separation process with TEVA Resin. The large soil matrix is removed easily and rapidly using these two simple precipitations with high chemical recoveries and effective removal of interferences. Vacuum box technology and rapid flow rates were used to reduce analytical time. Challenges associated with the mineral content in the volcanic soil will be discussed. Air filter samples were reported within twenty-four (24) hours of receipt using rapid techniques published previously. The rapid reporting of high quality analytical data arranged through the U.S. Department of Energy Consequence Management Home Team was critical to allow the government of Japan to readily evaluate radiological impacts from the nuclear reactor incident to both personnel and the environment. SRNL employed unique rapid methods capability for radionuclides to support Japan that can also be applied to environmental, bioassay and waste management samples. New rapid radiochemical techniques for radionuclides in soil and other environmental matrices as well as some of the unique challenges associated with this work will be presented that can be used for application to environmental monitoring, environmental remediation, decommissioning and decontamination activities.« less

Analysis of Tank 38H (HTF-38-17-52, -53) and Tank 43H (HTF-43-17-54, -55) Samples for Support of the Enrichment Control and Corrosion Control Programs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hay, M.; Coleman, C.; Diprete, D.

SRNL analyzed samples from Tank 38H and Tank 43H to support ECP and CCP. The total uranium in the Tank 38H surface sample was 41.3 mg/L while the sub-surface sample was 43.5 mg/L. The Tank 43H samples contained total uranium concentrations of 28.5 mg/L in the surface sample and 28.1 mg/L in the sub-surface sample. The U-235 percentage ranged from 0.62% to 0.63% for the Tank 38H samples and Tank 43H samples. The total uranium and percent U-235 results in the table appear slightly lower than recent Tank 38H and Tank 43H uranium measurements. The plutonium results in the tablemore » show a large difference between the surface and sub-surface sample concentrations for Tank 38H. The Tank 43H plutonium results closely match the range of values measured on previous samples. The Cs-137 results for the Tank 38H surface and sub-surface samples show similar concentrations slightly higher than the concentrations measured in recent samples. The Cs-137 results for the two Tank 43H samples also show similar concentrations within the range of values measured on previous samples. The four samples show silicon concentrations somewhat lower than the previous samples with values ranging from 124 to 168 mg/L.« less

EVALUATION OF RANGE ESTIMATES FOR TOYOTA FCHV-ADV UNDER OPEN ROAD DRIVING CONDITIONS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anton, D.; Wipke, K.; Sprik, S.

2009-07-10

The objective of this evaluation was to independently and objectively verify driving ranges of >400 miles announced by Toyota for its new advanced Fuel Cell Hybrid Vehicle (FCHV-adv) utilizing 70 MPa compressed hydrogen. To accomplish this, participants from both Savannah River National Laboratory (SRNL) and the National Renewable Energy Laboratory (NREL) witnessed and participated in a 2-vehicle evaluation with Toyota Motor Engineering & Manufacturing North America, Inc. (TEMA) over a typical open road route for over 11 hours in one day with all relevant data recorded. SRNL and TEMA first entered into discussions of verifying the range of the advancedmore » Toyota Fuel Cell Hybrid Vehicle (FCHV-adv) in August 2008 resulting from reported 400+ mile range by Toyota. After extended negotiations, a CRADA agreement, SRNS CRADA No. CR-04-003, was signed on May 6, 2009. Subsequently, on June 30, 2009 SRNL and NREL participated in an all-day evaluation of the FCHV-adv with TEMA to determine the real-world driving range of this vehicle through on-road driving on an extended round-trip drive between Torrance and San Diego, California. SRNL and NREL observed the vehicles being refueled at Toyota's headquarters the day before the evaluation in Torrance, CA on June 29. At 8:00 AM on June 30, the vehicles departed Torrance north toward downtown Los Angeles, then west to the Pacific Coast Highway, and down to San Diego. After lunch the vehicles retraced their route back to Torrance. The traffic encountered was much heavier than anticipated, causing the vehicles to not return to Torrance until 9 PM. Each vehicle was driven by the same Toyota driver all day, with one SRNL/NREL observer in each vehicle the entire route. Data was logged by Toyota and analyzed by NREL. The maximum range of the FCHV-adv vehicles was calculated to be 431 miles under these driving conditions. This distance was calculated from the actual range of 331.5 miles during over 11 hours driving, plus 99.5 miles of additional range calculated from the average fuel economy from the day times the remaining usable hydrogen. Driving range results were independently calculated for each vehicle, and these results averaged together to achieve the final 431-mile range estimate. The uncertainty on these results is relatively low due to eight independent measurements of distance and six separate measurements of hydrogen usage, with a resulting uncertainty of {+-} 7 miles ({+-} 1.7%) based on spread between the low and high values from all of the multiple measurements. The average fuel economy resulting from the day's driving was 68.3 miles/kg and the total hydrogen stored on-board at 70 MPa was calculated to be 6.31 kg. The speed profiles were analyzed and compared to standard driving cycles, and were determined to be of moderate aggressiveness. The city segments of the route had average speeds slightly greater than the UDDS cycle and the highway segments were close to the HWFET & US06 cycles. The average acceleration for the highway driving was very close to the HWFET cycle, and the city portions had average accelerations lower than the UDDS and US06 cycles. We feel that the route accurately reflects realistic driving behaviors in southern California on a typical weekday, and is an appropriate benchmark to use in the verification of a fuel cell vehicle's range.« less

Assessment of the Impact of a New Guanidine Suppressor In NGS on F/H Laboratory Analyses For DWPF and Saltstone MCU Transfers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.

2013-04-29

Implementation of the Next Generation Solvent (NGS) in the Modular Caustic-Side Solvent Extraction Unit (MCU) will now proceed with a new suppressor compound, 1,2,3-tris(3,7-dimethyloctyl)guanidine (TiDG), replacing the originally planned suppressor for NGS, 1,3-dicyclohexyl-2-(11-methyldodecyl) guanidine (DCiTG). The Savannah River National Laboratory (SRNL) was tasked with evaluating the potential impact to F/H Laboratory analyses supporting the Defense Waste Processing Facility (DWPF) Waste Acceptance Criteria (WAC) used to qualify transfers of MCU Strip Effluent (SE) into the facility and the Saltstone WAC used to qualify transfers of Tank 50 containing Decontaminated Salt Solution (DSS) from MCU into Saltstone. This assigned scope is coveredmore » by a Task Technical and Quality Assurance Plan (TTQAP). Previous impact evaluations were conducted when the DCiTG suppressor was planned for NGS and concluded that there was no impact to either the determination of MCU SE pH nor the analysis of Isopar® L carryover in the MCU SE and DSS streams. SRNL reported on this series of cross-check studies between the SRNL and F/H Laboratories. The change in suppressor from DCiTG to TiDG in the NGS should not impact the measurement of Isopar® L or pH in SE or DSS necessary to satisfy DWPF and Saltstone WAC (Tank 50) criteria, respectively. A statistical study of the low bias observed in Isopar® L measurements in both SRNL and F/H Laboratories may be necessary now that the final NGS composition is fixed in order to quantify the low bias so that a proper correction can be applied to measurements critical to the DWPF and Saltstone WACs. Depending upon the final DWPF WAC requirement put in place for SE pH, it could become necessary to implement an alternative ICP-AES measurement of boron. The current blended solvent system testing in SRNL should address any impacts to Isopar® L carryover into either the DSS or the SE. It is recommended that SRNL monitor the current blended solvent work underway with simulants in SRNL as well as any DWPF CPC testing done with the new SE stream to ascertain whether any need develops that could result in modification of any currently planned F/H Laboratory testing protocols.« less

1QCY17 Saltstone waste characterization analysis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Johnson, F. C.

2017-07-25

In the first quarter of calendar year 2017, a salt solution sample was collected from Tank 50 on January 16, 2017 in order to meet South Carolina (SC) Regulation 61-107.19 Part I C, “Solid Waste Management: Solid Waste Landfills and Structural Fill – General Requirements” and the Saltstone Disposal Facility Class 3 Landfill Permit. The Savannah River National Laboratory (SRNL) was requested to prepare and ship saltstone samples to a United States Environmental Protection Agency (EPA) certified laboratory to perform the Toxicity Characteristic Leaching Procedure (TCLP) and subsequent characterization.

Status of SRNL radiological field lysimeter experiment-Year 1

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kaplan, D.; Roberts, K.; Bagwell, L.

The Savannah River National Laboratory (SRNL) Radiological Field Lysimeter Experiment is a one-of-a-kind field facility designed to study radionuclide geochemical processes at a larger spatial scale (from grams to tens of kilograms sediment) and temporal scale (from months to 10 years) than is readily afforded through laboratory studies. The lysimeter facility is intended to capture the natural heterogeneity of moisture and temperature regimes in the vadose zone, the unsaturated subsurface region between the surface soil and the underlying aquifer. The 48 lysimeter columns, which contain various radionuclides (and stable iodine), were opened to rainfall infiltration on July 5, 2012. Themore » objective of this report is to provide a status of the lysimeter facility operations and to compile data collected during FY13, including leachate volume, rainfall, and soil moisture and temperature in situ probe data. Radiological leachate data are not presented in this document but will be the subject of a separate document.1 Leachate samples were collected quarterly and shipped to Clemson University for radiological analyses. Rainfall, leachate volume, moisture and temperature probe data were collected continuously. During operations of the facility this year, there were four safety or technical concerns that required additional maintenance: 1) radioactivity was detected in one of the overflow bottles (captured water collected from the secondary containment that does not come in contact with the radiological source material); 2) rainwater accumulated within the sample-bottle storage sheds; 3) overflow containers collected more liquid than anticipated; and 4) significant spider infestation occurred in the sample-bottle storage sheds. To address the first three concerns, each of the lysimeter columns was re-plumbed to improve and to minimize the number of joint unions. To address the fourth concern regarding spiders, new sample-bottle water sheds were purchased and a pest control program was established. During this retrofit, the lysimeters were temporarily capped (covered to preclude additional water from entering lysimeter columns) for about two months (except the four Tc-cementitious containing lysimeters, which remain capped). At a later date, data summarized in this report will be combined with the leachate radionuclide concentration data that are presently being analyzed. Together, these data can be numerically modeled to provide bench-marking information, to test hypotheses regarding hydrogeochemical conceptual models, and to estimate effective transport parameters under field conditions.« less

Solvent Hold Tank Sample Results For MCU-15-750-751-752-: June Monthly Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F.; Taylor-Pashow, K.

2015-10-07

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-15-750, MCU-15-751, and MCU-15-752), pulled on 06/22/2015 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-15-750-751-752 indicated a low concentration (~ 49 % of nominal) of the suppressor (TiDG) and slightly lower than nominal concentrations of the extractant (MaxCalix), and of the modifier (Cs-7SB) in the solvent. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent in February 2015. Based on the current monthly sample, the levels of TiDG, MaxCalix, and modifier are sufficient formore » continuing operation without adding a trim at this time but it is recommended that an addition of TiDG, modifier and Isopar™L should be made in the near future. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). In addition, up to 13.9 micrograms of mercury per gram of solvent (or 11.5 µg/mL) was detected in this sample. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.« less

Results Of Routine Strip Effluent Hold Tank, Decontaminated Salt Solution Hold Tank, Caustic Wash Tank And Caustic Storage Tank Samples From Modular Caustic-Side Solvent Extraction Unit During Macrobatch 6 Operations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.

Strip Effluent Hold Tank (SEHT), Decontaminated Salt Solution Hold Tank (DSSHT), Caustic Wash Tank (CWT) and Caustic Storage Tank (CST) samples from several of the ''microbatches'' of Integrated Salt Disposition Project (ISDP) Salt Batch (''Macrobatch'') 6 have been analyzed for {sup 238}Pu, {sup 90}Sr, {sup 137}Cs, and by Inductively Coupled Plasma Emission Spectroscopy (ICPES). The results from the current microbatch samples are similar to those from comparable samples in Macrobatch 5. From a bulk chemical point of view, the ICPES results do not vary considerably between this and the previous macrobatch. The titanium results in the DSSHT samples continue tomore » indicate the presence of Ti, when the feed material does not have detectable levels. This most likely indicates that leaching of Ti from MST in ARP continues to occur. Both the CST and CWT samples indicate that the target Free OH value of 0.03 has been surpassed. While at this time there is no indication that this has caused an operational problem, the CST should be adjusted into specification. The {sup 137}Cs results from the SRNL as well as F/H lab data indicate a potential decline in cesium decontamination factor. Further samples will be carefully monitored to investigate this.« less

SRNL PARTICIPATION IN THE MULTI-SCALE ENSEMBLE EXERCISES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Buckley, R

2007-10-29

Consequence assessment during emergency response often requires atmospheric transport and dispersion modeling to guide decision making. A statistical analysis of the ensemble of results from several models is a useful way of estimating the uncertainty for a given forecast. ENSEMBLE is a European Union program that utilizes an internet-based system to ingest transport results from numerous modeling agencies. A recent set of exercises required output on three distinct spatial and temporal scales. The Savannah River National Laboratory (SRNL) uses a regional prognostic model nested within a larger-scale synoptic model to generate the meteorological conditions which are in turn used inmore » a Lagrangian particle dispersion model. A discussion of SRNL participation in these exercises is given, with particular emphasis on requirements for provision of results in a timely manner with regard to the various spatial scales.« less

Utilization of SRNL-developed radiation-resistant polymer in high radiation environments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Skibo, A.

The radiation-resistant polymer developed by the Savannah River National Laboratory is adaptable for multiple applications to enhance polymer endurance and effectiveness in radiation environments. SRNL offers to collaborate with TEPCO in evaluation, testing, and utilization of SRNL’s radiation-resistant polymer in the D&D of the Fukushima Daiichi NPS. Refinement of the scope and associated costs will be conducted in consultation with TECPO.

ANALYSIS OF 2H-EVAPORATOR SCALE WALL [HTF-13-82] AND POT BOTTOM [HTF-13-77] SAMPLES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oji, L.

2013-06-21

Savannah River Remediation (SRR) is planning to remove a buildup of sodium aluminosilicate scale from the 2H-evaporator pot by loading and soaking the pot with heated 1.5 M nitric acid solution. Sampling and analysis of the scale material has been performed so that uranium and plutonium isotopic analysis can be input into a Nuclear Criticality Safety Assessment (NCSA) for scale removal by chemical cleaning. Historically, since the operation of the Defense Waste Processing Facility (DWPF), silicon in the DWPF recycle stream combines with aluminum in the typical tank farm supernate to form sodium aluminosilicate scale mineral deposits in the 2Hevaporatormore » pot and gravity drain line. The 2H-evaporator scale samples analyzed by Savannah River National Laboratory (SRNL) came from the bottom cone sections of the 2H-evaporator pot [Sample HTF-13-77] and the wall 2H-evaporator [sample HTF-13-82]. X-ray diffraction analysis (XRD) confirmed that both the 2H-evaporator pot scale and the wall samples consist of nitrated cancrinite (a crystalline sodium aluminosilicate solid) and clarkeite (a uranium oxy-hydroxide mineral). On “as received” basis, the bottom pot section scale sample contained an average of 2.59E+00 ± 1.40E-01 wt % total uranium with a U-235 enrichment of 6.12E-01 ± 1.48E-02 %, while the wall sample contained an average of 4.03E+00 ± 9.79E-01 wt % total uranium with a U-235 enrichment of 6.03E-01% ± 1.66E-02 wt %. The bottom pot section scale sample analyses results for Pu-238, Pu-239, and Pu-241 are 3.16E- 05 ± 5.40E-06 wt %, 3.28E-04 ± 1.45E-05 wt %, and <8.80E-07 wt %, respectively. The evaporator wall scale samples analysis values for Pu-238, Pu-239, and Pu-241 averages 3.74E-05 ± 6.01E-06 wt %, 4.38E-04 ± 5.08E-05 wt %, and <1.38E-06 wt %, respectively. The Pu-241 analyses results, as presented, are upper limit values. These results are provided so that SRR can calculate the equivalent uranium-235 concentrations for the NCSA. Results confirm that the uranium contained in the scale remains depleted with respect to natural uranium. SRNL did not calculate an equivalent U-235 enrichment, which takes into account other fissionable isotopes U-233, Pu-239 and Pu-241. The applicable method for calculation of equivalent U-235 will be determined in the NCSA.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tandon, Lav; Colletti, Lisa M.; Drake, Lawrence R.

This report discusses the process used to prove in the SRNL-Rev.2 coulometer for isotopic data analysis used in the special plutonium material project. In May of 2012, the PAR 173 coulometer system that had been the workhorse of the Plutonium Assay team since the early 1970s became inoperable. A new coulometer system had been purchased from Savannah River National Laboratory (SRNL) and installed in August of 2011. Due to funding issues the new system was not qualified at that time. Following the failure of the PAR 173, it became necessary to qualify the new system for use in Process 3401a,more » Plutonium Assay by Controlled Coulometry. A qualification plan similar to what is described in PQR -141a was followed. Experiments were performed to establish a statistical summary of the performance of the new system by monitoring the repetitive analysis of quality control sample, PEOL, and the assay of plutonium metals obtained from the Plutonium Exchange Program. The data for the experiments was acquired using work instructions ANC125 and ANC195. Figure 1 shows approximately 2 years of data for the PEOL material obtained using the PAR 173. The required acceptance criteria for the sample are that it returns the correct value for the quality control material of 88.00% within 2 sigma (95% Confidence Interval). It also must meet daily precision standards that are set from the historical data analysis of decades of data. The 2 sigma value that is currently used is 0.146 % as evaluated by the Statistical Science Group, CCS-6. The average value of the PEOL quality control material run in 10 separate days on the SRNL-03 coulometer is 87.98% with a relative standard deviation of 0.04 at the 95% Confidence interval. The date of data acquisition is between 5/23/2012 to 8/1/2012. The control samples are run every day experiments using the coulometer are carried out. It is also used to prove an instrument is in statistical control before any experiments are undertaken. The total number of replicate controls run with the new coulometer to date, is n=18. This value is identical to that calculated by the LANL statistical group for this material from data produced by the PAR 173 system over the period of October 2007 to May 2011. The final validation/verification test was to run a blind sample over multiple days. AAC participates in a plutonium exchange program which supplies blind Pu metal samples to the group on a regular basis. The Pu material supplied for this study was ran using the PAR 173 in the past and more recently with the new system. Table 1a contains the values determined through the use of the PAR 173 and Table 1b contains the values obtained with the new system. The Pu assay value obtained on the SRNL system is for paired analysis and had a value of 98.88+/-0.07% RSD at 95% CI. The Pu assay value (decay corrected to July 2012) of the material determined in prior measurements using the PAR173 is 99.05 +/- 0.06 % RSD at 95% CI. We believe that the instrument is adequate to meet the needs of the program.« less

Mercury speciation comparison. BrooksApplied Laboratories and Eurofins Frontier Global Sciences

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.; Wilmarth, W. R.

2016-12-16

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences (FGS), Inc. in Bothell, WA on behalf of the Savannah River Remediation (SRR) Mercury Program Team. These samples were analyzed for seven species including: total mercury, dissolved mercury, inorganic mercury ((Hg(I) and Hg(II)), elemental mercury, methylmercury, ethylmercury, and dimethylmercury, with an eighth species, particulate mercury, calculated from the difference between total and dissolved mercury after subtracting the elemental mercury. The species fraction of total mercury measured has ranged broadly from a low of 32% to a high of 146%,more » though the vast majority of samples have been <100%. This can be expected since one is summing multiple values that each have at least a ± 20% measurement uncertainty. Two liquid waste tanks particularly important to understanding the distribution of mercury species in the Savannah River Site (SRS) Tank Farm were selected for a round robin analysis by Eurofins FGS and BrooksApplied Laboratories (BAL). The analyses conducted by BAL on the Tank 22 and 38 samples and their agreement with those obtained from Eurofins FGS for total mercury, dissolved mercury, methylmercury, ethylmercury, and dimethylmercury provide a strong degree of confidence in these species measurements« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F.; Taylor-Pashow, K.

Savannah River National Laboratory (SRNL) received two sets of Solvent Hold Tank (SHT) samples (MCU-15-389 and MCU-15-390 pulled on February 23, 2015 and MCU-15-439, MCU-15-440, and MCU-15-441 pulled on February 28, 2015) for analysis. The samples in each set were combined and analyzed for composition. Analysis of the composite samples MCU-15-389-390 and MCU-15-439-440- 441 indicated a low concentration (~ 92 to 93 % of nominal) of the suppressor (TiDG) and slightly below nominal concentrations of the extractant (MaxCalix), but nominal levels of the modifier (CS-7SB) and of the Isopar™ L. This analysis confirms the addition of TiDG, MaxCalix, and modifiermore » to the solvent on February 22, 2015. Despite that the values are below the target component levels, the current levels of TiDG and MaxCalix are sufficient for continuing operation without adding a trim at this time. No impurities above the 1000 ppm level were found in this solvent. However, the p-nut vials that delivered the samples contained small (1 mm) droplets of oxidized modifier and amides. The laboratory will continue to monitor the quality of the solvent in particular for any new impurity or degradation of the solvent components.« less

Materials characterization studies on LANA75/85 materials for replacement beds

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shanahan, Kirk L.

2016-12-30

During FY15 and FY16, a purchase order (PO) was placed with Japan Metals and Chemicals, USA after an open bidding procurement process for 282 kg of LaNi 4.25Al 0.75 and 226 kg. of LaNi 4.15Al 0.85. These materials were to be used in Tritium Facility replacement beds for existing beds that have reached the end of their useful life. As part of the PO, a 100 g. sample of each material was delivered to the SRNL Hydrogen Processing Group for characterization studies as is typically done for all newly acquired hydride materials. The PO actually employed a “trust but verify”more » approach where JMCUSA was allowed to ship materials it felt met specifications without SRS confirmation, as long as the data used to do so was delivered to SRS as part of the PO documentation package. Subsequent SRNL analysis revealed that the material met all specifications and was of very high quality. This report documents those findings.« less

ELECTRONICS UPGRADE TO THE SAVANNAH RIVER NATIONAL LABORATORY COULOMETER FOR PLUTONIUM AND NEPTUNIUM ASSAY

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cordaro, J.; Holland, M.; Reeves, G.

The Savannah River Site (SRS) has the analytical measurement capability to perform high-precision plutonium concentration measurements by controlled-potential coulometry. State-of-the-art controlled-potential coulometers were designed and fabricated by the Savannah River National Laboratory and installed in the Analytical Laboratories process control laboratory. The Analytical Laboratories uses coulometry for routine accountability measurements of and for verification of standard preparations used to calibrate other plutonium measurement systems routinely applied to process control, nuclear safety, and other accountability applications. The SRNL Coulometer has a demonstrated measurement reliability of {approx}0.05% for 10 mg samples. The system has also been applied to the characterization of neptuniummore » standard solutions with a comparable reliability. The SRNL coulometer features: a patented current integration system; continuous electrical calibration versus Faraday's Constants and Ohm's Law; the control-potential adjustment technique for enhanced application of the Nernst Equation; a wide operating room temperature range; and a fully automated instrument control and data acquisition capability. Systems have been supplied to the International Atomic Energy Agency (IAEA), Russia, Japanese Atomic Energy Agency (JAEA) and the New Brunswick Laboratory (NBL). The most recent vintage of electronics was based on early 1990's integrated circuits. Many of the components are no longer available. At the request of the IAEA and the Department of State, SRNL has completed an electronics upgrade of their controlled-potential coulometer design. Three systems have built with the new design, one for the IAEA which was installed at SAL in May 2011, one system for Los Alamos National Laboratory, (LANL) and one for the SRS Analytical Laboratory. The LANL and SRS systems are undergoing startup testing with installation scheduled for this summer.« less

Actual waste demonstration of the nitric-glycolic flowsheet for sludge batch 9 qualification

DOE Office of Scientific and Technical Information (OSTI.GOV)

Newell, D.; Pareizs, J.; Martino, C.

For each sludge batch that is processed in the Defense Waste Processing Facility (DWPF), the Savannah River National Laboratory (SRNL) performs qualification testing to demonstrate that the sludge batch is processable. Based on the results of this actual-waste qualification and previous simulant studies, SRNL recommends implementation of the nitric-glycolic acid flowsheet in DWPF. Other recommendations resulting from this demonstration are reported in section 5.0.

Gold-manganese nanoparticles for targeted diagnostic and imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Murph, Simona Hunyadi

Imagine the possibility of non-invasive, non-radiation based Magnetic resonance imaging (MRI) in combating cardiac disease. Researchers at the Savannah River National Laboratory (SRNL) are developing a process that would use nanotechnology in a novel, targeted approach that would allow MRIs to be more descriptive and brighter, and to target specific organs. Researchers at SRNL have discovered a way to use multifunctional metallic gold-manganese nanoparticles to create a unique, targeted positive contrast agent. SRNL Senior Scientist Dr. Simona Hunyadi Murph says she first thought of using the nanoparticles for cardiac disease applications after learning that people who survive an infarct exhibitmore » up to 15 times higher rate of developing chronic heart failure, arrhythmias and/or sudden death compared to the general population. Without question, nanotechnology will revolutionize the future of technology. The development of functional nanomaterials with multi-detection modalities opens up new avenues for creating multi-purpose technologies for biomedical applications.« less

TANK 40 FINAL SB7B CHEMICAL CHARACTERIZATION RESULTS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C.

2012-03-15

A sample of Sludge Batch 7b (SB7b) was taken from Tank 40 in order to obtain radionuclide inventory analyses necessary for compliance with the Waste Acceptance Product Specifications (WAPS). The SB7b WAPS sample was also analyzed for chemical composition including noble metals and fissile constituents, and these results are reported here. These analyses along with the WAPS radionuclide analyses will help define the composition of the sludge in Tank 40 that is currently being fed to the Defense Waste Processing Facility (DWPF) as SB7b. At the Savannah River National Laboratory (SRNL) the 3-L Tank 40 SB7b sample was transferred frommore » the shipping container into a 4-L high density polyethylene bottle and solids were allowed to settle over the weekend. Supernate was then siphoned off and circulated through the shipping container to complete the transfer of the sample. Following thorough mixing of the 3-L sample, a 558 g sub-sample was removed. This sub-sample was then utilized for all subsequent analytical samples. Eight separate aliquots of the slurry were digested, four with HNO{sub 3}/HCl (aqua regia) in sealed Teflon{reg_sign} vessels and four with NaOH/Na{sub 2}O{sub 2} (alkali or peroxide fusion) using Zr crucibles. Two Analytical Reference Glass - 1 (ARG-1) standards were digested along with a blank for each preparation. Each aqua regia digestion and blank was diluted to 1:100 mL with deionized water and submitted to Analytical Development (AD) for inductively coupled plasma - atomic emission spectroscopy (ICP-AES) analysis, inductively coupled plasma - mass spectrometry (ICP-MS) analysis, atomic absorption spectroscopy (AA) for As and Se, and cold vapor atomic absorption spectroscopy (CV-AA) for Hg. Equivalent dilutions of the alkali fusion digestions and blank were submitted to AD for ICP-AES analysis. Tank 40 SB7b supernate was collected from a mixed slurry sample in the SRNL Shielded Cells and submitted to AD for ICP-AES, ion chromatography (IC), total base/free OH{sup -}/other base, total inorganic carbon/total organic carbon (TIC/TOC) analyses, and Cs-137 gamma scan. Weighted dilutions of slurry were submitted for IC, TIC/TOC, and total base/free OH{sup -}/other base analyses. Activities for U-233, U-235, and Pu-239 were determined from the ICP-MS data for the aqua regia digestions of the Tank 40 WAPS slurry using the specific activity of each isotope. The Pu-241 value was determined from a Pu-238/-241 method developed by SRNL AD and previously described. The following conclusions were drawn from the analytical results reported here: (1) The ratios of the major elements for the SB7b WAPS sample are different from those measured for the SB7a WAPS sample. There is less Al and Mn relative to Fe than the previous sludge batch. (2) The elemental composition of this sample and the analyses conducted here are reasonable and consistent with DWPF batch data measurements in light of DWPF pre-sample concentration and SRAT product heel contributions to the DWPF SRAT receipt analyses. The element ratios for Al/Fe, Ca/Fe, Mn/Fe, and U/Fe agree within 10% between this work and the DWPF Sludge Receipt and Adjustment Tank (SRAT) receipt analyses. (3) Sulfur in the SB7b WAPS sample is 82% soluble, slightly less than results reported for SB3, SB4, and SB6 samples but unlike the 50% insoluble sulfur observed in the SB5 WAPS sample. In addition, 23% of the soluble sulfur is not present as sulfate in SB7b. (4) The average activities of the fissile isotopes of interest in the SB7b WAPS sample are (in {mu}Ci/g of total dried solids): 4.22E-02 U-233, 6.12E-04 U-235, 1.08E+01 Pu-239, and 5.09E+01 Pu-241. The full radionuclide composition will be reported in a future document. (5) The fission product noble metal and Ag concentrations appear to have largely peaked in previous DWPF sludge batches, with the exception of Ru, which still shows a slight increase in SB7b.« less

Solvent Hold Tank Sample Results for MCU-16-934-935-936: June 2016 Monthly Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Jones, D. H.

2016-08-30

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-934-935-936), pulled on 07/01/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-934-935-936 indicated the Isopar™L concentration is above its nominal level (101%). The modifier (CS-7SB) and the TiDG concentrations are 8% and 29 % below their nominal concentrations. This analysis confirms the solvent may require the addition of TiDG, and possibly of modifier. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease withmore » time. Periodic characterization and trimming additions to the solvent are recommended. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). However, up to 21.1 ± 4 micrograms of mercury per gram of solvent (or 17.5 μg/mL) was detected in this sample (as determined by the XRF method of undigested sample). The current gamma level (1.41E5 dpm/mL) confirmed that the gamma concentration has returned to previous levels (as observed in the late 2015 samples) where the process operated normally and as expected.« less

Summary Report For The Analysis Of The Sludge Batch 7b (Macrobatch 9) DWPF Pour Stream Glass Sample For Canister S04023

DOE Office of Scientific and Technical Information (OSTI.GOV)

Johnson, F. C.

2013-11-18

In order to comply with the Defense Waste Processing Facility (DWPF) Waste Form Compliance Plan for Sluldge Batch 7b, Savannah River National Laboratory (SRNL) personnel characterized the Defense Waste Processing Facility (DWPF) pour stream (PS) glass sample collected while filling canister S04023. This report summarizes the results of the compositional analysis for reportable oxides and radionuclides and the normalized Product Consistency Test (PCT) results. The PCT responses indicate that the DWPF produced glass that is significantly more durable than the Environmental Assessment glass.

Experimental Determination and Thermodynamic Modeling of Electrical Conductivity of SRS Waste Tank Supernate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pike, J.; Reboul, S.

2015-06-01

SRS High Level Waste Tank Farm personnel rely on conductivity probes for detection of incipient overflow conditions in waste tanks. Minimal information is available concerning the sensitivity that must be achieved such that that liquid detection is assured. Overly sensitive electronics results in numerous nuisance alarms for these safety-related instruments. In order to determine the minimum sensitivity required of the probe, Tank Farm Engineering personnel need adequate conductivity data to improve the existing designs. Little or no measurements of liquid waste conductivity exist; however, the liquid phase of the waste consists of inorganic electrolytes for which the conductivity may bemore » calculated. Savannah River Remediation (SRR) Tank Farm Facility Engineering requested SRNL to determine the conductivity of the supernate resident in SRS waste Tank 40 experimentally as well as computationally. In addition, SRNL was requested to develop a correlation, if possible, that would be generally applicable to liquid waste resident in SRS waste tanks. A waste sample from Tank 40 was analyzed for composition and electrical conductivity as shown in Table 4-6, Table 4-7, and Table 4-9. The conductivity for undiluted Tank 40 sample was 0.087 S/cm. The accuracy of OLI Analyzer™ was determined using available literature data. Overall, 95% of computed estimates of electrical conductivity are within ±15% of literature values for component concentrations from 0 to 15 M and temperatures from 0 to 125 °C. Though the computational results are generally in good agreement with the measured data, a small portion of literature data deviates as much as ±76%. A simplified model was created that can be used readily to estimate electrical conductivity of waste solution in computer spreadsheets. The variability of this simplified approach deviates up to 140% from measured values. Generally, this model can be applied to estimate the conductivity within a factor of two. The comparison of the simplified model to pure component literature data suggests that the simplified model will tend to under estimate the electrical conductivity. Comparison of the computed Tank 40 conductivity with the measured conductivity shows good agreement within the range of deviation identified based on pure component literature data.« less

POROUS WALL, HOLLOW GLASS MICROSPHERES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sexton, W.

Hollow Glass Microspheres (HGM) is not a new technology. All one has to do is go to the internet and Google{trademark} HGM. Anyone can buy HGM and they have a wide variety of uses. HGM are usually between 1 to 100 microns in diameter, although their size can range from 100 nanometers to 5 millimeters in diameter. HGM are used as lightweight filler in composite materials such as syntactic foam and lightweight concrete. In 1968 a patent was issued to W. Beck of the 3M{trademark} Company for 'Glass Bubbles Prepared by Reheating Solid Glass Particles'. In 1983 P. Howell wasmore » issued a patent for 'Glass Bubbles of Increased Collapse Strength' and in 1988 H. Marshall was issued a patent for 'Glass Microbubbles'. Now Google{trademark}, Porous Wall, Hollow Glass Microspheres (PW-HGMs), the key words here are Porous Wall. Almost every article has its beginning with the research done at the Savannah River National Laboratory (SRNL). The Savannah River Site (SRS) where SRNL is located has a long and successful history of working with hydrogen and its isotopes for national security, energy, waste management and environmental remediation applications. This includes more than 30 years of experience developing, processing, and implementing special ceramics, including glasses for a variety of Department of Energy (DOE) missions. In the case of glasses, SRS and SRNL have been involved in both the science and engineering of vitreous or glass based systems. As a part of this glass experience and expertise, SRNL has developed a number of niches in the glass arena, one of which is the development of porous glass systems for a variety of applications. These porous glass systems include sol gel glasses, which include both xerogels and aerogels, as well as phase separated glass compositions, that can be subsequently treated to produce another unique type of porosity within the glass forms. The porous glasses can increase the surface area compared to 'normal glasses of a 1 to 2 order of magnitude, which can result in unique properties in areas such as hydrogen storage, gas transport, gas separations and purifications, sensors, global warming applications, new drug delivery systems and so on. One of the most interesting porous glass products that SRNL has developed and patented is Porous Wall, Hollow Glass Microspheres (PW-HGMs) that are being studied for many different applications. The European Patent Office (EPO) just recently notified SRS that the continuation-in-part patent application for the PW-HGMs has been accepted. The original patent, which was granted by the EPO on June 2, 2010, was validated in France, Germany and the United Kingdom. The microspheres produced are generally in the range of 2 to 100 microns, with a 1 to 2 micron wall. What makes the SRNL microspheres unique from all others is that the team in Figure 1 has found a way to induce and control porosity through the thin walls on a scale of 100 to 3000 {angstrom}. This is what makes the SRNL HW-HGMs one-of-a-kind, and is responsible for many of their unique properties and potential for various applications, including those in tritium storage, gas separations, H-storage for vehicles, and even a variety of new medical applications in the areas of drug delivery and MRI contrast agents. SRNL Hollow Glass Microspheres, and subsequent, Porous Wall, Hollow Glass Microspheres are fabricated using a flame former apparatus. Figure 2 is a schematic of the apparatus.« less

Rapid determination of 210Po in water samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, Sherrod L.; Culligan, Brian K.; Hutchison, Jay B.

2013-08-02

A new rapid method for the determination of 210Po in water samples has been developed at the Savannah River National Laboratory (SRNL) that can be used for emergency response or routine water analyses. If a radiological dispersive device (RDD) event or a radiological attack associated with drinking water supplies occurs, there will be an urgent need for rapid analyses of water samples, including drinking water, ground water and other water effluents. Current analytical methods for the assay of 210Po in water samples have typically involved spontaneous auto-deposition of 210Po onto silver or other metal disks followed by counting by alphamore » spectrometry. The auto-deposition times range from 90 minutes to 24 hours or more, at times with yields that may be less than desirable. If sample interferences are present, decreased yields and degraded alpha spectrums can occur due to unpredictable thickening in the deposited layer. Separation methods have focused on the use of Sr Resin, often in combination with 210Pb analysis. A new rapid method for 210Po in water samples has been developed at the Savannah River National Laboratory (SRNL) that utilizes a rapid calcium phosphate co-precipitation method, separation using DGA Resin (N,N,N,N-tetraoctyldiglycolamide extractant-coated resin, Eichrom Technologies or Triskem-International), followed by rapid microprecipitation of 210Po using bismuth phosphate for counting by alpha spectrometry. This new method can be performed quickly with excellent removal of interferences, high chemical yields and very good alpha peak resolution, eliminating any potential problems with the alpha source preparation for emergency or routine samples. A rapid sequential separation method to separate 210Po and actinide isotopes was also developed. This new approach, rapid separation with DGA Resin plus microprecipitation for alpha source preparation, is a significant advance in radiochemistry for the rapid determination of 210Po.« less

DWPF DECON FRIT SUPERNATE ANALYSIS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peeler, D.; Crawford, C.

2010-09-22

The Savannah River National Laboratory (SRNL) has been requested to perform analyses on samples of the Defense Waste Processing Facility (DWPF) decon frit slurry (i.e., supernate samples and sump solid samples). Four 1-L liquid slurry samples were provided to SRNL by Savannah River Remediation (SRR) from the 'front-end' decon activities. Additionally, two 1-L sump solids samples were provided to SRNL for compositional and physical analysis. This report contains the results of the supernate analyses, while the solids (sump and slurry) results will be reported in a supplemental report. The analytical data from the decon frit supernate indicate that all ofmore » the radionuclide, organic, and inorganic concentrations met the limits in Revision 4 of the Effluent Treatment Plant (ETP) Waste Acceptance Criteria (WAC) with the exception of boron. The ETP WAC limit for boron is 15.0 mg/L while the average measured concentration (based on quadruplicate analysis) was 15.5 mg/L. The measured concentrations of Li, Na, and Si were also relatively high in the supernate analysis. These results are consistent with the relatively high measured value of B given the compositional make-up of Frit 418. Given these results, it was speculated that either (a) Frit 418 was dissolving into the supernate or aqueous fraction and/or (b) fine frit particulates were carried forward to the analytical instrument based on the sampling procedure used (i.e., the supernate samples were not filtered - only settled with the liquid fraction being transferred with a pipette). To address this issue, a filtered supernate sample (using a 0.45 um filter) was prepared and submitted for analysis. The results of the filtered sample were consistent with 'unfiltered or settled' sample - relatively high values of B, Li, Na, and Si were found. This suggests that Frit 418 is dissolving in the liquid phase which could be enhanced by the high surface area of the frit fines or particulates in suspension. Based on the results of this study, it is recommended that DWPF re-evaluate the technical basis for the B WAC limit (the only component that exceeds the ETP WAC limit from the supernate analyses) or assess if a waiver or exception can be obtained for exceeding this limit. Given the possible dissolution of B, Li, Na, and Si into the supernate (due to dissolution of frit), DWPF may need to assess if the release of these frit components into the supernate are a concern for the disposal options being considered. It should be noted that the results of this study may not be representative of future decon frit solutions or sump/slurry solids samples. Therefore, future DWPF decisions regarding the possible disposal pathways for either the aqueous or solid portions of the Decon Frit system need to factor in the potential differences. More specifically, introduction of a different frit or changes to other DWPF flowsheet unit operations (e.g., different sludge batch or coupling with other process streams) may impact not only the results but also the conclusions regarding acceptability with respect to the ETF WAC limits.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Almond, P.; Livingston, R.; Traver, L.

The Savannah River National Laboratory (SRNL) 3013 destructive examination program performs surveillances on 3013 containers originating from multiple sites across the DOE complex. The bases for the packaging, storage, and surveillance activities are derived from the Department of Energy's 3013 Standard (DOE-STD-3013-2004). During destructive examination, headspace gas samples are obtained from the 3013 inner container and the annulus between the outer and inner containers. To characterize gas species, the samples are analyzed by gas chromatography (GC), direct-inlet mass spectrometry (DIMS), and Fourier-transform infrared spectroscopy (FTIR). The GC results, as well as other parameters, are utilized as input into the gasmore » evaluation software tool (GEST) program for computation of pre-puncture gas compositions and pressures. Over 30 containers from the Hanford Site and the Rocky Flats Environmental Technology Site (RFETS) have been examined in the first three years of the surveillance program. Several containers were shown to have appreciable hydrogen content (some greater than 30 mol %), yet little or no oxygen was detected in any of the containers, including those exhibiting high hydrogen concentrations. Characteristics including moisture content, surface area, and material composition, along with the headspace gas composition, are utilized in an attempt to explain the chemical behavior of the packaged materials.« less

Speciation of mercury in sludge solids: washed sludge

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.; Lourie, A. P.

2017-10-24

The objective of this applied research task was to study the type and concentration of mercury compounds found within the contaminated Savannah River Site Liquid Waste System (SRS LWS). A method of selective sequential extraction (SSE), developed by Eurofins Frontier Global Sciences1,2 and adapted by SRNL, utilizes an extraction procedure divided into seven separate tests for different species of mercury. In the SRNL’s modified procedure four of these tests were applied to a washed sample of high level radioactive waste sludge.

Analysis of tank 38H (HTF-38-17-18, -19) and tank 43H (HTF-43-17-20, -21) samples for support of the enrichment control and corrosion control programs

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hay, M. S.; Coleman, C. J.; Diprete, D. P.

SRNL analyzed samples from Tank 38H and Tank 43H to support ECP and CCP. The total uranium in the Tank 38H samples ranged from 53.7 mg/L for the surface sample to 57.0 mg/L in the sub-surface sample. The Tank 43H samples showed uranium concentrations of 46.2 mg/L for the surface sample and 45.7 mg/L in the sub-surface sample. The U-235 percentage was 0.63% in the Tank 38H samples and 0.62% in the Tank 43H samples. The total uranium and percent U-235 results appear consistent with recent Tank 38H and Tank 43H uranium measurements. The plutonium results for the Tank 38Hmore » surface sample are slightly higher than recent sample results, while the Tank 43H plutonium results are within the range of values measured on previous samples. The Cs-137 results for the Tank 38H surface and subsurface samples are slightly higher than the concentrations measured in recent samples. The Cs-137 results for the two Tank 43H samples are within the range of values measured on previous samples. The comparison of the sum of the cations in each sample versus the sum of the anions shows a difference of 23% for the Tank 38H surface sample and 18% for the Tank 43H surface sample. The four samples show silicon concentrations somewhat lower than the previous samples with values ranging from 80.2 to 105 mg/L.« less

One-dimensional Spatial Distributions of Gamma-ray Emitting Contaminants in Field Lysimeters Using a Collimated Gamma-ray Spectroscopy System.

PubMed

Erdmann, Bryan J; Powell, Brian A; Kaplan, Daniel I; DeVol, Timothy A

2018-05-01

One-dimensional scans of gamma-ray emitting contaminants were conducted on lysimeters from the RadFLEX facility at the Savannah River Nationals Laboratory (SRNL). The lysimeters each contained a contamination source that was buried in SRNL soil. A source consisted of Cs, Co, Ba, and Eu incorporated either into a solid waste form (Portland cement and reducing grout) or applied to a filter paper for direct soil exposure. The lysimeters were exposed to natural environmental conditions for 3 to 4 y. The initial contaminant activities range from 4.0 to 9.0 MBq for the solid wasteforms and 0.25 to 0.47 MBq for the soil-incorporated source. The measurements were performed using a collimated high-purity germanium gamma-ray spectrometer with a spatial resolution of 2.5 mm. These scans showed downward mobility of Co and Ba when the radionuclides were incorporated directly into the SRNL soil. When radionuclides were incorporated into the solid waste forms positioned in the SRNL soil, Cs exhibited both upward and downward dispersion while the other radionuclides showed no movement. This dispersion was more significant for the Portland cement than the reducing grout wasteform. Europium-152 was the only radionuclide of those studied that showed no movement within the spatial resolution of the scanner from the original placement within the lysimeter. Understanding radionuclide movement in the environment is important for developing strategies for waste management and disposal.

CESIUM REMOVAL FROM TANKS 241-AN-103 & 241-SX-105 & 241-AZ-101/102 COMPOSITE FOR TESTING IN BENCH SCALE STEAM REFORMER

DOE Office of Scientific and Technical Information (OSTI.GOV)

DUNCAN JB; HUBER HJ

2011-06-08

This report documents the preparation of three actual Hanford tank waste samples for shipment to the Savannah River National Laboratory (SRNL). Two of the samples were dissolved saltcakes from tank 241-AN-103 (hereafter AN-103) and tank 241-SX-105 (hereafter SX-105); one sample was a supernate composite from tanks 241-AZ-101 and 241-AZ-102 (hereafter AZ-101/102). The preparation of the samples was executed following the test plans LAB-PLAN-10-00006, Test Plan for the Preparation of Samples from Hanford Tanks 241-SX-105, 241-AN-103, 241-AN-107, and LAB-PLN-10-00014, Test Plan for the Preparation of a Composite Sample from Hanford Tanks 241-AZ-101 and 241-AZ-102 for Steam Reformer Testing at the Savannahmore » River National Laboratory. All procedural steps were recorded in laboratory notebook HNF-N-274 3. Sample breakdown diagrams for AN-103 and SX-105 are presented in Appendix A. The tank samples were prepared in support of a series of treatability studies of the Fluidized Bed Steam Reforming (FBSR) process using a Bench-Scale Reformer (BSR) at SRNL. Tests with simulants have shown that the FBSR mineralized waste form is comparable to low-activity waste glass with respect to environmental durability (WSRC-STI-2008-00268, Mineralization of Radioactive Wastes by Fluidized Bed Steam Reforming (FBSR): Comparisons to Vitreous Waste Forms and Pertinent Durability Testing). However, a rigorous assessment requires long-term performance data from FB SR product formed from actual Hanford tank waste. Washington River Protection Solutions, LLC (WRPS) has initiated a Waste Form Qualification Program (WP-S.2.1-20 1 0-00 1, Fluidized Bed Steam Reformer Low-level Waste Form Qualification) to gather the data required to demonstrate that an adequate FBSR mineralized waste form can be produced. The documentation of the selection process of the three tank samples has been separately reported in RPP-48824, 'Sample Selection Process for Bench-Scale Steam Reforming Treatability Studies Using Hanford Waste Samples.'« less

CESIUM REMOVAL FROM TANKS 241-AN-103 & 241-SX-105 & 241-AZ-101 & 241AZ-102 COMPOSITE FOR TESTING IN BENCH SCALE STEAM REFORMER

DOE Office of Scientific and Technical Information (OSTI.GOV)

DUNCAN JB; HUBER HJ

2011-04-21

This report documents the preparation of three actual Hanford tank waste samples for shipment to the Savannah River National Laboratory (SRNL). Two of the samples were dissolved saltcakes from tank 241-AN-103 (hereafter AN-103) and tank 241-SX-105 (hereafter SX-105); one sample was a supernate composite from tanks 241-AZ-101 and 241-AZ-102 (hereafter AZ-101/102). The preparation of the samples was executed following the test plans LAB-PLAN-10-00006, Test Plan for the Preparation of Samples from Hanford Tanks 241-SX-105, 241-AN-103, 241-AN-107, and LAB-PLN-l0-00014, Test Plan for the Preparation of a Composite Sample from Hanford Tanks 241-AZ-101 and 241-AZ-102 for Steam Reformer Testing at the Savannahmore » River National Laboratory. All procedural steps were recorded in laboratory notebook HNF-N-274 3. Sample breakdown diagrams for AN-103 and SX-105 are presented in Appendix A. The tank samples were prepared in support of a series of treatability studies of the Fluidized Bed Steam Reforming (FBSR) process using a Bench-Scale Reformer (BSR) at SRNL. Tests with simulants have shown that the FBSR mineralized waste form is comparable to low-activity waste glass with respect to environmental durability (WSRC-STI-2008-00268, Mineralization of Radioactive Wastes by Fluidized Bed Steam Reforming (FBSR): Comparisons to Vitreous Waste Forms and Pertinent Durability Testing). However, a rigorous assessment requires long-term performance data from FBSR product formed from actual Hanford tank waste. Washington River Protection Solutions, LLC (WRPS) has initiated a Waste Form Qualification Program (WP-5.2.1-2010-001, Fluidized Bed Steam Reformer Low-level Waste Form Qualification) to gather the data required to demonstrate that an adequate FBSR mineralized waste form can be produced. The documentation of the selection process of the three tank samples has been separately reported in RPP-48824, Sample Selection Process for Bench-Scale Steam Reforming Treatability Studies Using Hanford Waste Samples.« less

Characterization Results for the March 2016 H-Tank Farm 2H Evaporator Overhead Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nicholson, J. C.

This report contains the radioanalytical results of the 2H evaporator overhead sample received at SRNL on March 16, 2016. Specifically, concentrations of 137Cs, 90Sr, and 129I are reported and compared to the corresponding Waste Acceptance Criteria (WAC) limits of the Effluent Treatment Project (ETP) Waste Water Collection Tank (WWCT) (rev. 6). All of the radionuclide concentrations in the sample were found to be in compliance with the ETP WAC limits. Revision 1 of this document corrects the cumulative beta count initially reported for 90Sr content with the sole 90Sr count obtained after recharacterization of the sample. The initial data wasmore » found to be a cumulative beta count rather than the 90Sr count requested.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miller, D. H.; Reigel, M. M.

A full-scale formed core sampler was designed and functionally tested for use in the Saltstone Disposal Facility (SDF). Savannah River National Laboratory (SRNL) was requested to compare properties of the formed core samples and core drilled samples taken from adjacent areas in the full-scale sampler. While several physical properties were evaluated, the primary property of interest was hydraulic conductivity. Differences in hydraulic conductivity between the samples from the formed core sampler and those representing the bulk material were noted with respect to the initial handling and storage of the samples. Due to testing conditions, the site port samples were exposedmore » to uncontrolled temperature and humidity conditions prior to testing whereas the formed core samples were kept in sealed containers with minimal exposure to an uncontrolled environment prior to testing. Based on the results of the testing, no significant differences in porosity or density were found between the formed core samples and those representing the bulk material in the test stand.« less

APPLICATION OF VACUUM SALT DISTILLATION TECHNOLOGY FOR THE REMOVAL OF FLUORIDE AND CHLORIDE FROM LEGACY FISSILE MATERIALS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pierce, R.; Peters, T.

2011-11-01

Between September 2009 and January 2011, the Savannah River National Laboratory (SRNL) and the Savannah River Site (SRS) HB-Line Facility designed, developed, tested, and successfully deployed a production-scale system for the distillation of sodium chloride (NaCl) and potassium chloride (KCl) from plutonium oxide (PuO{sub 2}). Subsequent efforts adapted the vacuum salt distillation (VSD) technology for the removal of chloride and fluoride from less-volatile halide salts at the same process temperature and vacuum. Calcium chloride (CaCl{sub 2}), calcium fluoride (CaF{sub 2}), and plutonium fluoride (PuF{sub 3}) were of particular concern. To enable the use of the same operating conditions for themore » distillation process, SRNL employed in situ exchange reactions to convert the less-volatile halide salts to compounds that facilitated the distillation of halide without removal of plutonium. SRNL demonstrated the removal of halide from CaCl{sub 2}, CaF{sub 2} and PuF{sub 3} below 1000 C using VSD technology.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Jones, D. H.

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-15-815-816-817-818-819-820), pulled on 11/29/2015 for analysis. The samples were inspected, combined, and analyzed for composition. Chemical analysis of the composite sample MCU-15-815-816-817-818-819-820 indicated the TiDG, Isopar™L, and MaxCalix are at nominal levels. The modifier concentration is 3% below its nominal concentration. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent on November 28, 2015. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterizationmore » and trimming additions to the solvent are recommended. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). However, up to 12.5 ± 3 micrograms of mercury per gram of solvent (or 10.4 μg/mL) was detected in this sample. The solids residues found at the bottom of the p-nut vial from sample MCU-15-815 were determined to be left-over pipe residues that were flushed into the sample and they were found to have no impact on the solvent purity or on the chemical and physical properties of the solvent. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.« less

Aging Study Of EPDM O-Ring Material For The H1616 Shipping Package - Three Year Status

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stefek, T.; Daugherty, W.; Skidmore, E.

This is a 3-year status report for tasks carried out per Task Technical Plan SRNL-STI-2011-00506. A series of tasks/experiments were performed at the Savannah River National Laboratory (SRNL) to monitor the aging performance of ethylene propylene diene monomer (EPDM) O-rings used in the H1616 shipping package. The test data provide a technical basis to extend the annual maintenance of the H1616 shipping package to three years and to predict the life of the EPDM O-rings at the bounding service conditions.

Hanford double shell waste tank corrosion studies - final report FY2014

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wiersma, B. J.; Fuentes, R. E.; Hicks, K.

2014-12-19

SRNL tasks for FY14 included studies to evaluate the susceptibility of carbon steel to vapor space corrosion (VSC), liquid-air interface (LAI) corrosion, and pitting corrosion. Additionally, SRNL evaluated the susceptibility of carbon steel to pitting corrosion under buffered waste conditions, with the objective of determining the adequate amount of inhibitor (e.g., nitrite) necessary to mitigate pitting corrosion. Other CPP experiments were performed in historical waste simulants and the results were compared to previously gathered results. The results of these activities were utilized to assess the robustness of the standardized CPP protocol

DWPF simulant CPC studies for SB8

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koopman, D. C.; Zamecnik, J. R.

2013-06-25

The Savannah River National Laboratory (SRNL) accepted a technical task request (TTR) from Waste Solidification Engineering to perform simulant tests to support the qualification of Sludge Batch 8 (SB8) and to develop the flowsheet for SB8 in the Defense Waste Processing Facility (DWPF). These efforts pertained to the DWPF Chemical Process Cell (CPC). Separate studies were conducted for frit development and glass properties (including REDOX). The SRNL CPC effort had two primary phases divided by the decision to drop Tank 12 from the SB8 constituents. This report focuses on the second phase with SB8 compositions that do not contain themore » Tank 12 piece. A separate report will document the initial phase of SB8 testing that included Tank 12. The second phase of SB8 studies consisted of two sets of CPC studies. The first study involved CPC testing of an SB8 simulant for Tank 51 to support the CPC demonstration of the washed Tank 51 qualification sample in the SRNL Shielded Cells facility. SB8-Tank 51 was a high iron-low aluminum waste with fairly high mercury and moderate noble metal concentrations. Tank 51 was ultimately washed to about 1.5 M sodium which is the highest wash endpoint since SB3-Tank 51. This study included three simulations of the DWPF Sludge Receipt and Adjustment Tank (SRAT) cycle and Slurry Mix Evaporator (SME) cycle with the sludge-only flowsheet at nominal DWPF processing conditions and three different acid stoichiometries. These runs produced a set of recommendations that were used to guide the successful SRNL qualification SRAT/SME demonstration with actual Tank 51 washed waste. The second study involved five SRAT/SME runs with SB8-Tank 40 simulant. Four of the runs were designed to define the acid requirements for sludge-only processing in DWPF with respect to nitrite destruction and hydrogen generation. The fifth run was an intermediate acid stoichiometry demonstration of the coupled flowsheet for SB8. These runs produced a set of processing recommendations for DWPF along with some data related to Safety Class documentation at DWPF. Some significant observations regarding SB8 follow: Reduced washing in Tank 51 led to an increase in the wt.% soluble solids of the DWPF feed. If wt.% total solids for the SRAT and SME product weren’t adjusted upward to maintain insoluble solids levels similar to past sludge batches, then the rheological properties of the slurry went below the low end of the DWPF design bases for the SRAT and SME. Much higher levels of dissolved manganese were found in the SRAT and SME products than in recent sludge batches. Closed crucible melts were more reduced than expected. The working hypothesis is that the soluble Mn is less oxidizing than assumed in the REDOX calculations. A change in the coefficient for Mn in the REDOX equation was recommended in a separate report. The DWPF (Hsu) stoichiometric acid equation was examined in detail to better evaluate how to control acid in DWPF. The existing DWPF equation can likely be improved without changing the required sample analyses through a paper study using existing data. The recommended acid stoichiometry for initial SB8 SRAT batches is 115-120% stoichiometry until some processing experience is gained. The conservative range (based on feed properties) of stoichiometric factors derived in this study was from 110-147%, but SRNL recommends using only the lower half of this range, 110-126% even after initial batches provide processing experience. The stoichiometric range for sludge-only processing appears to be suitable for coupled operation based on results from the run in the middle of the range. Catalytic hydrogen was detectable (>0.005 vol%) in all SRAT and SME cycles. Hydrogen reached 30-35% of the SRAT and SME limits at the mid-point of the stoichiometry window (bounding noble metals and acid demand).« less

CRADA Final Report For CRADA NO. CR-12-006 [Operation and Testing of an SO 2-depolarized Electrolyzer (SDE) for the Purpose of Hydrogen and Sulfuric Acid Production

DOE Office of Scientific and Technical Information (OSTI.GOV)

Summers, W. A.; Colon-Mercado, H. R.; Steimke, J. L.

2014-02-24

Over the past several years, Savannah River National Laboratory (SRNL) has led a team of collaborators under the Department of Energy’s (DOE) nuclear hydrogen production program to develop the Hybrid Sulfur (HyS) Process. HyS is a 2-step water-splitting process consisting of high temperature decomposition of sulfuric acid to generate SO 2, followed by the electrolysis of aqueous SO 2 to generate hydrogen and sulfuric acid. The latter is fed back into the high temperature reactor. SRNL designed and built an SO 2-depolarized electrolyzer (SDE) and a test facility. Over 40 SDE’s were tested using different catalysts, membranes and other components.more » SRNL demonstrated that an SDE could be operated continuously for approximately 200 hours under certain conditions without buildup of sulfur at the SDE’s cathode, thus solving a key technical problem with SDE technology. Air Products and Chemicals, Inc. (APCI) is a major supplier of hydrogen production systems, and they have proprietary technology that could benefit from the SDE developed by SRNS, or some improved version thereof. However, to demonstrate that SRNL’s SDE is a truly viable approach to the electrolyzer design, continuous operation for far greater periods of time than 200 hours must be demonstrated, and the electrolyzer must be scaled up to greater hydrogen production capacities. SRNL and Air Products entered into a Cooperative Research and Development Agreement with the objective of demonstrating the effectiveness of the SDE for hydrogen and sulfuric acid production and to demonstrate long-term continuous operation so as to dramatically increase the confidence in the SDE design for commercial operation. SRNL prepared a detailed technical report documenting previous SDE development, including the current SDE design and operating conditions that led to the 200-hour sulfurfree testing. SRNL refurbished its single cell SDE test facility and qualified the equipment for continuous operation. A new membrane electrode assembly (MEA) was fabricated and installed in the single cell electrolyzer (60 cm 2 active cell area). Shakedown testing was conducted, and several modifications were made to the test facility equipment. Seven different MEAs were used during testing. Beginning on May 20, 2013, SRNL was able to test the SDE continuously for 1200 hours, including 1000 hours under power to generate hydrogen at an average rate of 10.8 liters per hour. The SDE was not removed or repaired during the 50-day test and was successfully restarted after each shutdown. The test was intentionally stopped after 1200 hours (1000 hours of hydrogen production) due to funding constraints. Post-test examination of the MEA using Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Microanalysis (EDAX) showed no elemental sulfur deposits or sulfur layer inside the cell, thus successfully achieving the test goals. The results demonstrated that the SDE could be operated for extended periods without major performance degradation or the buildup of sulfur inside the MEA. Air Products conducted an assessment of the economic viability of the SDE based on the “as tested” design. The results indicated that the SDE faces significant economic obstacles in its current state. Further development and scale-up are necessary before the SDE is ready for commercialization.« less

STATISTICAL ANALYSIS OF TANK 5 FLOOR SAMPLE RESULTS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shine, E.

2012-03-14

Sampling has been completed for the characterization of the residual material on the floor of Tank 5 in the F-Area Tank Farm at the Savannah River Site (SRS), near Aiken, SC. The sampling was performed by Savannah River Remediation (SRR) LLC using a stratified random sampling plan with volume-proportional compositing. The plan consisted of partitioning the residual material on the floor of Tank 5 into three non-overlapping strata: two strata enclosed accumulations, and a third stratum consisted of a thin layer of material outside the regions of the two accumulations. Each of three composite samples was constructed from five primarymore » sample locations of residual material on the floor of Tank 5. Three of the primary samples were obtained from the stratum containing the thin layer of material, and one primary sample was obtained from each of the two strata containing an accumulation. This report documents the statistical analyses of the analytical results for the composite samples. The objective of the analysis is to determine the mean concentrations and upper 95% confidence (UCL95) bounds for the mean concentrations for a set of analytes in the tank residuals. The statistical procedures employed in the analyses were consistent with the Environmental Protection Agency (EPA) technical guidance by Singh and others [2010]. Savannah River National Laboratory (SRNL) measured the sample bulk density, nonvolatile beta, gross alpha, radionuclide, inorganic, and anion concentrations three times for each of the composite samples. The analyte concentration data were partitioned into three separate groups for further analysis: analytes with every measurement above their minimum detectable concentrations (MDCs), analytes with no measurements above their MDCs, and analytes with a mixture of some measurement results above and below their MDCs. The means, standard deviations, and UCL95s were computed for the analytes in the two groups that had at least some measurements above their MDCs. The identification of distributions and the selection of UCL95 procedures generally followed the protocol in Singh, Armbya, and Singh [2010]. When all of an analyte's measurements lie below their MDCs, only a summary of the MDCs can be provided. The measurement results reported by SRNL are listed in Appendix A, and the results of this analysis are reported in Appendix B. The data were generally found to follow a normal distribution, and to be homogeneous across composite samples.« less

Statistical Analysis of Tank 5 Floor Sample Results

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shine, E. P.

2013-01-31

Sampling has been completed for the characterization of the residual material on the floor of Tank 5 in the F-Area Tank Farm at the Savannah River Site (SRS), near Aiken, SC. The sampling was performed by Savannah River Remediation (SRR) LLC using a stratified random sampling plan with volume-proportional compositing. The plan consisted of partitioning the residual material on the floor of Tank 5 into three non-overlapping strata: two strata enclosed accumulations, and a third stratum consisted of a thin layer of material outside the regions of the two accumulations. Each of three composite samples was constructed from five primarymore » sample locations of residual material on the floor of Tank 5. Three of the primary samples were obtained from the stratum containing the thin layer of material, and one primary sample was obtained from each of the two strata containing an accumulation. This report documents the statistical analyses of the analytical results for the composite samples. The objective of the analysis is to determine the mean concentrations and upper 95% confidence (UCL95) bounds for the mean concentrations for a set of analytes in the tank residuals. The statistical procedures employed in the analyses were consistent with the Environmental Protection Agency (EPA) technical guidance by Singh and others [2010]. Savannah River National Laboratory (SRNL) measured the sample bulk density, nonvolatile beta, gross alpha, and the radionuclide1, elemental, and chemical concentrations three times for each of the composite samples. The analyte concentration data were partitioned into three separate groups for further analysis: analytes with every measurement above their minimum detectable concentrations (MDCs), analytes with no measurements above their MDCs, and analytes with a mixture of some measurement results above and below their MDCs. The means, standard deviations, and UCL95s were computed for the analytes in the two groups that had at least some measurements above their MDCs. The identification of distributions and the selection of UCL95 procedures generally followed the protocol in Singh, Armbya, and Singh [2010]. When all of an analyte's measurements lie below their MDCs, only a summary of the MDCs can be provided. The measurement results reported by SRNL are listed, and the results of this analysis are reported. The data were generally found to follow a normal distribution, and to be homogenous across composite samples.« less

Statistical Analysis Of Tank 5 Floor Sample Results

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shine, E. P.

2012-08-01

Sampling has been completed for the characterization of the residual material on the floor of Tank 5 in the F-Area Tank Farm at the Savannah River Site (SRS), near Aiken, SC. The sampling was performed by Savannah River Remediation (SRR) LLC using a stratified random sampling plan with volume-proportional compositing. The plan consisted of partitioning the residual material on the floor of Tank 5 into three non-overlapping strata: two strata enclosed accumulations, and a third stratum consisted of a thin layer of material outside the regions of the two accumulations. Each of three composite samples was constructed from five primarymore » sample locations of residual material on the floor of Tank 5. Three of the primary samples were obtained from the stratum containing the thin layer of material, and one primary sample was obtained from each of the two strata containing an accumulation. This report documents the statistical analyses of the analytical results for the composite samples. The objective of the analysis is to determine the mean concentrations and upper 95% confidence (UCL95) bounds for the mean concentrations for a set of analytes in the tank residuals. The statistical procedures employed in the analyses were consistent with the Environmental Protection Agency (EPA) technical guidance by Singh and others [2010]. Savannah River National Laboratory (SRNL) measured the sample bulk density, nonvolatile beta, gross alpha, and the radionuclide, elemental, and chemical concentrations three times for each of the composite samples. The analyte concentration data were partitioned into three separate groups for further analysis: analytes with every measurement above their minimum detectable concentrations (MDCs), analytes with no measurements above their MDCs, and analytes with a mixture of some measurement results above and below their MDCs. The means, standard deviations, and UCL95s were computed for the analytes in the two groups that had at least some measurements above their MDCs. The identification of distributions and the selection of UCL95 procedures generally followed the protocol in Singh, Armbya, and Singh [2010]. When all of an analyte's measurements lie below their MDCs, only a summary of the MDCs can be provided. The measurement results reported by SRNL are listed in Appendix A, and the results of this analysis are reported in Appendix B. The data were generally found to follow a normal distribution, and to be homogenous across composite samples.« less

Solvent Hold Tank Sample Results for MCU-15-661-662-663: April 2015 Monthly Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F.; Taylor-Pashow, K.

2015-07-08

The Savannah River National Lab (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-15-661, MCU-15-662, and MCU-15-663 pulled on April 2, 2015) for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-15-661-662-663 indicated a low concentration (~ 63% of nominal) of the suppressor (TiDG) and a slightly below the nominal concentration (~ 10% below nominal) of the extractant (MaxCalix). The modifier (CS-7SB) level was also 10% below its nominal value while the Isopar™ L level was slightly above its nominal value. This analysis confirms the addition of Isopar™L to the solvent onmore » March 6, 2015. Despite that the values are below target component levels, the current levels of TiDG, CS-7SB and MaxCalix are sufficient for continuing operation without adding a trim at this time until the next monthly sample. No impurities above the 1000 ppm level were found in this solvent. However, the sample was found to contain approximately 18.4 ug/g solvent mercury. The gamma level increased to 8 E5 dpm/mL solvent and it represents an order of magnitude increase relative to previous solvent samples. The increase means less cesium is being stripped from the solvent. Further analysis is needed to determine if the recent spike in the gamma measurement is due to external factors such as algae or other material that may impede stripping. The laboratory will continue to monitor the quality of the solvent in particular for any new impurity or degradation of the solvent components.« less

Solvent hold tank sample results for MCU-15-914-915-916. December 2015 Monthly sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Jones, D. H.

2016-03-01

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-15-914-915-916), pulled on 12/22/2015 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-15-914-915-916 indicated the TiDG, Isopar™L, and MaxCalix are at nominal levels. The modifier concentration is 3% below its nominal concentration. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent in November 2015. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additionsmore » to the solvent are recommended. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). However, the Fourier transform infra-red spectroscopy (FTIR) method detected trace levels (a few ppm) of amides (more indicative of bacteria than a possible degradation product of TiDG). In addition, up to 18 ± 4 micrograms of mercury per gram of solvent (or 14.8 μg/mL) was detected in this sample. The current gamma concentration level (8.48E4 dpm/mL) confirmed that the gamma concentration has returned to the previous level where the process operated normally as expected. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.« less

Solvent hold tank sample results for MCU-16-53-55. January 2016 Monthly sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Jones, D. H.

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-53-54-55), pulled on 01/25/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-53-54-55 indicated the Isopar™L, and MaxCalix are at nominal levels. The modifier and TiDG concentrations are 3% and 23 % below their nominal concentrations. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent on November 28, 2015. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time.more » Periodic characterization and trimming additions to the solvent are recommended. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). However, the Fourier transform infra-red spectroscopy (FTIR) method detected trace levels (a few ppm) of amides (a possible degradation product of TiDG). In addition, up to 21 ± 4 micrograms of mercury per gram of solvent (or 17.5 μg/mL) was detected in this sample. There appears to be a possible correlation between the mercury level and the TiDG concentration in the solvent. The current gamma level (9.16 E4 dpm/mL) confirmed that the gamma concentration has returned to previous level where the process operated normally and as expected. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.« less

STATISTICAL ANALYSIS OF TANK 18F FLOOR SAMPLE RESULTS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harris, S.

2010-09-02

Representative sampling has been completed for characterization of the residual material on the floor of Tank 18F as per the statistical sampling plan developed by Shine [1]. Samples from eight locations have been obtained from the tank floor and two of the samples were archived as a contingency. Six samples, referred to in this report as the current scrape samples, have been submitted to and analyzed by SRNL [2]. This report contains the statistical analysis of the floor sample analytical results to determine if further data are needed to reduce uncertainty. Included are comparisons with the prior Mantis samples resultsmore » [3] to determine if they can be pooled with the current scrape samples to estimate the upper 95% confidence limits (UCL{sub 95%}) for concentration. Statistical analysis revealed that the Mantis and current scrape sample results are not compatible. Therefore, the Mantis sample results were not used to support the quantification of analytes in the residual material. Significant spatial variability among the current sample results was not found. Constituent concentrations were similar between the North and South hemispheres as well as between the inner and outer regions of the tank floor. The current scrape sample results from all six samples fall within their 3-sigma limits. In view of the results from numerous statistical tests, the data were pooled from all six current scrape samples. As such, an adequate sample size was provided for quantification of the residual material on the floor of Tank 18F. The uncertainty is quantified in this report by an upper 95% confidence limit (UCL{sub 95%}) on each analyte concentration. The uncertainty in analyte concentration was calculated as a function of the number of samples, the average, and the standard deviation of the analytical results. The UCL{sub 95%} was based entirely on the six current scrape sample results (each averaged across three analytical determinations).« less

STATISTICAL ANALYSIS OF TANK 19F FLOOR SAMPLE RESULTS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harris, S.

2010-09-02

Representative sampling has been completed for characterization of the residual material on the floor of Tank 19F as per the statistical sampling plan developed by Harris and Shine. Samples from eight locations have been obtained from the tank floor and two of the samples were archived as a contingency. Six samples, referred to in this report as the current scrape samples, have been submitted to and analyzed by SRNL. This report contains the statistical analysis of the floor sample analytical results to determine if further data are needed to reduce uncertainty. Included are comparisons with the prior Mantis samples resultsmore » to determine if they can be pooled with the current scrape samples to estimate the upper 95% confidence limits (UCL95%) for concentration. Statistical analysis revealed that the Mantis and current scrape sample results are not compatible. Therefore, the Mantis sample results were not used to support the quantification of analytes in the residual material. Significant spatial variability among the current scrape sample results was not found. Constituent concentrations were similar between the North and South hemispheres as well as between the inner and outer regions of the tank floor. The current scrape sample results from all six samples fall within their 3-sigma limits. In view of the results from numerous statistical tests, the data were pooled from all six current scrape samples. As such, an adequate sample size was provided for quantification of the residual material on the floor of Tank 19F. The uncertainty is quantified in this report by an UCL95% on each analyte concentration. The uncertainty in analyte concentration was calculated as a function of the number of samples, the average, and the standard deviation of the analytical results. The UCL95% was based entirely on the six current scrape sample results (each averaged across three analytical determinations).« less

Identification And Characterization Of The Solids Found In Extraction Contactor SEP-401 In June 2012

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Fink, S. D.

2012-12-10

The Modular Caustic-Side Solvent Extraction Unit (MCU) recently conducted an outage that included maintenance on the centrifugal contactors. Operations personnel observed solids or deposits in two contactors and attempted to collect samples for analyses by Savannah River National Laboratory (SRNL). The residues found in Extraction Contactor SEP-401 are a mixture of amorphous silica, aluminosilicate, titanium, and debris from low alloy steel. The solids contain low concentrations of plutonium and strontium. These isotopes are associated with the titanium that came from the monosodium titanate (MST) added in the Actinide Removal Process (ARP) most likely as leached Ti from the MST thatmore » precipitated subsequently in MCU. An attempt was also made to obtain samples from the contents of Wash Contactor SEP-702. However, sampling provide ineffective.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Restivo, M.

SRNL Environmental and Chemical Process Technology (E&CPT) was requested to perform testing of vacuum pumps per a verbal request from the Customer, SRNL Hydrogen Processing Technology. Tritium Operations is currently having difficulties procuring the Normetex™® Model 15 m 3/hr (9 CFM) vacuum pump (formerly Normetex Pompes, now Eumeca SARL). One possible solution proposed by Hydrogen Processing Technology personnel is to use two Senior Aerospace Metal Bellows MB-601 vacuum pumps piped with the heads in series, and the pumps in series (Figure 1 below). This memorandum documents the ultimate vacuum testing that was performed to determine if this concept was amore » viable alternate vacuum pump strategy. This testing dovetails with previous pump evaluations documented in references 1 and 2.« less

2013 SRNL LDRD Annual Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

McWhorter, S.

2014-03-07

This report demonstrates the execution of our LDRD program within the objectives and guidelines outlined by the Department of Energy (DOE) through the DOE Order 413.2b. The projects described within the report align purposefully with SRNL’s strategic vision and provide great value to the DOE. The diversity exhibited in the research and development projects underscores the DOE Office of Environmental Management (DOE-EM) mission and enhances that mission by developing the technical capabilities and human capital necessary to support future DOE-EM national needs. As a multiprogram national laboratory, SRNL is applying those capabilities to achieve tangible results for the nation inmore » National Security, Environmental Stewardship, Clean Energy and Nuclear Materials Management.« less

PILOT-SCALE REMOVAL OF FLUORIDE FROM LEGACY PLUTONIUM MATERIALS USING VACUUM SALT DISTILLATION

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pierce, R. A.; Pak, D. J.

2012-09-11

Between September 2009 and January 2011, the Savannah River National Laboratory (SRNL) and HB-Line designed, developed, tested, and successfully deployed a system for the distillation of chloride salts. In 2011, SRNL adapted the technology for the removal of fluoride from fluoride-bearing salts. The method involved an in situ reaction between potassium hydroxide (KOH) and the fluoride salt to yield potassium fluoride (KF) and the corresponding oxide. The KF and excess KOH can be distilled below 1000{deg}C using vacuum salt distillation (VSD). The apparatus for vacuum distillation contains a zone heated by a furnace and a zone actively cooled using eithermore » recirculated water or compressed air. During a vacuum distillation operation, a sample boat containing the feed material is placed into the apparatus while it is cool, and the system is sealed. The system is evacuated using a vacuum pump. Once a sufficient vacuum is attaned, heating begins. Volatile salts distill from the heated zone to the cooled zone where they condense, leaving behind the non-volatile material in the feed boat. Studies discussed in this report were performed involving the use of non-radioactive simulants in small-scale and pilot-scale systems as well as radioactive testing of a small-scale system with plutonium-bearing materials. Aspects of interest include removable liner design considerations, boat materials, in-line moisture absorption, and salt deposition.« less

CHARACTERIZATION OF A PRECIPITATE REACTOR FEED TANK (PRFT) SAMPLE FROM THE DEFENSE WASTE PROCESSING FACILITY (DWPF)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Crawford, C.; Bannochie, C.

2014-05-12

A sample of from the Defense Waste Processing Facility (DWPF) Precipitate Reactor Feed Tank (PRFT) was pulled and sent to the Savannah River National Laboratory (SRNL) in June of 2013. The PRFT in DWPF receives Actinide Removal Process (ARP)/ Monosodium Titanate (MST) material from the 512-S Facility via the 511-S Facility. This 2.2 L sample was to be used in small-scale DWPF chemical process cell testing in the Shielded Cells Facility of SRNL. A 1L sub-sample portion was characterized to determine the physical properties such as weight percent solids, density, particle size distribution and crystalline phase identification. Further chemical analysismore » of the PRFT filtrate and dissolved slurry included metals and anions as well as carbon and base analysis. This technical report describes the characterization and analysis of the PRFT sample from DWPF. At SRNL, the 2.2 L PRFT sample was composited from eleven separate samples received from DWPF. The visible solids were observed to be relatively quick settling which allowed for the rinsing of the original shipping vials with PRFT supernate on the same day as compositing. Most analyses were performed in triplicate except for particle size distribution (PSD), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and thermogravimetric analysis (TGA). PRFT slurry samples were dissolved using a mixed HNO3/HF acid for subsequent Inductively Coupled Plasma Atomic Emission Spectroscopy (ICPAES) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) analyses performed by SRNL Analytical Development (AD). Per the task request for this work, analysis of the PRFT slurry and filtrate for metals, anions, carbon and base were primarily performed to support the planned chemical process cell testing and to provide additional component concentrations in addition to the limited data available from DWPF. Analysis of the insoluble solids portion of the PRFT slurry was aimed at detailed characterization of these solids (TGA, PSD, XRD and SEM) in support of the Salt IPT chemistry team. The overall conclusions from analyses performed in this study are that the PRFT slurry consists of 0.61 Wt.% insoluble MST solids suspended in a 0.77 M [Na+] caustic solution containing various anions such as nitrate, nitrite, sulfate, carbonate and oxalate. The corresponding measured sulfur level in the PRFT slurry, a critical element for determining how much of the PRFT slurry gets blended into the SRAT, is 0.437 Wt.% TS. The PRFT slurry does not contain insoluble oxalates nor significant quantities of high activity sludge solids. The lack of sludge solids has been alluded to by the Salt IPT chemistry team in citing that the mixing pump has been removed from Tank 49H, the feed tank to ARP-MCU, thus allowing the sludge solids to settle out. The PRFT aqueous slurry from DWPF was found to contain 5.96 Wt.% total dried solids. Of these total dried solids, relatively low levels of insoluble solids (0.61 Wt.%) were measured. The densities of both the filtrate and slurry were 1.05 g/mL. Particle size distribution of the PRFT solids in filtered caustic simulant and XRD analysis of washed/dried PRFT solids indicate that the PRFT slurry contains a bimodal distribution of particles in the range of 1 and 6 μm and that the particles contain sodium titanium oxide hydroxide Na2Ti2O4(OH)2 crystalline material as determined by XRD. These data are in excellent agreement with similar data obtained from laboratory sampling of vendor supplied MST. Scanning Electron Microscopy (SEM) combined with Energy Dispersive X-ray Spectroscopy (EDS) analysis of washed/dried PRFT solids shows the particles to be like previous MST analyses consisting of irregular shaped micron-sized solids consisting primarily of Na and Ti. Thermogravimetric analysis of the washed and unwashed PRFT solids shows that the washed solids are very similar to MST solids. The TGA mass loss signal for the unwashed solids shows similar features to TGA performed on cellulose nitrate filter paper indicating significant presence of the deteriorated filter in this unwashed sample. Neither the washed nor unwashed PRFT solids TGA traces showed any features that would indicate presence of sodium oxalate solids. The PRFT Filtrate elemental analysis shows that Na, S and Al are major soluble species with trace levels of B, Cr, Cu, K, Li, Si, Tc, Th and U present. Nitrate, nitrite, sulfate, oxalate, carbonate and hydroxide are major soluble anion species. There is good agreement between the analyzed TOC and the total carbon calculated from the sum of oxalate and minor species formate. Comparison of the amount and speciation of the carbon species between filtrate and slurry indicates no significant carbon-containing species, e.g., sodium oxalate, are present in the slurry solids. Dissolution of the PRFT slurry and subsequent analysis shows that Na, Ti, Si and U are the major elements present on a Wt.% total dried solids basis with 30, 5.8 and 0.47 and 0.11 Wt.% total dried solids, respectively. The amount of Al in the dissolved PRFT slurry is less than that calculated from the PRFT filtrate alone which suggests that the mixed acid digestion used in this work is not optimized for Al recovery. The concentrations of Ca, Fe, Hg and U are all low (at or below 0.11 wt%) and there is no detectable Mn or Ni present which indicates no significant HLW sludge solids are present in the PRFT slurry sample.« less

Rapid fusion method for the determination of Pu, Np, and Am in large soil samples

DOE PAGES

Maxwell, Sherrod L.; Culligan, Brian; Hutchison, Jay B.; ...

2015-02-14

A new rapid sodium hydroxide fusion method for the preparation of 10-20 g soil samples has been developed by the Savannah River National Laboratory (SRNL). The method enables lower detection limits for plutonium, neptunium, and americium in environmental soil samples. The method also significantly reduces sample processing time and acid fume generation compared to traditional soil digestion techniques using hydrofluoric acid. Ten gram soil aliquots can be ashed and fused using the new method in 1-2 hours, completely dissolving samples, including refractory particles. Pu, Np and Am are separated using stacked 2mL cartridges of TEVA and DGA Resin and measuredmore » using alpha spectrometry. The method can be adapted for measurement by inductively-coupled plasma mass spectrometry (ICP-MS). Two 10 g soil aliquots of fused soil may be combined prior to chromatographic separations to further improve detection limits. Total sample preparation time, including chromatographic separations and alpha spectrometry source preparation, is less than 8 hours.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Taylor-Pashow, K.; Fondeur, F.; White, T.

Savannah River National Laboratory (SRNL) was tasked with identifying and developing at least one, but preferably two methods for quantifying the suppressor in the Next Generation Solvent (NGS) system. The suppressor is a guanidine derivative, N,N',N"-tris(3,7-dimethyloctyl)guanidine (TiDG). A list of 10 possible methods was generated, and screening experiments were performed for 8 of the 10 methods. After completion of the screening experiments, the non-aqueous acid-base titration was determined to be the most promising, and was selected for further development as the primary method. {sup 1}H NMR also showed promising results from the screening experiments, and this method was selected formore » further development as the secondary method. Other methods, including {sup 36}Cl radiocounting and ion chromatography, also showed promise; however, due to the similarity to the primary method (titration) and the inability to differentiate between TiDG and TOA (tri-n-ocytlamine) in the blended solvent, {sup 1}H NMR was selected over these methods. Analysis of radioactive samples obtained from real waste ESS (extraction, scrub, strip) testing using the titration method showed good results. Based on these results, the titration method was selected as the method of choice for TiDG measurement. {sup 1}H NMR has been selected as the secondary (back-up) method, and additional work is planned to further develop this method and to verify the method using radioactive samples. Procedures for analyzing radioactive samples of both pure NGS and blended solvent were developed and issued for the both methods.« less

TAGGING, TRACKING AND LOCATING WITHOUT GPS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cordaro, J.; Coleman, T.; Shull, D.

The Savannah River National Laboratory (SRNL) was requested to lead a Law Enforcement Working Group that was formed to collaborate on common operational needs. All agencies represented on the working group ranked their need to tag, track, and locate a witting or unwitting target as their highest priority. Specifically, they were looking for technologies more robust than Global Positioning Satellite (GPS), could communicate back to the owner, and worked where normal cell phone communications did not work or were unreliable. SRNL brought together multiple technologies in a demonstration that was held in in various Alaska venues, including metropolitan, wilderness, andmore » at-sea that met the working group's requirements. Using prototypical technologies from Boeing, On Ramp, and Fortress, SRNL was able to demonstrate the ability to track personnel and material in all scenarios including indoors, in heavily wooden areas, canyons, and in parking garages. In all cases GPS signals were too weak to measure. Bi-directional communication was achieved in areas that Wi-Fi, cell towers, or traditional radios would not perform. The results of the exercise will be presented. These technologies are considered ideal for tracking high value material such has nuclear material with a platform that allows seamless tracking anywhere in the world, indoors or outdoors.« less

Solvent Hold Tank Sample Results for MCU-16-991-992-993: July 2016 Monthly sample and MCU-16-1033-1034-1035: July 2016 Superwashed Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F.; Jones, D.

SRNL received one set of SHT samples (MCU-16-991, MCU-16-992 and MCU-16-993), pulled on 07/13/2016 and another set of SHT samples (MCU-16-1033, MCU-16-1034, and MCU-16-1035) that were pulled on 07/24/2016 after the solvent was superwashed with 300 mM sodium hydroxide for analysis. Samples MCU-16-991, MCU-16-992, and MCU-16-993 were combined into one sample (MCU-16-991-992-993) and samples MCU-16-1033, MCU-16-1034, and MCU-16-1035 were combined into one sample (MCU-16-1033-1034-1035). Of the two composite samples MCU-16-1033-1034-1035 represents the current chemical state of the solvent at MCU. All analytical conclusions are based on the chemical analysis of MCU-16-1033-1034-1035. There were no chemical differences between MCU-16- 991-992-993 andmore » superwashed MCU-16-1033-1034-1035.« less

Characterization of DWPF recycle condensate materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.; Adamson, D. J.; King, W. D.

2015-04-01

A Defense Waste Processing Facility (DWPF) Recycle Condensate Tank (RCT) sample was delivered to the Savannah River National Laboratory (SRNL) for characterization with particular interest in the concentration of I-129, U-233, U-235, total U, and total Pu. Since a portion of Salt Batch 8 will contain DWPF recycle materials, the concentration of I-129 is important to understand for salt batch planning purposes. The chemical and physical characterizations are also needed as input to the interpretation of future work aimed at determining the propensity of the RCT material to foam, and methods to remediate any foaming potential. According to DWPF themore » Tank Farm 2H evaporator has experienced foaming while processing DWPF recycle materials. The characterization work on the RCT samples has been completed and is reported here.« less

Verification Of The Defense Waste Processing Facility's (DWPF) Process Digestion Methods For The Sludge Batch 8 Qualification Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Click, D. R.; Edwards, T. B.; Wiedenman, B. J.

2013-03-18

This report contains the results and comparison of data generated from inductively coupled plasma – atomic emission spectroscopy (ICP-AES) analysis of Aqua Regia (AR), Sodium Peroxide/Sodium Hydroxide Fusion Dissolution (PF) and Cold Chem (CC) method digestions and Cold Vapor Atomic Absorption analysis of Hg digestions from the DWPF Hg digestion method of Sludge Batch 8 (SB8) Sludge Receipt and Adjustment Tank (SRAT) Receipt and SB8 SRAT Product samples. The SB8 SRAT Receipt and SB8 SRAT Product samples were prepared in the SRNL Shielded Cells, and the SRAT Receipt material is representative of the sludge that constitutes the SB8 Batch ormore » qualification composition. This is the sludge in Tank 51 that is to be transferred into Tank 40, which will contain the heel of Sludge Batch 7b (SB7b), to form the SB8 Blend composition.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, C.; Brigmon, R.

Legionnaires disease is a pneumonia caused by the inhalation of the bacterium Legionella pneumophila. The majority of illnesses have been associated with cooling towers since these devices can harbor and disseminate the bacterium in the aerosolized mist generated by these systems. Historically, Savannah River Site (SRS) cooling towers have had occurrences of elevated levels of Legionella in all seasons of the year and in patterns that are difficult to predict. Since elevated Legionella in cooling tower water are a potential health concern a question has been raised as to the best control methodology. In this work we analyze available chemical,more » biological, and atmospheric data to determine the best method or key parameter for control. The SRS 4Q Industrial Hygiene Manual, 4Q-1203, 1 - G Cooling Tower Operation and the SRNL Legionella Sampling Program, states that 'Participation in the SRNL Legionella Sampling Program is MANDATORY for all operating cooling towers'. The resulting reports include L. pneumophila concentration information in cells/L. L. pneumophila concentrations >10{sup 7} cells/L are considered elevated and unsafe so action must be taken to reduce these densities. These remedial actions typically include increase biocide addition or 'shocking'. Sometimes additional actions are required if the problem persists including increase tower maintenance (e.g. cleaning). Evaluation of 14 SRS cooling towers, seven water quality parameters, and five Legionella serogroups over a three-plus year time frame demonstrated that cooling tower water Legionella densities varied widely though out this time period. In fact there was no one common consistent significant variable across all towers. The significant factors that did show up most frequently were related to suspended particulates, conductivity, pH, and dissolved oxygen, not chlorine or bromine as might be expected. Analyses of atmospheric data showed that there were more frequent significant elevated Legionella concentrations when the dew point temperature was high--a summertime occurrence. However, analysis of the three years of Legionella monitoring data of the 14 different SRS Cooling Towers demonstrated that elevated concentrations are observed at all temperatures and seasons. The objective of this study is to evaluate the ecology of L. pneumophila including serogroups and population densities, chemical, and atmospheric data, on cooling towers at SRS to determine whether relationships exist among water chemistry, and atmospheric conditions. The goal is to more fully understand the conditions which inhibit or encourage L. pneumophila growth and supply this data and associated recommendations to SRS Cooling Tower personnel for improved management of operation. Hopefully this information could then be used to help control L. pneumophila growth more effectively in SRS cooling tower water.« less

Rapid fusion method for the determination of refractory thorium and uranium isotopes in soil samples

DOE PAGES

Maxwell, Sherrod L.; Hutchison, Jay B.; McAlister, Daniel R.

2015-02-14

Recently, approximately 80% of participating laboratories failed to accurately determine uranium isotopes in soil samples in the U.S Department of Energy Mixed Analyte Performance Evaluation Program (MAPEP) Session 30, due to incomplete dissolution of refractory particles in the samples. Failing laboratories employed acid dissolution methods, including hydrofluoric acid, to recover uranium from the soil matrix. The failures illustrate the importance of rugged soil dissolution methods for the accurate measurement of analytes in the sample matrix. A new rapid fusion method has been developed by the Savannah River National Laboratory (SRNL) to prepare 1-2 g soil sample aliquots very quickly, withmore » total dissolution of refractory particles. Soil samples are fused with sodium hydroxide at 600 ºC in zirconium crucibles to enable complete dissolution of the sample. Uranium and thorium are separated on stacked TEVA and TRU extraction chromatographic resin cartridges, prior to isotopic measurements by alpha spectrometry on cerium fluoride microprecipitation sources. Plutonium can also be separated and measured using this method. Batches of 12 samples can be prepared for measurement in <5 hours.« less

Hanford Tank Farm Vapors Abatement Technology and Vendor Proposals Assessment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Burns, H. H.; Farrar, M. E.; Fink, S. D.

2016-09-20

Suspected chemical vapor releases from the Hanford nuclear waste tank system pose concerns for worker exposure. Washington River Protection Solutions (WRPS) contracted the Savannah River National Laboratory (SRNL) to explore abatement technologies and strategies to remediate the vapors emitted through the ventilation system. In response, SRNL conducted an evaluation of technologies to abate, or reduce, vapor emissions to below 10% of the recognized occupational exposure limits (OELs). The evaluation included a review of published literature and a broadly communicated Request for Information to commercial vendors through a Federal Business Opportunities (Fed Biz Opps) web posting. In addition, SRNL conducted amore » workshop and post-workshop conference calls with interested suppliers (vendors) to assess proposals of relevant technologies. This report reviews applicable technologies and summarizes the approaches proposed by the vendors who participated in the workshop and teleconference interviews. In addition, the report evaluates the estimated performance of the individual technologies for the various classes of chemical compounds present in the Hanford Chemicals of Potential Concern (COPCs) list. Similarly, the report provides a relative evaluation of the vendor proposed approaches against criteria of: technical feasibility (and maturity), design features, operational considerations, secondary waste generation, safety/regulatory, and cost / schedule. These rough order-of-magnitude (ROM) cost estimates are intended to provide a comparison basis between technologies and are not intended to be actual project estimates.« less

Biota dose assessment of small mammals sampled near uranium mines in northern Arizona

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jannik, T.; Minter, K.; Kuhne, W.

In 2015, the U. S. Geological Survey (USGS) collected approximately 50 small mammal carcasses from Northern Arizona uranium mines and other background locations. Based on the highest gross alpha results, 11 small mammal samples were selected for radioisotopic analyses. None of the background samples had significant gross alpha results. The 11 small mammals were identified relative to the three ‘indicator’ mines located south of Fredonia, AZ on the Kanab Plateau (Kanab North Mine, Pinenut Mine, and Arizona 1 Mine) (Figure 1-1) and are operated by Energy Fuels Resources Inc. (EFRI). EFRI annually reports soil analysis for uranium and radium-226 usingmore » Arizona Department of Environmental Quality (ADEQ)-approved Standard Operating Procedures for Soil Sampling (EFRI 2016a, 2016b, 2017). In combination with the USGS small mammal radioiosotopic tissue analyses, a biota dose assessment was completed by Savannah River National Laboratory (SRNL) using the RESidual RADioactivity-BIOTA (RESRAD-BIOTA, V. 1.8) dose assessment tool provided by the Argonne National Laboratory (ANL 2017).« less

Baseline process description for simulating plutonium oxide production for precalc project

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pike, J. A.

Savannah River National Laboratory (SRNL) started a multi-year project, the PreCalc Project, to develop a computational simulation of a plutonium oxide (PuO 2) production facility with the objective to study the fundamental relationships between morphological and physicochemical properties. This report provides a detailed baseline process description to be used by SRNL personnel and collaborators to facilitate the initial design and construction of the simulation. The PreCalc Project team selected the HB-Line Plutonium Finishing Facility as the basis for a nominal baseline process since the facility is operational and significant model validation data can be obtained. The process boundary as wellmore » as process and facility design details necessary for multi-scale, multi-physics models are provided.« less

Characterization of Laboratory Prepared Concrete Pastes Exposed to High Alkaline and High Sodium Salt Solutions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Langton, C. A.

The objective of this study was to identify potential chemical degradation mechanisms for the Saltstone Disposal Unit (SDU) concretes, which over the performance life of the structures may be exposed to highly alkaline sodium salt solutions containing sulfate, hydroxide, and other potentially corrosive chemicals in salt solution and saltstone flush water, drain water, leachate and / or pore solution. The samples analyzed in this study were cement pastes prepared in the SIMCO Technologies, Inc. concrete laboratory. They were based on the paste fractions of the concretes used to construct the Saltstone Disposal Units (SDUs). SDU 1 and 4 concrete pastesmore » were represented by the PV1 test specimens. The paste in the SDU 2, 3, 5, and 6 concrete was represented by the PV2 test specimens. SIMCO Technologies, Inc. selected the chemicals and proportions in the aggressive solutions to approximate proportions in the saltstone pore solution [2, 3, 5, and 6]. These test specimens were cured for 56 days in curing chamber before being immersed in aggressive solutions. After exposure, the samples were frozen to prevent additional chemical transport and reaction. Selected archived (retrieved from the freezer) samples were sent to the Savannah River National Laboratory (SRNL) for additional characterization using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive x-ray (EDX) spectroscopy. Characterization results are summarized in this report. In addition, a correlation between the oxide composition of the pastes and their chemical durability in the alkaline salt solutions is provided.« less

Reconfirmation of frit 803 based on the January 2016 sludge batch 9 reprojection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Johnson, F.; Edwards, T.

2016-02-10

On January 11, 2016, Savannah River Remediation (SRR) provided the Savannah River National Laboratory (SRNL) with a Sludge Batch 9 (SB9) reprojection that was developed from the analyzed composition of a Tank 51 sample. This sample was collected after field washing had been completed in Tank 51 to support the alternate reductant task. Based on this reprojection, Frit 803 is still a viable option for the processing of SB9 under sludge-only operations and coupled (Actinide Removal Process (ARP) product with and without monosodium titanate (MST)) operations. The maximum projected volumes of ARP product that can be transferred from the Precipitatemore » Reactor Feed Tank (PRFT) per Sludge Receipt and Adjustment Tank (SRAT) batch and the resulting Na 2O concentrations in the SRAT for coupled operations were determined. The Na 2O concentrations in the SRAT resulting from the maximum projected ARP product transfer volumes are consistent with those from the previous assessments that were based on the August 2015 projections. Regardless of the presence or absence of MST in the ARP product, the contribution of Na 2O to the resulting glass will be similar at the same waste loading (WL). These projected volumes of ARP product are not anticipated to be an issue for SB9. The actual transfer volumes from the PRFT to the SRAT are determined based upon the analyzed Na 2O concentrations in the PRFT samples, which has resulted in larger transfer volumes than those allowed by the projections for Sludge Batch 8 (SB8). An operating window of 32-40% WL around the nominal WL of 36% is achievable for both sludge-only and coupled operations; however, each of the glass systems studied does become limited by waste form affecting constraints (durability) at higher volumes of ARP product and WLs of 41-42%.« less

Method development for thermal analyses testing on Reillex HPQ resin using the advanced reactive system screening tool (ARSST)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Best, D.

Reillex™ HPQ resin was developed by Los Alamos Laboratory and Reilly Industries Inc. in an effort to increase safety and process efficiency during the recovery and purification of plutonium. Ionac™ A-641, another strong base macroporous anion exchange resin used in the nuclear industry, was known to undergo a runaway reaction in hot nitric acid solutions. Because of this, an extensive amount of thermal analyses testing on the Reillex™ HPQ resin in SRNL was performed in 1999-2001 prior to use. A report on the thermal stability qualification of the Reillex™ HPQ resin in 8M (35%) and 12M (53%) HNO 3 wasmore » reported in 2000. In 2001, the reactivity of Reillex™ HPQ resin in 14.4M (64%) HNO 3 was evaluated. In January of 2001, thermal stability scoping tests were performed on irradiated Reillex™ HPQ resin in 14.4M (64%) HNO 3 (as a worst case scenario) and the results sent to Fauske and Associates to calculate a rupture disk size for the HB-Line resin column. A technical report by Fauske and Associates was issued in February 2001 recommending a 2.0” vent line with a rupture disk set pressure of 60 psig. This calculation was based on ARSST thermal analyses scoping tests at SRNL in which 4 grams of dried resin and 6.0 grams of 64% nitric acid in a 10 gram test cell, produced a maximum pressure rate (dP/dt) of 720 psi/min (12 psi/sec) and a maximum temperature of 250 °C. In 2015, a new batch of Reillex™ HPQ resin was manufactured by Vertellus Industries. A test sample of the resin was sent to SRNL to perform acceptance and qualification thermal stability testing using the ARSST. During these tests, method development was performed to ensure that a representative resin to acid ratios were used while running the tests in the ARSST. Fauske and Associates recommended to either use a full test cell representative of the HB-Line column or a 10 gram sample in the test cell that was representative of the ratios of resin to nitric acid in the actual HB-Line column. An observation was made during method development testing that the 4 grams of resin to 6 grams of 64% acid ratio used in 2001 to determine the rupture disk size did not entirely wet the resin and was not representative of the actual HB-Line column. The results of this study raised questions as to whether the ratio of 4 grams of resin to 6 grams of 64% nitric acid recommended by Fauske and Associates in 2001 was the correct ratio.« less

Properties important to mixing and simulant recommendations for WTP full-scale vessel testing

DOE Office of Scientific and Technical Information (OSTI.GOV)

Poirier, M. R.; Martino, C. J.

2015-12-01

Full Scale Vessel Testing (FSVT) is being planned by Bechtel National, Inc., to demonstrate the ability of the standard high solids vessel design (SHSVD) to meet mixing requirements over the range of fluid properties planned for processing in the Pretreatment Facility (PTF) of the Hanford Waste Treatment and Immobilization Plant (WTP). Testing will use simulated waste rather than actual Hanford waste. Therefore, the use of suitable simulants is critical to achieving the goals of the test program. WTP personnel requested the Savannah River National Laboratory (SRNL) to assist with development of simulants for use in FSVT. Among the tasks assignedmore » to SRNL was to develop a list of waste properties that are important to pulse-jet mixer (PJM) performance in WTP vessels with elevated concentrations of solids.« less

DWPF DECON FRIT: SUMP AND SLURRY SOLIDS ANALYSIS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Crawford, C.; Peeler, D.; Click, D.

The Savannah River National Laboratory (SRNL) has been requested to perform analyses on samples of the Defense Waste Processing Facility (DWPF) decon frit slurry (i.e., supernate samples and sump solid samples). Four 1-L liquid slurry samples were provided to SRNL by Savannah River Remediation (SRR) from the 'front-end' decon activities. Additionally, two 1-L sump solids samples were provided to SRNL for compositional and physical analysis. In this report, the physical and chemical characterization results of the slurry solids and sump solids are reported. Crawford et al. (2010) provide the results of the supernate analysis. The results of the sump solidsmore » are reported on a mass basis given the samples were essentially dry upon receipt. The results of the slurry solids were converted to a volume basis given approximately 2.4 grams of slurry solids were obtained from the {approx}4 liters of liquid slurry sample. Although there were slight differences in the analytical results between the sump solids and slurry solids the following general summary statements can be made. Slight differences in the results are also captured for specific analysis. (1) Physical characterization - (a) SEM/EDS analysis suggested that the samples were enriched in Li and Si (B and Na not detectable using the current EDS system) which is consistent with two of the four principle oxides of Frit 418 (B{sub 2}O{sub 3}, Na{sub 2}O, Li{sub 2}O and SiO{sub 2}). (b) SEM/EDS analysis also identified impurities which were elementally consistent with stainless steel (i.e., Fe, Ni, Cr contamination). (c) XRD results indicated that the sump solids samples were amorphous which is consistent with XRD results expected for a Frit 418 based sample. (d) For the sump solids, SEM/EDS analysis indicated that the particle size of the sump solids were consistent with that of an as received Frit 418 sample from a current DWPF vendor. (e) For the slurry solids, SEM/EDS analysis indicated that the particle size range of the slurry solids was much broader than compared to the sump solids. More specifically, there were significantly more fines in the slurry solids as compared to the sump solids. (f) PSD results indicated that > 99% of both the sump and slurry solids were less than 350 microns. The PSD results also supported SEM/EDS analysis that there were significantly more fines in the slurry solids as compared to the sump solids. (2) Weight Percent Solids - Based on the measured supernate density and mass of insoluble solids (2.388 grams) filtered from the four liters of liquid slurry samples, the weight percent insoluble solids was estimated to be 0.060 wt%. This level of insoluble solids is higher than the ETP WAC limit of 100 mg/L, or 0.01 wt% which suggests a separation technology of some type would be required. (3) Chemical Analysis - (a) Elemental results from ICP-ES analysis indicated that the sump solids and slurry were very consistent with the nominal composition of Frit 418. There were other elements identified by ICP analysis which were either consistent with the presence of stainless steel (as identified by SEM/EDS analysis) or impurities that have been observed in 'as received' Frit 418 from the vendor. (b) IC anion analysis of the sump solids and slurry solids indicated all of the species were less than detection limits. (c) Radionuclide analysis of the sump solids also indicated that most of the analytes were either at or below the detection limits. (d) Organic analysis of the sump solids and slurry solids indicated all of the species were less than detection limits. It should be noted that the results of this study may not be representative of future decon frit solutions or sump/slurry solids samples. Therefore, future DWPF decisions regarding the possible disposal pathways for either the aqueous or solid portions of the Decon Frit system need to factor in the potential differences. More specifically, introduction of a different frit or changes to other DWPF flowsheet unit operations (e.g., different sludge batch or coupling with other process streams) may impact not only the results but also the conclusions regarding acceptability with respect to the ETF WAC limits or other alternative disposal options.« less

Analysis Of 2H-Evaporator Scale Wall [HTF-13-82] And Pot Bottom [HTF-13-77] Samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oji, L. N.

2013-09-11

Savannah River Remediation (SRR) is planning to remove a buildup of sodium aluminosilicate scale from the 2H-evaporator pot by loading and soaking the pot with heated 1.5 M nitric acid solution. Sampling and analysis of the scale material has been performed so that uranium and plutonium isotopic analysis can be input into a Nuclear Criticality Safety Assessment (NCSA) for scale removal by chemical cleaning. Historically, since the operation of the Defense Waste Processing Facility (DWPF), silicon in the DWPF recycle stream combines with aluminum in the typical tank farm supernate to form sodium aluminosilicate scale mineral deposits in the 2H-evaporatormore » pot and gravity drain line. The 2H-evaporator scale samples analyzed by Savannah River National Laboratory (SRNL) came from two different locations within the evaporator pot; the bottom cone sections of the 2H-evaporator pot [Sample HTF-13-77] and the wall 2H-evaporator [sample HTF-13-82]. X-ray diffraction analysis (XRD) confirmed that both the 2H-evaporator pot scale and the wall samples consist of nitrated cancrinite (a crystalline sodium aluminosilicate solid) and clarkeite (a uranium oxyhydroxide mineral). On ''as received'' basis, the bottom pot section scale sample contained an average of 2.59E+00 {+-} 1.40E-01 wt % total uranium with a U-235 enrichment of 6.12E-01 {+-} 1.48E-02 %, while the wall sample contained an average of 4.03E+00 {+-} 9.79E-01 wt % total uranium with a U-235 enrichment of 6.03E-01% {+-} 1.66E-02 wt %. The bottom pot section scale sample analyses results for Pu-238, Pu-239, and Pu-241 are 3.16E-05 {+-} 5.40E-06 wt %, 3.28E-04 {+-} 1.45E-05 wt %, and <8.80E-07 wt %, respectively. The evaporator wall scale samples analysis values for Pu-238, Pu-239, and Pu-241 averages 3.74E-05 {+-} 6.01E-06 wt %, 4.38E-04 {+-} 5.08E-05 wt %, and <1.38E-06 wt %, respectively. The Pu-241 analyses results, as presented, are upper limit values. For these two evaporator scale samples obtained at two different locations within the evaporator pot the major radioactive components (on a mass basis) in the additional radionuclide analyses were Sr-90, Cs-137 Np-237, Pu-239/240 and Th-232. Small quantities of americium and curium were detected in the blanks used for Am/Cm method for these radionuclides. These trace radionuclide amounts are assumed to come from airborne contamination in the shielded cells drying or digestion oven, which has been replaced. Therefore, the Am/Cm results, as presented, may be higher than the true Am/Cm values for these samples. These results are provided so that SRR can calculate the equivalent uranium-235 concentrations for the NCSA. Results confirm that the uranium contained in the scale remains depleted with respect to natural uranium. SRNL did not calculate an equivalent U-235 enrichment, which takes into account other fissionable isotopes U-233, Pu-239 and Pu-241. The applicable method for calculation of equivalent U-235 will be determined in the NCSA. With a few exceptions, a comparison of select radionuclides measurements from this 2013 2H evaporator scale characterization (pot bottom and wall scale samples) with those measurements for the same radionuclides in the 2010 2H evaporator scale analysis shows that the radionuclide analysis for both years are fairly comparable; the analyses results are about the same order of magnitude.« less

SRNL Atmospheric Technologies Group

ScienceCinema

Viner, Brian; Parker, Matthew J.

2018-01-16

The Savannah River National Laboratory, Atmospheric Technologies Group, conducts a best-in class Applied Meteorology Program to ensure the Department of Energy’s Savannah River Site is operated safely and complies with stringent environmental regulations.

WTP Waste Feed Qualification: Glass Fabrication Unit Operation Testing Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stone, M. E.; Newell, J. D.; Johnson, F. C.

The waste feed qualification program is being developed to protect the Hanford Tank Waste Treatment and Immobilization Plant (WTP) design, safety basis, and technical basis by assuring waste acceptance requirements are met for each staged waste feed campaign prior to transfer from the Tank Operations Contractor to the feed receipt vessels inside the Pretreatment Facility. The Waste Feed Qualification Program Plan describes the three components of waste feed qualification: 1. Demonstrate compliance with the waste acceptance criteria 2. Determine waste processability 3. Test unit operations at laboratory scale. The glass fabrication unit operation is the final step in the processmore » demonstration portion of the waste feed qualification process. This unit operation generally consists of combining each of the waste feed streams (high-level waste (HLW) and low-activity waste (LAW)) with Glass Forming Chemicals (GFCs), fabricating glass coupons, performing chemical composition analysis before and after glass fabrication, measuring hydrogen generation rate either before or after glass former addition, measuring rheological properties before and after glass former addition, and visual observation of the resulting glass coupons. Critical aspects of this unit operation are mixing and sampling of the waste and melter feeds to ensure representative samples are obtained as well as ensuring the fabrication process for the glass coupon is adequate. Testing was performed using a range of simulants (LAW and HLW simulants), and these simulants were mixed with high and low bounding amounts of GFCs to evaluate the mixing, sampling, and glass preparation steps in shielded cells using laboratory techniques. The tests were performed with off-the-shelf equipment at the Savannah River National Laboratory (SRNL) that is similar to equipment used in the SRNL work during qualification of waste feed for the Defense Waste Processing Facility (DWPF) and other waste treatment facilities at the Savannah River Site. It is not expected that the exact equipment used during this testing will be used during the waste feed qualification testing for WTP, but functionally similar equipment will be used such that the techniques demonstrated would be applicable. For example, the mixing apparatus could use any suitable mixer capable of being remoted and achieving similar mixing speeds to those tested.« less

Technetium Sorption By Cementitious Materials Under Reducing Conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kaplan, Daniel I.; Estes, Shanna L.; Arai, Yuji

2013-07-18

The objective of this study was to measure Tc sorption to cementitious materials under reducing conditions to simulate Saltstone Disposal Facility conditions. Earlier studies were conducted and the experimental conditions were found not to simulate those of the facility. Through a five month subcontract with Clemson University, sorption of {sup 99}Tc to four cementitious materials was examined within an anaerobic glovebag targeting a 0.1% H{sub 2}(g)/ 99.9% N{sub 2}(g) atmosphere. Early experiments based on Tc sorption and Eh indicated that 0.1% H{sub 2}(g) (a reductant) was necessary to preclude experimental impacts from O{sub 2}(g) diffusion into the glovebag. Preliminary datamore » to date (up to 56 days) indicates that sorption of {sup 99}Tc to cementitious materials increased with increasing slag content for simulated saltstone samples. This is consistent with the conceptual model that redox active sulfide groups within the reducing slag facilitate reduction of Tc(VII) to Tc(IV). These experiments differ from previous experiments where a 2% H{sub 2}(g) atmosphere was maintained (Kaplan et al., 2011 (SRNL-STI-2010-00668)). The impact of the 2% H{sub 2}(g) reducing atmosphere on this data was examined and determined to cause the reduction of Tc in experimental samples without slag. In the present ongoing study, after 56 days, Tc sorption by the 50-year old cement samples (no slag) was undetectable, whereas Tc sorption in the cementitious materials containing slag continues to increase with contact time (measured after 1, 4, 8, 19 and 56 days). Sorption was not consistent with spike concentrations and steady state has not been demonstrated after 56 days. The average conditional K{sub d} value for the Vault 2 cementitious material was 873 mL/g (17% slag), for the TR547 Saltstone (45% slag) the conditional K{sub d} was 168 mL/g, and for TR545 (90% slag) the conditional K{sub d} was 1,619 mL/g. It is anticipated that additional samples will be collected until steady state conditions are established to permit measuring more representative K{sub d} and solubility values under these experimental conditions. The purpose of this revision is to correct K{sub d} values reported in the original document. This document reports results for the first 56 days of a 319 day experiment. After the experiment had finished and all the data were compiled for QA/QC analysis, a mistake in the K{sub d} calculations was found. The K{sub d} values reported in revision 0 of this report were essentially one order of magnitude higher than the actual values. In this revision, the text references to K{sub d} values have been updated along with the data in Figure 2 and Appendix B. Between the time the original document was issued, Janurary 2012, and this document was issued, a final report (Estes et al. 2012; SRNL-STI-2012-00596, Rev. 0) describing all the corrected data for the 319 day experiment was issued. This document does not contain any data that is not already reported in the final report (SRNL-STI-2012-00596, Rev. 0).« less

Inadvertent Intruder Calculatios for F Tank Farm

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koffman, L

2005-09-12

Savannah River National Laboratory (SRNL) has been providing radiological performance assessment analysis for Savannah River Site (SRS) solid waste disposal facilities (McDowell-Boyer 2000). The performance assessment considers numerous potential exposure pathways that could occur in the future. One set of exposure scenarios, known as inadvertent intruder analysis, considers the impact on hypothetical individuals who are assumed to inadvertently intrude onto the waste disposal site. An Automated Intruder Analysis application was developed by SRNL (Koffman 2004) that simplifies the inadvertent intruder analysis into a routine, automated calculation. Based on SRNL's experience, personnel from Planning Integration & Technology of Closure Business Unitmore » asked SRNL to assist with inadvertent intruder calculations for F Tank Farm to support the development of the Tank Closure Waste Determination Document. Meetings were held to discuss the scenarios to be calculated and the assumptions to be used in the calculations. As a result of the meetings, SRNL was asked to perform four scenario calculations. Two of the scenarios are the same as those calculated by the Automated Intruder Analysis application and these can be calculated directly by providing appropriate inputs. The other two scenarios involve use of groundwater by the intruder and the Automated Intruder Analysis application was adapted to perform these calculations. The four calculations to be performed are: (1) A post-drilling scenario in which the drilling penetrates a transfer line. (2) A calculation of internal exposure due to drinking water from a well located near a waste tank. (3) A post-drilling calculation in which waste is introduced by irrigation of the garden with water from a well located near a waste tank. (4) A resident scenario where a house is built above transfer lines. Note that calculations 1 and 4 use sources from the waste inventory in the transfer line (given in Table 1) whereas calculations 2 and 3 use sources from groundwater beneath the waste tank (given in Appendix B). It is important to recognize that there are two different sources in the calculations. In these calculations, assumptions are made for parameter values. Three key parameters are the size of the garden, the amount of vegetables eaten, and the distance of the well from the waste tank. For these three parameters, different values are considered in the calculations to determine the impact of the change in these parameters. Another key parameter is the length of time of institutional control, which determines when an inadvertent intruder could first be exposed. The standard length of time for institutional control is 100 years from the time of closure. In this analysis, waste inventory values are used from year 2005 but tanks will not be closed until year 2020. Thus, the effective length of time of institutional control used in the calculations is 115 years from year 2005, which is taken to be time zero for radiological decay calculations. All calculations are carried out for a period of 10,000 years.« less

Recommended aquifer grid resolution for E-Area PA revision transport simulations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Flach, G.

This memorandum addresses portions of Section 3.5.2 of SRNL (2016) by recommending horizontal and vertical grid resolution for aquifer transport, in preparation for the next E-Area Performance Assessment (WSRC 2008) revision.

Accelerated Leach Testing of GLASS: ALTGLASS Version 3.0

DOE Office of Scientific and Technical Information (OSTI.GOV)

Trivelpiece, Cory L.; Jantzen, Carol M.; Crawford, Charles L.

The Accelerated Leach Testing of GLASS (ALTGLASS) database is a collection of data from short- and long-term product consistency tests (PCT, ASTM C1285 A and B) on high level waste (HLW) as well as low activity waste (LAW) glasses. The database provides both U.S. and international researchers with an archive of experimental data for the purpose of studying, modeling, or validating existing models of nuclear waste glass corrosion. The ALTGLASS database is maintained and updated by researchers at the Savannah River National Laboratory (SRNL). This newest version, ALTGLASS Version 3.0, has been updated with an additional 503 rows of datamore » representing PCT results from corrosion experiments conducted in the United States by the Savannah River National Laboratory, Pacific Northwest National Laboratory, Argonne National Laboratory, and the Vitreous State Laboratory (SRNL, PNNL, ANL, VSL, respectively) as well as the National Nuclear Laboratory (NNL) in the United Kingdom.« less

Alternate Tritium Production Methods Using A Liquid Lithium Target

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wilson, J.

For over 60 years, the Savannah River Site’s primary mission has been the production of tritium. From the beginning, the Savannah River National Laboratory (SRNL) has provided the technical foundation to ensure the successful execution of this critical defense mission. SRNL has developed most of the processes used in the tritium mission and provides the research and development necessary to supply this critical component. This project was executed by first developing reactor models that could be used as a neutron source. In parallel to this development calculations were carried out testing the feasibility of accelerator technologies that could also bemore » used for tritium production. Targets were designed with internal moderating material and optimized target was calculated to be capable of 3000 grams using a 1400 MWt sodium fast reactor, 850 grams using a 400 MWt sodium fast reactor, and 100 grams using a 62 MWt reactor, annually.« less

9978 AND 9975 TYPE B PACKAGING INTERNAL DATA COLLECTION FEASIBILITY TESTING

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fogle, R.

The objective of this report is to document the findings from a series of proof-of-concept tests performed by Savannah River National Laboratory (SRNL) R and D Engineering, for the DOE Packaging Certification Program to determine if a viable radio link could be established from within the stainless steel confines of several drum-style DOE certified Type B radioactive materials packagings. Two in-hand, off-the-shelf radio systems were tested. The first system was a Wi-Fi Librestream Onsight{trademark} camera with a Fortress ES820 Access Point and the second was the On-Ramp Wireless Ultra-Link Processing{trademark} (ULP) radio system. These radio systems were tested within themore » Model 9975 and 9978 Type B packagings at the SRNL. This report documents the test methods and results. A path forward will also be recommended.« less

Evaluation of Wet Chemical ICP-AES Elemental Analysis Methods usingSimulated Hanford Waste Samples-Phase I Interim Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Coleman, Charles J.; Edwards, Thomas B.

2005-04-30

The wet chemistry digestion method development for providing process control elemental analyses of the Hanford Tank Waste Treatment and Immobilization Plant (WTP) Melter Feed Preparation Vessel (MFPV) samples is divided into two phases: Phase I consists of: (1) optimizing digestion methods as a precursor to elemental analyses by ICP-AES techniques; (2) selecting methods with the desired analytical reliability and speed to support the nine-hour or less turnaround time requirement of the WTP; and (3) providing baseline comparison to the laser ablation (LA) sample introduction technique for ICP-AES elemental analyses that is being developed at the Savannah River National Laboratory (SRNL).more » Phase II consists of: (1) Time-and-Motion study of the selected methods from Phase I with actual Hanford waste or waste simulants in shielded cell facilities to ensure that the methods can be performed remotely and maintain the desired characteristics; and (2) digestion of glass samples prepared from actual Hanford Waste tank sludge for providing comparative results to the LA Phase II study. Based on the Phase I testing discussed in this report, a tandem digestion approach consisting of sodium peroxide fusion digestions carried out in nickel crucibles and warm mixed-acid digestions carried out in plastic bottles has been selected for Time-and-Motion study in Phase II. SRNL experience with performing this analytical approach in laboratory hoods indicates that well-trained cell operator teams will be able to perform the tandem digestions in five hours or less. The selected approach will produce two sets of solutions for analysis by ICP-AES techniques. Four hours would then be allocated for performing the ICP-AES analyses and reporting results to meet the nine-hour or less turnaround time requirement. The tandem digestion approach will need to be performed in two separate shielded analytical cells by two separate cell operator teams in order to achieve the nine-hour or less turnaround time. Because of the simplicity of the warm mixed-acid method, a well-trained cell operator team may in time be able to perform both sets of digestions. However, having separate shielded cells for each of the methods is prudent to avoid overcrowding problems that would impede a minimal turnaround time.« less

CBP TOOLBOX VERSION 2.0: CODE INTEGRATION ENHANCEMENTS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, F.; Flach, G.; BROWN, K.

2013-06-01

This report describes enhancements made to code integration aspects of the Cementitious Barriers Project (CBP) Toolbox as a result of development work performed at the Savannah River National Laboratory (SRNL) in collaboration with Vanderbilt University (VU) in the first half of fiscal year 2013. Code integration refers to the interfacing to standalone CBP partner codes, used to analyze the performance of cementitious materials, with the CBP Software Toolbox. The most significant enhancements are: 1) Improved graphical display of model results. 2) Improved error analysis and reporting. 3) Increase in the default maximum model mesh size from 301 to 501 nodes.more » 4) The ability to set the LeachXS/Orchestra simulation times through the GoldSim interface. These code interface enhancements have been included in a new release (Version 2.0) of the CBP Toolbox.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fox, K. M.

The U.S. Department of Energy (DOE), Office of Environmental Management (EM) is sponsoring an international, collaborative project to develop a fundamental model for sulfate solubility in nuclear waste glass. The solubility of sulfate has a significant impact on the achievable waste loading for nuclear waste forms within the DOE complex. These wastes can contain relatively high concentrations of sulfate, which has low solubility in borosilicate glass. This is a significant issue for low-activity waste (LAW) glass and is projected to have a major impact on the Hanford Tank Waste Treatment and Immobilization Plant (WTP). Sulfate solubility has also been amore » limiting factor for recent high level waste (HLW) sludge processed at the Savannah River Site (SRS) Defense Waste Processing Facility (DWPF). The low solubility of sulfate in glass, along with melter and off-gas corrosion constraints, dictate that the waste be blended with lower sulfate concentration waste sources or washed to remove sulfate prior to vitrification. The development of enhanced borosilicate glass compositions with improved sulfate solubility will allow for higher waste loadings and accelerate mission completion.The objective of the current scope being pursued by SHU is to mature the sulfate solubility model to the point where it can be used to guide glass composition development for DWPF and WTP, allowing for enhanced waste loadings and waste throughput at these facilities. A series of targeted glass compositions was selected to resolve data gaps in the model and is identified as Stage III. SHU fabricated these glasses and sent samples to SRNL for chemical composition analysis. SHU will use the resulting data to enhance the sulfate solubility model and resolve any deficiencies. In this report, SRNL provides chemical analyses for the Stage III, simulated HLW glasses fabricated by SHU in support of the sulfate solubility model development.« less

Planning Tool for Strategic Evaluation of Facility Plans - 13570

DOE Office of Scientific and Technical Information (OSTI.GOV)

Magoulas, Virginia; Cercy, Michael; Hall, Irin

2013-07-01

Savannah River National Laboratory (SRNL) has developed a strategic planning tool for the evaluation of the utilization of its unique resources for processing and research and development of nuclear materials. The Planning Tool is a strategic level tool for assessing multiple missions that could be conducted utilizing the SRNL facilities and showcasing the plan. Traditional approaches using standard scheduling tools and laying out a strategy on paper tended to be labor intensive and offered either a limited or cluttered view for visualizing and communicating results. A tool that can assess the process throughput, duration, and utilization of the facility wasmore » needed. SRNL teamed with Newport News Shipbuilding (NNS), a division of Huntington Ingalls Industries, to create the next generation Planning Tool. The goal of this collaboration was to create a simulation based tool that allows for quick evaluation of strategies with respect to new or changing missions, and clearly communicates results to the decision makers. This tool has been built upon a mature modeling and simulation software previously developed by NNS. The Planning Tool provides a forum for capturing dependencies, constraints, activity flows, and variable factors. It is also a platform for quickly evaluating multiple mission scenarios, dynamically adding/updating scenarios, generating multiple views for evaluating/communicating results, and understanding where there are areas of risks and opportunities with respect to capacity. The Planning Tool that has been developed is useful in that it presents a clear visual plan for the missions at the Savannah River Site (SRS). It not only assists in communicating the plans to SRS corporate management, but also allows the area stakeholders a visual look at the future plans for SRS. The design of this tool makes it easily deployable to other facility and mission planning endeavors. (authors)« less

Climate Change Resilience Planning at the Department of Energy's Savannah River Site

NASA Astrophysics Data System (ADS)

Werth, D. W.; Johnson, A.

2015-12-01

The Savannah River National Laboratory (SRNL) is developing a site sustainability plan for the Department of Energy's Savannah River Site (SRS) in South Carolina in accordance with Executive Order 13693, which charges each DOE agency with "identifying and addressing projected impacts of climate change" and "calculating the potential cost and risk to mission associated with agency operations". The plan will comprise i) projections of climate change, ii) surveys of site managers to estimate the effects of climate change on site operations, and iii) a determination of adaptive actions. Climate change projections for SRS are obtained from multiple sources, including an online repository of downscaled global climate model (GCM) simulations of future climate and downscaled GCM simulations produced at SRNL. Taken together, we have projected data for temperature, precipitation, humidity, and wind - all variables with a strong influence on site operations. SRNL is working to engage site facility managers and facilitate a "bottom up" approach to climate change resilience planning, where the needs and priorities of stakeholders are addressed throughout the process. We make use of the Vulnerability Assessment Scoring Tool, an Excel-based program designed to accept as input various climate scenarios ('exposure'), the susceptibility of assets to climate change ('sensitivity'), and the ability of these assets to cope with climate change ('adaptive capacity'). These are combined to produce a series of scores that highlight vulnerabilities. Working with site managers, we have selected the most important assets, estimated their expected response to climate change, and prepared a report highlighting the most endangered facilities. Primary risks include increased energy consumption, decreased water availability, increased forest fire danger, natural resource degradation, and compromised outdoor worker safety in a warmer and more humid climate. Results of this study will aid in driving future management decisions and promoting sustainable practices at SRS.

ANALYSES OF HTF-48-12-20/24 (FEBRUARY, 2012) AND ARCHIVED HTF-E-05-021 TANK 48H SLURRY SAMPLES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nash, C.; Peters, T.

Personnel characterized a Savannah River National Laboratory (SRNL) archived sample of Tank 48H slurry (HTF-E-05-021) in addition to the composite of samples HTF-48-12-20 and HTF-48-12-24, which were both retrieved in February 2012. The combined February 2012 sample is referred to as HTF-48-12-20/24 in this report. The results from these analyses are compared with Tank 48H samples analyzed in 2003, 2004, and 2005. This work supports the effort to demonstrate copper-catalyzed peroxide oxidation (CCPO) of organic content in this material. The principal findings with respect to the chemical and physical characteristics of the most recent sample are: (1) The measured potassiummore » tetraphenylborate (KTPB) solid concentration is 1.76 wt %; (2) Titanium was in line with 2004 and 2005 slurry measurements at 897 mg/L, it represents 0.1535 {+-} 0.0012 wt % monosodium titanate (MST); (3) The measured insoluble solids content was 1.467 wt %; (4) The free hydroxide concentration in the Tank 48H filtrate sample (1.02 {+-} 0.02 M) is close to the Tank 48H limit (1.0 M); (5) Carbonate reported by total inorganic carbon (TIC, 1.39 {+-} 0.03 M) is more than double the concentrations measured in past (2003-2005) samples; (6) The soluble potassium content (measured at 286 {+-} 23 mg/L) in the filtrate is in line with all past measurements; and (7) The measured {sup 137}Cs concentration is 7.81E + 08 {+-} 3.9E + 07 dpm/mL of slurry (1.33 {+-} 5% Ci/gallon or 3.18E + 05 {+-} 5% curies of {sup 137}Cs in the tank) in the slurry which is in agreement with the 2005 report of 3.14E + 05 {+-} 1.5% curies of {sup 137}Cs in the tank. The filtrate {sup 137}Cs concentration is 2.57E + 07 {+-} 2.6E + 05 dpm/mL. This result is consistent with previous results. Significant analytical data are summarized in Table 1.« less

3.8 Proposed approach to uncertainty quantification and sensitivity analysis in the next PA

DOE Office of Scientific and Technical Information (OSTI.GOV)

Flach, Greg; Wohlwend, Jen

2017-10-02

This memorandum builds upon Section 3.8 of SRNL (2016) and Flach (2017) by defining key error analysis, uncertainty quantification, and sensitivity analysis concepts and terms, in preparation for the next E-Area Performance Assessment (WSRC 2008) revision.

Glycolic acid physical properties and impurities assessment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lambert, D. P.; Pickenheim, B. R.; Hay, M. S.

This document has been revised to add analytical data for fresh, 1 year old, and 4 year old glycolic acid as recommended in Revision 2 of this document. This was needed to understand the concentration of formaldehyde and methoxyacetic acid, impurities present in the glycolic acid used in Savannah River National Laboratory (SRNL) experiments. Based on this information, the concentration of these impurities did not change during storage. These impurities were in the glycolic acid used in the testing included in this report and in subsequent testing using DuPont (now called Chemours) supplied Technical Grade 70 wt% glycolic acid. However,more » these impurities were not reported in the first two versions of this report. The Defense Waste Processing Facility (DWPF) is planning to implement a nitric-glycolic acid flowsheets to increase attainment to meet closure commitment dates during Sludge Batch 9. In fiscal year 2009, SRNL was requested to determine the physical properties of formic and glycolic acid blends.« less

Natural Gas Storage Research at Savannah River National Laboratory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Anton, Don; Sulic, Martin; Tamburello, David A.

As an alternative to imported oil, scientists at the Department of Energy’s Savannah River National Laboratory are looking at abundant, domestically sourced natural gas, as an alternative transportation fuel. SRNL is investigating light, inexpensive, adsorbed natural gas storage systems that may fuel the next generation of automobiles.

Natural Gas Storage Research at Savannah River National Laboratory

ScienceCinema

Anton, Don; Sulic, Martin; Tamburello, David A.

2018-01-16

As an alternative to imported oil, scientists at the Department of Energy’s Savannah River National Laboratory are looking at abundant, domestically sourced natural gas, as an alternative transportation fuel. SRNL is investigating light, inexpensive, adsorbed natural gas storage systems that may fuel the next generation of automobiles.

Waste Isolation Pilot Plant Technical Assessment Team Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

None, None

This report provides the results of the Waste Isolation Pilot Plant (WIPP) technical assessment led by the Savannah River National Laboratory and conducted by a team of experts in pertinent disciplines from SRNL and Lawrence Livermore National Laboratory (LLNL), Oak Ridge National Laboratory (ORNL), Pacific Northwest National Laboratory (PNNL), and Sandia National Laboratories (SNL).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smartt, Heidi A.; Romero, Juan A.; Custer, Joyce Olsen

Containment/Surveillance (C/S) measures are critical to any verification regime in order to maintain Continuity of Knowledge (CoK). The Ceramic Seal project is research into the next generation technologies to advance C/S, in particular improving security and efficiency. The Ceramic Seal is a small form factor loop seal with improved tamper-indication including a frangible seal body, tamper planes, external coatings, and electronic monitoring of the seal body integrity. It improves efficiency through a self-securing wire and in-situ verification with a handheld reader. Sandia National Laboratories (SNL) and Savannah River National Laboratory (SRNL), under sponsorship from the U.S. National Nuclear Security Administrationmore » (NNSA) Office of Defense Nuclear Nonproliferation Research and Development (DNN R&D), have previously designed and have now fabricated and tested Ceramic Seals. Tests have occurred at both SNL and SRNL, with different types of tests occurring at each facility. This interim report will describe the Ceramic Seal prototype, the design and development of a handheld standalone reader and an interface to a data acquisition system, fabrication of the seals, and results of initial testing.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Butcher, T.; Hamm, L.; Flach, G.

Revision 0 of this UDQE addressed the proposal to place Engineered Trench #3 (ET#3) in the footprint designated for Slit Trench #12 (ST#12) and operate using ST#12 disposal limits. Similarly, Revision 1 evaluates whether ET#4 can be located in and operated to Slit Trench #13 (ST#13) disposal limits. Both evaluations conclude that the proposed operations result in an acceptably small risk of exceeding a SOF of 1.0 and approve these actions from a performance assessment (PA) perspective. Because ET#3 will be placed in the location previously designated for ST#12, Solid Waste Management (SWM) requested that the Savannah River National Laboratorymore » (SRNL) determine if the ST#12 limits could be employed as surrogate disposal limits for ET#3 operations. SRNL documented in this Unreviewed Disposal Question Evaluation (UDQE) that the use of ST#12 limits as surrogates for the new ET#3 disposal unit will provide reasonable assurance that Department of Energy (DOE) 435.1 performance objectives and measures (USDOE, 1999) will be protected. Therefore, new ET#3 inventory limits as determined by a Special Analysis (SA) are not required.« less

GrayQb TM Single-Faced Version 2 (SF2) Hanford Plutonium Reclamation Facility (PRF) deployment report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Plummer, J. R.; Immel, D. M.; Serrato, M. G.

2015-11-18

The Savannah River National Laboratory (SRNL) in partnership with CH2M Plateau Remediation Company (CHPRC) deployed the GrayQb TM SF2 radiation imaging device at the Hanford Plutonium Reclamation Facility (PRF) to assist in the radiological characterization of the canyon. The deployment goal was to locate radiological contamination hot spots in the PRF canyon, where pencil tanks were removed and decontamination/debris removal operations are on-going, to support the CHPRC facility decontamination and decommissioning (D&D) effort. The PRF canyon D&D effort supports completion of the CHPRC Plutonium Finishing Plant Decommissioning Project. The GrayQb TM SF2 (Single Faced Version 2) is a non-destructive examinationmore » device developed by SRNL to generate radiation contour maps showing source locations and relative radiological levels present in the area under examination. The Hanford PRF GrayQbTM Deployment was sponsored by CH2M Plateau Remediation Company (CHPRC) through the DOE Richland Operations Office, Inter-Entity Work Order (IEWO), DOE-RL IEWO- M0SR900210.« less

BLENDING ANALYSIS FOR RADIOACTIVE SALT WASTE PROCESSING FACILITY

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, S.

2012-05-10

Savannah River National Laboratory (SRNL) evaluated methods to mix and blend the contents of the blend tanks to ensure the contents are properly blended before they are transferred from the blend tank such as Tank 21 and Tank 24 to the Salt Waste Processing Facility (SWPF) feed tank. The tank contents consist of three forms: dissolved salt solution, other waste salt solutions, and sludge containing settled solids. This paper focuses on developing the computational model and estimating the operation time of submersible slurry pump when the tank contents are adequately blended prior to their transfer to the SWPF facility. Amore » three-dimensional computational fluid dynamics approach was taken by using the full scale configuration of SRS Type-IV tank, Tank 21H. Major solid obstructions such as the tank wall boundary, the transfer pump column, and three slurry pump housings including one active and two inactive pumps were included in the mixing performance model. Basic flow pattern results predicted by the computational model were benchmarked against the SRNL test results and literature data. Tank 21 is a waste tank that is used to prepare batches of salt feed for SWPF. The salt feed must be a homogeneous solution satisfying the acceptance criterion of the solids entrainment during transfer operation. The work scope described here consists of two modeling areas. They are the steady state flow pattern calculations before the addition of acid solution for tank blending operation and the transient mixing analysis during miscible liquid blending operation. The transient blending calculations were performed by using the 95% homogeneity criterion for the entire liquid domain of the tank. The initial conditions for the entire modeling domain were based on the steady-state flow pattern results with zero second phase concentration. The performance model was also benchmarked against the SRNL test results and literature data.« less

Plutonium Isotopes in the Terrestrial Environment at the Savannah River Site, USA. A Long-Term Study

DOE PAGES

Armstrong, Christopher R.; Nuessle, Patterson R.; Brant, Heather A.; ...

2015-01-16

This work presents the findings of a long term plutonium study at Savannah River Site (SRS) conducted between 2003 and 2013. Terrestrial environmental samples were obtained at Savannah River National Laboratory (SRNL) in A-area. Plutonium content and isotopic abundances were measured over this time period by alpha spectrometry and three stage thermal ionization mass spectrometry (3STIMS). Here we detail the complete sample collection, radiochemical separation, and measurement procedure specifically targeted to trace plutonium in bulk environmental samples. Total plutonium activities were determined to be not significantly above atmospheric global fallout. However, the 238Pu/ 239+240Pu activity ratios attributed to SRS aremore » above atmospheric global fallout ranges. The 240Pu/ 239Pu atom ratios are reasonably consistent from year to year and are lower than fallout, while the 242Pu/ 239Pu atom ratios are higher than fallout values. Overall, the plutonium signatures obtained in this study reflect a mixture of weapons-grade, higher burn-up, and fallout material. This study provides a blue print for long term low level monitoring of plutonium in the environment.« less

HYBRID SULFUR PROCESS REFERENCE DESIGN AND COST ANALYSIS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gorensek, M.; Summers, W.; Boltrunis, C.

2009-05-12

This report documents a detailed study to determine the expected efficiency and product costs for producing hydrogen via water-splitting using energy from an advanced nuclear reactor. It was determined that the overall efficiency from nuclear heat to hydrogen is high, and the cost of hydrogen is competitive under a high energy cost scenario. It would require over 40% more nuclear energy to generate an equivalent amount of hydrogen using conventional water-cooled nuclear reactors combined with water electrolysis compared to the proposed plant design described herein. There is a great deal of interest worldwide in reducing dependence on fossil fuels, whilemore » also minimizing the impact of the energy sector on global climate change. One potential opportunity to contribute to this effort is to replace the use of fossil fuels for hydrogen production by the use of water-splitting powered by nuclear energy. Hydrogen production is required for fertilizer (e.g. ammonia) production, oil refining, synfuels production, and other important industrial applications. It is typically produced by reacting natural gas, naphtha or coal with steam, which consumes significant amounts of energy and produces carbon dioxide as a byproduct. In the future, hydrogen could also be used as a transportation fuel, replacing petroleum. New processes are being developed that would permit hydrogen to be produced from water using only heat or a combination of heat and electricity produced by advanced, high temperature nuclear reactors. The U.S. Department of Energy (DOE) is developing these processes under a program known as the Nuclear Hydrogen Initiative (NHI). The Republic of South Africa (RSA) also is interested in developing advanced high temperature nuclear reactors and related chemical processes that could produce hydrogen fuel via water-splitting. This report focuses on the analysis of a nuclear hydrogen production system that combines the Pebble Bed Modular Reactor (PBMR), under development by PBMR (Pty.) Ltd. in the RSA, with the Hybrid Sulfur (HyS) Process, under development by the Savannah River National Laboratory (SRNL) in the US as part of the NHI. This work was performed by SRNL, Westinghouse Electric Company, Shaw, PBMR (Pty) Ltd., and Technology Insights under a Technical Consulting Agreement (TCA). Westinghouse Electric, serving as the lead for the PBMR process heat application team, established a cost-shared TCA with SRNL to prepare an updated HyS thermochemical water-splitting process flowsheet, a nuclear hydrogen plant preconceptual design and a cost estimate, including the cost of hydrogen production. SRNL was funded by DOE under the NHI program, and the Westinghouse team was self-funded. The results of this work are presented in this Final Report. Appendices have been attached to provide a detailed source of information in order to document the work under the TCA contract.« less

Numerical convergence improvements for porflow unsaturated flow simulations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Flach, Greg

2017-08-14

Section 3.6 of SRNL (2016) discusses various PORFLOW code improvements to increase modeling efficiency, in preparation for the next E-Area Performance Assessment (WSRC 2008) revision. This memorandum documents interaction with Analytic & Computational Research, Inc. (http://www.acricfd.com/default.htm) to improve numerical convergence efficiency using PORFLOW version 6.42 for unsaturated flow simulations.

Preliminary Tests For Development Of A Non-Pertechnetate Analysis Method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Diprete, D.; McCabe, D.

2016-09-28

The objective of this task was to develop a non-pertechnetate analysis method that 222-S lab could easily implement. The initial scope involved working with 222-S laboratory personnel to adapt the existing Tc analytical method to fractionate the non-pertechnetate and pertechnetate. SRNL then developed and tested a method using commercial sorbents containing Aliquat ® 336 to extract the pertechnetate (thereby separating it from non-pertechnetate), followed by oxidation, extraction, and stripping steps, and finally analysis by beta counting and Mass Spectroscopy. Several additional items were partially investigated, including impacts of a 137Cs removal step. The method was initially tested on SRS tankmore » waste samples to determine its viability. Although SRS tank waste does not contain non-pertechnetate, testing with it was useful to investigate the compatibility, separation efficiency, interference removal efficacy, and method sensitivity.« less

Extraction, scrub, and strip test results for the solvent transfer to salt waste processing facility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T.

The Savannah River National Laboratory (SRNL) prepared approximately 240 gallons of Caustic-Side Solvent Extraction (CSSX) solvent for use at the Salt Waste Processing Facility (SWPF). An Extraction, Scrub, and Strip (ESS) test was performed on a sample of the prepared solvent using a salt solution prepared by Parsons to determine cesium distribution ratios (D(Cs)), and cesium concentration in the strip effluent (SE) and decontaminated salt solution (DSS) streams. This data will be used by Parsons to help qualify the solvent for use at the SWPF. The ESS test showed acceptable performance of the solvent for extraction, scrub, and strip operations.more » The extraction D(Cs) measured 15.5, exceeding the required value of 8. This value is consistent with results from previous ESS tests using similar solvent formulations. Similarly, scrub and strip cesium distribution ratios fell within acceptable ranges.« less

Annual Report, Fall 2016: Identifying Cost Effective Tank Waste Characterization Approaches

DOE Office of Scientific and Technical Information (OSTI.GOV)

Reboul, S. H.; DiPrete, D. P.

2016-12-12

This report documents the activities that were performed during the second year of a project undertaken to improve the cost effectiveness and timeliness of SRNL’s tank closure characterization practices. The activities performed during the first year of the project were previously reported in SRNL-STI-2015-00144. The scope of the second year activities was divided into the following three primary tasks: 1) develop a technical basis and strategy for improving the cost effectiveness and schedule of SRNL’s tank closure characterization program; 2) initiate the design and assembly of a new waste removal system for improving the throughput and reducing the personnel dosemore » associated with extraction chromatography radiochemical separations; and 3) develop and perform feasibility testing of three alternative radiochemical separation protocols holding promise for improving high resource demand/time consuming tank closure sample analysis methods.« less

Innovative In-Situ Remediation of Contaminated Sediments for Simultaneous Control of Contamination and Erosion. Part 1

DTIC Science & Technology

2010-12-27

Erosion Rates and Critical Shear Stress ......................... 45 Erosion Rate Ratio Analysis...inductively coupled plasma – mass spectrometry Kd – partition coefficient Meq – milliequivalents MNR – monitored natural recovery SRNL-STI-2010...186 Figure 82. Critical Shear Stress Comparison among Biopolymer Materials at 2, 10, and 175 Days. Each value is an average of

A Permeable Active Amendment Concrete (PAAC) for Contaminant Remediation and Erosion Control

DTIC Science & Technology

2012-06-01

124: 131 -143. SRNL-STI-2012-00356 70 Tessier, A., Campbell, P.G.C., and Bisson, M. 1979. Sequential extraction procedure for the speciation of...Bulk Density, Dry, (AI( C-D)]* p, pcf 134.85 Bulk Dens ity after Immersion, [BI(C-D)]* p, pcf 146.65 Bulk Density after Immersion & Boiling1 jCI (C

Preliminary Mark-18A (Mk-18A) Target Material Recovery Program Product Acceptance Criteria

DOE Office of Scientific and Technical Information (OSTI.GOV)

Robinson, Sharon M.; Patton, Bradley D.

2016-09-01

The Mk-18A Target Material Recovery Program (MTMRP) was established in 2015 to preserve the unique materials, e.g. 244Pu, in 65 previously irradiated Mk-18A targets for future use. This program utilizes existing capabilities at SRS and Savannah River National Laboratory (SRNL) to process targets, recover materials from them, and to package the recovered materials for shipping to ORNL. It also utilizes existing capabilities at ORNL to receive and store the recovered materials, and to provide any additional processing of the recovered materials or residuals required to prepare them for future beneficial use. The MTMRP is presently preparing for the processing ofmore » these valuable targets which is expected to begin in ~2019. As part of the preparations for operations, this report documents the preliminary acceptance criteria for the plutonium and heavy curium materials to be recovered from the Mk-18A targets at SRNL for transport and storage at ORNL. These acceptance criteria were developed based on preliminary concepts developed for processing, transporting, and storing the recovered Mk-18A materials. They will need to be refined as these concepts are developed in more detail.« less

Gamma-ray imaging assay of cells 3-5 of the east cell line in the 235-F plutonium fuel form facility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brand, A. D.; Aucott, T. J.; Diprete, D. P.

In August and September, 2016, scientists from the Savannah River National Laboratory (SRNL) took a series of gamma-ray imaging measurements through the cell windows in front of Cells 3-5 on the east line of the Plutonium Fuel Form (PuFF) Facility using an electrically cooled, high-purity germanium detector. A Germanium Gamma Ray Imager (GeGI) was utilized since it allowed for the location from which the radiation was being emitted to be identified by incoming gamma-ray energy. This measurement technique provided a tool which allowed for the relative concentration of Pu-238 to be mapped throughout each cell. The mapping and new assaymore » data were then used to update the model used in an assay discussed in a 2014 report (SRNL-STI-2014-00629) and to calculate a more accurate value for the holdup in each of the cells [1]. Note that the mapping and new assay data did not replace the previous assay data in the model. Rather, the mapping and new assay data provided additional details on source distribution, which supplemented the previous assay data.« less

RadBall Technology Testing and MCNP Modeling of the Tungsten Collimator.

PubMed

Farfán, Eduardo B; Foley, Trevor Q; Coleman, J Rusty; Jannik, G Timothy; Holmes, Christopher J; Oldham, Mark; Adamovics, John; Stanley, Steven J

2010-01-01

The United Kingdom's National Nuclear Laboratory (NNL) has developed a remote, non-electrical, radiation-mapping device known as RadBall(™), which can locate and quantify radioactive hazards within contaminated areas of the nuclear industry. RadBall(™) consists of a colander-like outer shell that houses a radiation-sensitive polymer sphere. The outer shell works to collimate radiation sources and those areas of the polymer sphere that are exposed react, becoming increasingly more opaque, in proportion to the absorbed dose. The polymer sphere is imaged in an optical-CT scanner, which produces a high resolution 3D map of optical attenuation coefficients. Subsequent analysis of the optical attenuation matrix provides information on the spatial distribution of sources in a given area forming a 3D characterization of the area of interest. RadBall(™) has no power requirements and can be positioned in tight or hard-to reach locations. The RadBall(™) technology has been deployed in a number of technology trials in nuclear waste reprocessing plants at Sellafield in the United Kingdom and facilities of the Savannah River National Laboratory (SRNL). This study focuses on the RadBall(™) testing and modeling accomplished at SRNL.

RadBall™ Technology Testing and MCNP Modeling of the Tungsten Collimator

PubMed Central

Farfán, Eduardo B.; Foley, Trevor Q.; Coleman, J. Rusty; Jannik, G. Timothy; Holmes, Christopher J.; Oldham, Mark; Adamovics, John; Stanley, Steven J.

2010-01-01

The United Kingdom’s National Nuclear Laboratory (NNL) has developed a remote, non-electrical, radiation-mapping device known as RadBall™, which can locate and quantify radioactive hazards within contaminated areas of the nuclear industry. RadBall™ consists of a colander-like outer shell that houses a radiation-sensitive polymer sphere. The outer shell works to collimate radiation sources and those areas of the polymer sphere that are exposed react, becoming increasingly more opaque, in proportion to the absorbed dose. The polymer sphere is imaged in an optical-CT scanner, which produces a high resolution 3D map of optical attenuation coefficients. Subsequent analysis of the optical attenuation matrix provides information on the spatial distribution of sources in a given area forming a 3D characterization of the area of interest. RadBall™ has no power requirements and can be positioned in tight or hard-to reach locations. The RadBall™ technology has been deployed in a number of technology trials in nuclear waste reprocessing plants at Sellafield in the United Kingdom and facilities of the Savannah River National Laboratory (SRNL). This study focuses on the RadBall™ testing and modeling accomplished at SRNL. PMID:21617740

Dissolution of Material and Test reactor Fuel in an H-Canyon Dissolver

DOE Office of Scientific and Technical Information (OSTI.GOV)

Daniel, W. E.; Rudisill, T. S.; O'Rourke, P. E.

2017-01-26

In an amended record of decision for the management of spent nuclear fuel (SNF) at the Savannah River Site, the US Department of Energy has authorized the dissolution and recovery of U from 1000 bundles of Al-clad SNF. The SNF is fuel from domestic and foreign research reactors and is typically referred to as Material Test Reactor (MTR) fuel. Bundles of MTR fuel containing assemblies fabricated from U-Al alloys (or other U compounds) are currently dissolved using a Hg-catalyzed HNO3 flowsheet. Since the development of the existing flowsheet, improved experimental methods have been developed to more accurately characterize the offgasmore » composition and generation rate during laboratory dissolutions. Recently, these new techniques were successfully used to develop a flowsheet for the dissolution of High Flux Isotope Reactor (HFIR) fuel. Using the data from the HFIR dissolution flowsheet development and necessary laboratory experiments, the Savannah River National Laboratory (SRNL) was requested to define flowsheet conditions for the dissolution of MTR fuels. With improved offgas characterization techniques, SRNL will be able define the number of bundles of fuel which can be charged to an H-Canyon dissolver with much less conservatism.« less

Discoloration of the wetted surface in the 6.1D dissolver

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rudisill, T.; Mickalonis, J.; Crapse, K.

During a camera inspection of a failed coil in the 6.1D dissolver, an orange discoloration was observed on a portion of the dissolver wall and coils. At the request of H-Canyon Engineering, the inspection video of the dissolver was reviewed by SRNL to assess if the observed condition (a non-uniform, orange-colored substance on internal surfaces) was a result of corrosion. Although the dissolver vessel and coil corrode during dissolution operations, the high acid conditions are not consistent with the formation of ferrous oxides (i.e., orange/rust-colored corrosion products). In a subsequent investigation, SRNL performed dissolution experiments to determine if residues frommore » the nylon bags used for Pu containment could have generated the orange discoloration following dissolution. When small pieces of a nylon bag were placed in boiling 8 M nitric acid solutions containing other components representative of the H-Canyon process, complete dissolution occurred almost immediately. No residues were obtained even when a nylon mass to volume ratio greater than 100 times the 6.1D dissolver value was used. Degradation products from the dissolution of nylon bags are not responsible for the discoloration observed in the dissolver.« less

Engineering scale demonstration of a prospective Cast Stone process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cozzi, A.; Fowley, M.; Hansen, E.

2014-09-30

This report documents an engineering-scale demonstration with non-radioactive simulants that was performed at SRNL using the Scaled Continuous Processing Facility (SCPF) to fill an 8.5 ft container with simulated Cast Stone grout. The Cast Stone formulation was chosen from the previous screening tests. Legacy salt solution from previous Hanford salt waste testing was adjusted to correspond to the average composition generated from the Hanford Tank Waste Operation Simulator (HTWOS). The dry blend materials, ordinary portland cement (OPC), Class F fly ash, and ground granulated blast furnace slag (GGBFS or BFS), were obtained from Lafarge North America in Pasco, WA. Overmore » three days, the SCPF was used to fill a 1600 gallon container, staged outside the facility, with simulated Cast Stone grout. The container, staged outside the building approximately 60 ft from the SCPF, was instrumented with x-, y-, and z-axis thermocouples to monitor curing temperature. The container was also fitted with two formed core sampling vials. For the operation, the targeted grout production rate was 1.5 gpm. This required a salt solution flow rate of approximately 1 gpm and a premix feed rate of approximately 580 lb/h. During the final day of operation, the dry feed rate was increased to evaluate the ability of the system to handle increased throughput. Although non-steady state operational periods created free surface liquids, no bleed water was observed either before or after operations. The final surface slope at a fill height of 39.5 inches was 1-1.5 inches across the 8.5 foot diameter container, highest at the final fill point and lowest diametrically opposed to the fill point. During processing, grout was collected in cylindrical containers from both the mixer discharge and the discharge into the container. These samples were stored in a humid environment either in a closed box proximal to the container or inside the laboratory. Additional samples collected at these sampling points were analyzed for rheological properties and density. Both the rheological properties (plastic viscosity and yield strength) and density were consistent with previous and later SCPF runs.« less

NUCLEAR INCIDENT CAPABILITIES, KNOWLEDGE & ENABLER LEVERAGING

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kinney, J.; Newman, J.; Goodwyn, A.

2011-04-18

The detonation of a 10 Kiloton Improvised Nuclear Device (IND) is a serious scenario that the United States must be prepared to address. The likelihood of a single nuclear bomb exploding in a single city is greater today than at the height of the Cold War. Layered defenses against domestic nuclear terrorism indicate that our government continues to view the threat as credible. The risk of such an event is further evidenced by terrorists desire to acquire nuclear weapons. The act of nuclear terrorism, particularly an act directed against a large population center in the United States, will overwhelm themore » capabilities of many local and state governments to respond, and will seriously challenge existing federal response capabilities. A 10 Kiloton IND detonation would cause total infrastructure damage in a 3-mile radius and levels of radiation spanning out 3,000 square miles. In a densely populated urban area, the anticipated casualties would be in excess of several hundred thousand. Although there would be enormous loss of life, housing and infrastructure, an IND detonation is a recoverable event. We can reduce the risk of these high-consequence, nontraditional threats by enhancing our nuclear detection architecture and establishing well planned and rehearsed plans for coordinated response. It is also important for us to identify new and improved ways to foster collaboration regarding the response to the IND threat to ensure the demand and density of expertise required for such an event is postured and prepared to mobilize, integrate, and support a myriad of anticipated challenges. We must be prepared to manage the consequences of such an event in a deliberate manner and get beyond notions of total devastation by adopting planning assumptions around survivability and resiliency. Planning for such a scenario needs to be decisive in determining a response based on competencies and desired outcomes. It is time to synthesize known threats and plausible consequences into action. Much work needs to be accomplished to enhance nuclear preparedness and to substantially bolster and clarify the capacity to deploy competent resources. Until detailed plans are scripted, and personnel and other resources are postured, and exercised, IND specific planning remains an urgent need requiring attention and action. Although strategic guidance, policies, concepts of operations, roles, responsibilities, and plans governing the response and consequence management for the IND scenario exist, an ongoing integration challenge prevails regarding how best to get capable and competent surge capacity personnel (disaster reservists) and other resources engaged and readied in an up-front manner with pre-scripted assignments to augment the magnitude of anticipated demands of expertise. With the above in mind, Savannah River National Laboratory (SRNL) puts science to work to create and deploy practical, high-value, cost-effective nuclear solutions. As the Department of Energy's (DOE) applied research and development laboratory, SRNL supports Savannah River Site (SRS) operations, DOE, national initiatives, and other federal agencies, across the country and around the world. SRNL's parent at SRS also employs more than 8,000 personnel. The team is a great asset that seeks to continue their service in the interest of national security and stands ready to accomplish new missions. Overall, an integral part of the vision for SRNL's National and Homeland Security Directorate is the establishment of a National Security Center at SRNL, and development of state of the science capabilities (technologies and trained technical personnel) for responding to emergency events on local, regional, or national scales. This entails leveraging and posturing the skills, knowledge and experience base of SRS personnel to deliver an integrated capability to support local, state, and federal authorities through the development of pre-scripted requests for assistance, agreements, and plans. It also includes developing plans, training, exercises, recruitment strategies, and processes to establish a 1,000 plus person nuclear disaster workforce capable of providing surge capacity support that can be deployed in part or in all.« less

SALTSTONE VAULT CLASSIFICATION SAMPLES MODULAR CAUSTIC SIDE SOLVENT EXTRACTION UNIT/ACTINIDE REMOVAL PROCESS WASTE STREAM APRIL 2011

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eibling, R.

Savannah River National Laboratory (SRNL) was asked to prepare saltstone from samples of Tank 50H obtained by SRNL on April 5, 2011 (Tank 50H sampling occurred on April 4, 2011) during 2QCY11 to determine the non-hazardous nature of the grout and for additional vault classification analyses. The samples were cured and shipped to Babcock & Wilcox Technical Services Group-Radioisotope and Analytical Chemistry Laboratory (B&W TSG-RACL) to perform the Toxic Characteristic Leaching Procedure (TCLP) and subsequent extract analysis on saltstone samples for the analytes required for the quarterly analysis saltstone sample. In addition to the eight toxic metals - arsenic, barium,more » cadmium, chromium, mercury, lead, selenium and silver - analytes included the underlying hazardous constituents (UHC) antimony, beryllium, nickel, and thallium which could not be eliminated from analysis by process knowledge. Additional inorganic species determined by B&W TSG-RACL include aluminum, boron, chloride, cobalt, copper, fluoride, iron, lithium, manganese, molybdenum, nitrate/nitrite as Nitrogen, strontium, sulfate, uranium, and zinc and the following radionuclides: gross alpha, gross beta/gamma, 3H, 60Co, 90Sr, 99Tc, 106Ru, 106Rh, 125Sb, 137Cs, 137mBa, 154Eu, 238Pu, 239/240Pu, 241Pu, 241Am, 242Cm, and 243/244Cm. B&W TSG-RACL provided subsamples to GEL Laboratories, LLC for analysis for the VOCs benzene, toluene, and 1-butanol. GEL also determines phenol (total) and the following radionuclides: 147Pm, 226Ra and 228Ra. Preparation of the 2QCY11 saltstone samples for the quarterly analysis and for vault classification purposes and the subsequent TCLP analyses of these samples showed that: (1) The saltstone waste form disposed of in the Saltstone Disposal Facility in 2QCY11 was not characteristically hazardous for toxicity. (2) The concentrations of the eight RCRA metals and UHCs identified as possible in the saltstone waste form were present at levels below the UTS. (3) Most of the inorganic species measured in the leachate do not exceed the MCL, SMCL or TW limits. (4) The inorganic waste species that exceeded the MCL by more than a factor of 10 were nitrate, nitrite and the sum of nitrate and nitrite. (5) Analyses met all quality assurance specifications of US EPA SW-846. (6) The organic species (benzene, toluene, 1-butanol, phenol) were either not detected or were less than reportable for the vault classification samples. (7) The gross alpha and radium isotopes could not be determined to the MCL because of the elevated background which raised the detection limits. (8) Most of the beta/gamma activity was from 137Cs and its daughter 137mBa. (9) The concentration of 137Cs and 90Sr were present in the leachate at concentrations 1/40th and 1/8th respectively than in the 2003 vault classification samples. The saltstone waste form placed in the Saltstone Disposal Facility in 2QCY11 met the SCHWMR R.61-79.261.24(b) RCRA metals requirements for a nonhazardous waste form. The TCLP leachate concentrations for nitrate, nitrite and the sum of nitrate and nitrite were greater than 10x the MCLs in SCDHEC Regulations R.61-107.19, Part I A, which confirms the Saltstone Disposal Facility classification as a Class 3 Landfill. The saltstone waste form placed in the Saltstone Disposal Facility in 2QCY11 met the R.61-79.268.48(a) non wastewater treatment standards.« less

Impact Of Standing Water On Saltstone Placement II - Hydraulic Conductivity Data

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cozzi, A. D.; Pickenheim, B. R.

2012-12-06

The amount of water present during placement and subsequent curing of saltstone has the potential to impact several properties important for grout quality. An active drain water system can remove residual standing water and expose the surface of the placed saltstone to air. Oxidation of the saltstone may result in an increase in the leachability of redox sensitive elements. A dry surface can lead to cracking, causing an increase in hydraulic conductivity. An inactive drain water system can allow standing water that generates unnecessary hydrostatic head on the vault walls. Standing water that cannot be removed via the drain systemmore » will be available for potential incorporation into subsequent grout placements. The objective of this work is to study the impact of standing water on grout quality pertaining to disposal units. A series of saltstone mixes was prepared and cured at ambient temperature to evaluate the impact of standing water on saltstone placement. The samples were managed to control drying effects on leachability by either exposing or capping the samples. The water to premix ratio was varied to represent a range of processing conditions. Samples were analyzed for density, leachability, and hydraulic conductivity. Report SRNL-STI-2012-00546 was issued detailing the experimental procedure, results, and conclusions related to density and leachability. In the previous report, it was concluded that: density tends to increase toward the bottom of the samples. This effect is pronounced with excess bleed water; drying of the saltstone during curing leads to decreased Leachability Index (more leaching) for potassium, sodium, rhenium, nitrite, and nitrate; there is no noticeable effect on saltstone oxidation/leachability by changing the water to premix ratio (over the range studied), or by pouring into standing water (when tested up to 10 volume percent). The hydraulic conductivity data presented in this report show that samples cured exposed to the atmosphere had about three orders of magnitude higher hydraulic conductivity than any of the other samples. Considering these data, along with the results presented in the previous report, leads to the conclusion that small changes in water to premix ratio and the inclusion of up to 10 volume percent standing water should not be expected to have a detrimental effect on saltstone grout quality. The hydraulic conductivity results further demonstrate that curing in a moist environment is critical to maintaining saltstone quality.« less

Solvent Hold Tank Sample Results for MCU-16-701-702-703: May 2016 Monthly Sample and MCU-16-710-711-712: May 2016 Superwashed Sample

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fondeur, F. F.; Jones, D. H.

The Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-701, MCU-16-702 and MCU-16-703), pulled on 05/23/2016, and another set of SHT samples (MCU-16-710, MCU-16-711, and MCU-16-712) were pulled on 05/28/2016 after the solvent was superwashed with 300 mM sodium hydroxide for analysis. Samples MCU-16-701, MCU-16-702, and MCU-16-703 were combined into one sample (MCU-16-701-702-703) and samples MCU-16-710, MCU- 16-711, and MCU-16-712 were combined into one sample (MCU-16-710-711-712). Of the two composite samples MCU-16-710-711-712 represents the current chemical state of the solvent at MCU. All analytical conclusions are based on the chemical analysis of MCU-16-710-711-712. Theremore » were no chemical differences between MCU-16-701-702-703 and superwashed MCU-16-710-711-712. Analysis of the composited sample MCU-16-710-712-713 indicated the Isopar™L concentration is above its nominal level (102%). The modifier (CS-7SB) is 16% below its nominal concentration, while the TiDG and MaxCalix concentrations are at and above their nominal concentrations, respectively. The TiDG level has begun to decrease, and it is 7% below its nominal level as of May 28, 2016. Based on this current analysis, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended.« less

Sample Results from MCU Solids Outage

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T.; Washington, A.; Oji, L.

2014-09-22

Savannah River National Laboratory (SRNL) has received several solid and liquid samples from MCU in an effort to understand and recover from the system outage starting on April 6, 2014. SRNL concludes that the presence of solids in the Salt Solution Feed Tank (SSFT) is the likely root cause for the outage, based upon the following discoveries: A solids sample from the extraction contactor #1 proved to be mostly sodium oxalate; A solids sample from the scrub contactor#1 proved to be mostly sodium oxalate; A solids sample from the Salt Solution Feed Tank (SSFT) proved to be mostly sodium oxalate;more » An archived sample from Tank 49H taken last year was shown to contain a fine precipitate of sodium oxalate; A solids sample from ; A liquid sample from the SSFT was shown to have elevated levels of oxalate anion compared to the expected concentration in the feed. Visual inspection of the SSFT indicated the presence of precipitated or transferred solids, which were likely also in the Salt Solution Receipt Tank (SSRT). The presence of the solids coupled with agitation performed to maintain feed temperature resulted in oxalate solids migration through the MCU system and caused hydraulic issues that resulted in unplanned phase carryover from the extraction into the scrub, and ultimately the strip contactors. Not only did this carryover result in the Strip Effluent (SE) being pushed out of waste acceptance specification, but it resulted in the deposition of solids into several of the contactors. At the same time, extensive deposits of aluminosilicates were found in the drain tube in the extraction contactor #1. However it is not known at this time how the aluminosilicate solids are related to the oxalate solids. The solids were successfully cleaned out of the MCU system. However, future consideration must be given to the exclusion of oxalate solids into the MCU system. There were 53 recommendations for improving operations recently identified. Some additional considerations or additional details are provided below as recommendations. From this point on, IC-Anions analyses of the DSSHT should be part of the monthly routine analysis in order to spot negative trends in the oxalate leaving the MCU system. Care must be taken to monitor the oxalate content to watch for sudden precipitation of oxalate salts in the system; Conduct a study to optimize the cleaning strategy at ARP-MCU through decreasing the concentration or entirely eliminating the oxalic acid; The contents of the SSFT should remain unagitated. Routine visual observation should be maintained to ensure there is not a large buildup of solids. As water with agitation provided sufficient removal of the solids in the feed tank, it should be considered as a good means for dissolving oxalate solids if they are found in the future; Conduct a study to improve prediction of oxalate solubility in salt batch feed materials. As titanium and mercury have been found in various solids in this report, evaluate if either element plays a role in oxalate solubility during processing; Salt batch characterization focuses primarily on characterization and testing of unaltered Tank 21H material; however, non-typical feeds are developed through cleaning, washing, and/or sump transfers. As these solutions are processed through MCU, they may precipitate solids or reduce performance. Salt batch characterization and testing should be expanded to encompass a broader range of feeds that may be processed through ARPMCU.« less

User Guide for GoldSim Model to Calculate PA/CA Doses and Limits

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, F.

2016-10-31

A model to calculate doses for solid waste disposal at the Savannah River Site (SRS) and corresponding disposal limits has been developed using the GoldSim commercial software. The model implements the dose calculations documented in SRNL-STI-2015-00056, Rev. 0 “Dose Calculation Methodology and Data for Solid Waste Performance Assessment (PA) and Composite Analysis (CA) at the Savannah River Site”.

Comparison of U.S. Environmental Protection Agency’s CAP88 PC versions 3.0 and 4.0

DOE PAGES

Jannik, Tim; Farfan, Eduardo B.; Dixon, Ken; ...

2015-08-01

The Savannah River National Laboratory (SRNL) with the assistance of Georgia Regents University, completed a comparison of the U.S. Environmental Protection Agency's (EPA) environmental dosimetry code CAP88 PC V3.0 with the recently developed V4.0. CAP88 is a set of computer programs and databases used for estimation of dose and risk from radionuclide emissions to air. At the U.S. Department of Energy's Savannah River Site, CAP88 is used by SRNL for determining compliance with EPA's National Emission Standards for Hazardous Air Pollutants (40 CFR 61, Subpart H) regulations. Using standardized input parameters, individual runs were conducted for each radionuclide within itsmore » corresponding database. Some radioactive decay constants, human usage parameters, and dose coefficients changed between the two versions, directly causing a proportional change in the total effective 137Cs, 3H, 129I, 239Pu, and 90Sr) is provided. In general, the total effective doses will decrease for alpha/beta emitters because of reduced inhalation and ingestion rates in V4.0. However, for gamma emitters, such as 60Co and 137Cs, the total effective doses will increase because of changes EPA made in the external ground shine calculations.« less

ANALYTICAL PLANS SUPPORTING THE SWPF GAP ANALYSIS BEING CONDUCTED WITH ENERGYSOLUTIONS AND THE VITREOUS STATE LABORATORY AT THE CUA

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edwards, T.; Peeler, D.

2014-10-28

EnergySolutions (ES) and its partner, the Vitreous State Laboratory (VSL) of The Catholic University of America (CUA), are to provide engineering and technical services support to Savannah River Remediation, LLC (SRR) for ongoing operation of the Defense Waste Processing Facility (DWPF) flowsheet as well as for modifications to improve overall plant performance. SRR has requested that the glass formulation team of Savannah River National Laboratory (SRNL) and ES-VSL develop a technical basis that validates the current Product Composition Control System models for use during the processing of the coupled flowsheet or that leads to the refinements of or modifications tomore » the models that are needed so that they may be used during the processing of the coupled flowsheet. SRNL has developed a matrix of test glasses that are to be batched and fabricated by ES-VSL as part of this effort. This document provides two analytical plans for use by ES-VSL: one plan is to guide the measurement of the chemical composition of the study glasses while the second is to guide the measurement of the durability of the study glasses based upon the results of testing by ASTM’s Product Consistency Test (PCT) Method A.« less

The Coming Nuclear Renaissance for Next Generation Safeguards Specialists--Maximizing Potential and Minimizing the Risks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eipeldauer, Mary D

2009-01-01

This document is intended to provide an overview of the workshop entitled 'The Coming Nuclear Renaissance for the Next Generation Safeguards Experts-Maximizing Benefits While Minimizing Proliferation Risks', conducted at Oak Ridge National Laboratory (ORNL) in partnership with the Y-12 National Security Complex (Y-12) and the Savannah River National Laboratory (SRNL). This document presents workshop objectives; lists the numerous participant universities and individuals, the nuclear nonproliferation lecture topics covered, and the facilities tours taken as part of the workshop; and discusses the university partnership sessions and proposed areas for collaboration between the universities and ORNL for 2009. Appendix A contains themore » agenda for the workshop; Appendix B lists the workshop attendees and presenters with contact information; Appendix C contains graphics of the evaluation form results and survey areas; and Appendix D summarizes the responses to the workshop evaluation form. The workshop was an opportunity for ORNL, Y-12, and SRNL staff with more than 30 years combined experience in nuclear nonproliferation to provide a comprehensive overview of their expertise for the university professors and their students. The overall goal of the workshop was to emphasize nonproliferation aspects of the nuclear fuel cycle and to identify specific areas where the universities and experts from operations and national laboratories could collaborate.« less

YIELD STRESS REDUCTION OF DWPF MELTER FEED SLURRIES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stone, M; Michael02 Smith, M

2006-12-28

The Defense Waste Processing Facility (DWPF) at the Savannah River Site vitrifies High Level Waste for repository internment. The process consists of three major steps: waste pretreatment, vitrification, and canister decontamination/sealing. The HLW consists of insoluble metal hydroxides (primarily iron, aluminum, magnesium, manganese, and uranium) and soluble sodium salts (carbonate, hydroxide, nitrite, nitrate, sulfate). The pretreatment process acidifies the sludge with nitric and formic acids, adds the glass formers as glass frit, then concentrates the resulting slurry to approximately 50 weight percent (wt%) total solids. This slurry is fed to the joule-heated melter where the remaining water is evaporated followedmore » by calcination of the solids and conversion to glass. The Savannah River National Laboratory (SRNL) is currently assisting DWPF efforts to increase throughput of the melter. As part of this effort, SRNL has investigated methods to increase the solids content of the melter feed to reduce the heat load required to complete the evaporation of water and allow more of the energy available to calcine and vitrify the waste. The process equipment in the facility is fixed and cannot process materials with high yield stresses, therefore increasing the solids content will require that the yield stress of the melter feed slurries be reduced. Changing the glass former added during pretreatment from an irregularly shaped glass frit to nearly spherical beads was evaluated. The evaluation required a systems approach which included evaluations of the effectiveness of beads in reducing the melter feed yield stress as well as evaluations of the processing impacts of changing the frit morphology. Processing impacts of beads include changing the settling rate of the glass former (which effects mixing and sampling of the melter feed slurry and the frit addition equipment) as well as impacts on the melt behavior due to decreased surface area of the beads versus frit. Beads were produced from the DWPF process frit by fire polishing. The frit was allowed to free fall through a flame, then quenched with a water spray. Approximately 90% of the frit was converted to beads by this process, as shown in Figure 1. Borosilicate beads of various diameters were also procured for initial testing.« less

Chemical Composition Analysis and Product Consistency Tests of the ORP Phase 5 Nepheline Study Glasses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fox, K. M.; Edwards, T. B.; Caldwell, M. E.

In this report, the Savannah River National Laboratory (SRNL) provides chemical analyses and Product Consistency Test (PCT) results for a series of simulated high-level waste glass compositions fabricated by the Pacific Northwest National Laboratory (PNNL). These data will be used in the development of improved models for the prediction of nepheline crystallization in support of the Hanford Tank Waste Treatment and Immobilization Plant (WTP).

Determination of the crystalline structure of scale solids from the 16H evaporator gravity drain line to tank 38H

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oji, L. N.

2015-10-01

August 2015, scale solids from the 16H Evaporator Gravity Drain Line (GDL) to the Tank 38H were delivered to SRNL for analysis. The desired analytical goal was to identify and confirm the crystalline structure of the scale material and determine if the form of the aluminosilicate mineral was consistent with previous analysis of the scale material from the GDL.

Testing of the Defense Waste Processing Facility Cold Chemical Dissolution Method in Sludge Batch 9 Qualification

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edwards, T.; Pareizs, J.; Coleman, C.

For each sludge batch that is processed in the Defense Waste Processing Facility (DWPF), the Savannah River National Laboratory (SRNL) tests the applicability of the digestion methods used by the DWPF Laboratory for elemental analysis of Sludge Receipt and Adjustment Tank (SRAT) Receipt samples and SRAT Product process control samples. DWPF SRAT samples are typically dissolved using a method referred to as the DWPF Cold Chemical or Cold Chem Method (CC), (see DWPF Procedure SW4- 15.201). Testing indicates that the CC method produced mixed results. The CC method did not result in complete dissolution of either the SRAT Receipt ormore » SRAT Product with some fine, dark solids remaining. However, elemental analyses did not reveal extreme biases for the major elements in the sludge when compared with analyses obtained following dissolution by hot aqua regia (AR) or sodium peroxide fusion (PF) methods. The CC elemental analyses agreed with the AR and PF methods well enough that it should be adequate for routine process control analyses in the DWPF after much more extensive side-by-side tests of the CC method and the PF method are performed on the first 10 SRAT cycles of the Sludge Batch 9 (SB9) campaign. The DWPF Laboratory should continue with their plans for further tests of the CC method during these 10 SRAT cycles.« less

Thermal Release of 3He from Tritium Aged LaNi 4.25Al 0.75 Hydride

DOE PAGES

Staack, Gregory C.; Crowder, Mark L.; Klein, James E.

2015-02-01

Recently, the demand for He-3 has increased dramatically due to widespread use in nuclear nonproliferation, cryogenic, and medical applications. Essentially all of the world’s supply of He-3 is created by the radiolytic decay of tritium. The Savannah River Site Tritium Facilities (SRS-TF) utilizes LANA.75 in the tritium process to store hydrogen isotopes. The vast majority of He-3 “born” from tritium stored in LANA.75 is trapped in the hydride metal matrix. The SRS-TF has multiple LANA.75 tritium storage beds that have been retired from service with significant quantities of He-3 trapped in the metal. To support He-3 recovery, the Savannah Rivermore » National Laboratory (SRNL) conducted thermogravimetric analysis coupled with mass spectrometry (TGA-MS) on a tritium aged LANA.75 sample. TGA-MS testing was performed in an argon environment. Prior to testing, the sample was isotopically exchanged with deuterium to reduce residual tritium and passivated with air to alleviate pyrophoric concerns associated with handling the material outside of an inert glovebox. Analyses indicated that gas release from this sample was bimodal, with peaks near 220 and 490°C. The first peak consisted of both He-3 and residual hydrogen isotopes, the second was primarily He-3. The bulk of the gas was released by 600 °C« less

DEVELOPMENT AND DEPLOYMENT OF VACUUM SALT DISTILLATION AT THE SAVANNAH RIVER SITE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pierce, R.; Pak, D.; Edwards, T.

2010-10-28

The Savannah River Site has a mission to dissolve fissile materials and disposition them. The primary fissile material is plutonium dioxide (PuO{sub 2}). To support dissolution of these materials, the Savannah River National Laboratory (SRNL) designed and demonstrated a vacuum salt distillation (VSD) apparatus using both representative radioactive samples and non-radioactive simulant materials. Vacuum salt distillation, through the removal of chloride salts, increases the quantity of materials suitable for processing in the site's HB-Line Facility. Small-scale non-radioactive experiments at 900-950 C show that >99.8 wt % of the initial charge of chloride salt distilled from the sample boat with recoverymore » of >99.8 wt % of the ceric oxide (CeO{sub 2}) - the surrogate for PuO{sub 2} - as a non-chloride bearing 'product'. Small-scale radioactive testing in a glovebox demonstrated the removal of sodium chloride (NaCl) and potassium chloride (KCl) from 13 PuO{sub 2} samples. Chloride concentrations were distilled from a starting concentration of 1.8-10.8 wt % to a final concentration <500 mg/kg chloride. Initial testing of a non-radioactive, full-scale production prototype is complete. A designed experiment evaluated the impact of distillation temperature, time at temperature, vacuum, product depth, and presence of a boat cover. Significant effort has been devoted to mechanical considerations to facilitate simplified operation in a glovebox.« less

Equilibrium studies of oxalate and aluminum containing solutions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hay, M. S.; King, W. D.; Peters, T. B.

2015-11-01

The Savannah River National Laboratory (SRNL) was tasked to develop data on the solubility and conditions leading to precipitation of sodium oxalate, sodium nitrate, Bayerite (a polymorph of gibbsite, Al(OH) 3), and sodium aluminosilicate solids recently found in the Modular Caustic Side Solvent Extraction Unit (MCU). The data generated will be used to improve the OLI Systems thermodynamic database for these compounds allowing better prediction of solids formation by the modeling software in the future.

Comparison of U.S. Environmental Protection Agency's CAP88 PC Versions 3.0 and 4.0.

PubMed

Jannik, Tim; Farfan, Eduardo B; Dixon, Ken; Newton, Joseph; Sailors, Christopher; Johnson, Levi; Moore, Kelsey; Stahman, Richard

2015-08-01

The Savannah River National Laboratory (SRNL) with the assistance of Georgia Regents University, completed a comparison of the U.S. Environmental Protection Agency's (U.S. EPA) environmental dosimetry code CAP88 PC V3.0 with the recently developed V4.0. CAP88 is a set of computer programs and databases used for estimation of dose and risk from radionuclide emissions to air. At the U.S. Department of Energy's Savannah River Site, CAP88 is used by SRNL for determining compliance with U.S. EPA's National Emission Standards for Hazardous Air Pollutants (40 CFR 61, Subpart H) regulations. Using standardized input parameters, individual runs were conducted for each radionuclide within its corresponding database. Some radioactive decay constants, human usage parameters, and dose coefficients changed between the two versions, directly causing a proportional change in the total effective dose. A detailed summary for select radionuclides of concern at the Savannah River Site (60Co, 137Cs, 3H, 129I, 239Pu, and 90Sr) is provided. In general, the total effective doses will decrease for alpha/beta emitters because of reduced inhalation and ingestion rates in V4.0. However, for gamma emitters, such as 60Co and 137Cs, the total effective doses will increase because of changes U.S. EPA made in the external ground shine calculations.

FINAL REPORT ON GDE GAP CELL

DOE Office of Scientific and Technical Information (OSTI.GOV)

Herman, D.; Summers, W.; Danko, E.

2009-09-28

A project has been undertaken to develop an electrochemical cell and support equipment for evaluation of a gas diffusion electrode-based, narrow-electrolyte-gap anode for SO{sub 2} oxidation in the hydrogen production cycle of the hybrid sulfur (HyS) process. The project supported the HyS development program at the Savannah River National Lab (SRNL). The benefits of using a gas diffusion electrode in conjunction with the narrow anolyte gap are being determined through electrochemical polarization testing under a variety conditions, and by comparison to results produced by SRNL and others using anode technologies that have no anolyte gap. These test results indicate thatmore » the NGA cell has low resistance suitable for use in the HyS electrolyzer, exhibits good efficiency at high current densities compared to the direct feed HyS electrolyzer, and indicates robust performance in extended testing over 65 hours. Seepage episodes were mostly caused by port clogging, which can be mitigated in future designs through minor modifications to the hardware. Significant reductions in sulfur crossover have not yet been demonstrated in the NGA configuration compared to in-house direct feed testing, but corroborative sulfur layer analysis is as yet incomplete. Further testing in a single-pass anolyte configuration is recommended for complete evaluation of steady-state electrochemical efficiency and SO{sub 2} crossover in the narrow gap configuration.« less

Organics Characterization Of DWPF Alternative Reductant Simulants, Glycolic Acid, And Antifoam 747

DOE Office of Scientific and Technical Information (OSTI.GOV)

White, T. L.; Wiedenman, B. J.; Lambert, D. P.

The present study examines the fate of glycolic acid and other organics added in the Chemical Processing Cell (CPC) of the Defense Waste Processing Facility (DWPF) as part of the glycolic alternate flowsheet. Adoption of this flowsheet is expected to provide certain benefits in terms of a reduction in the processing time, a decrease in hydrogen generation, simplification of chemical storage and handling issues, and an improvement in the processing characteristics of the waste stream including an increase in the amount of nitrate allowed in the CPC process. Understanding the fate of organics in this flowsheet is imperative because tankmore » farm waste processed in the CPC is eventually immobilized by vitrification; thus, the type and amount of organics present in the melter feed may affect optimal melt processing and the quality of the final glass product as well as alter flammability calculations on the DWPF melter off gas. To evaluate the fate of the organic compounds added as the part of the glycolic flowsheet, mainly glycolic acid and antifoam 747, samples of simulated waste that was processed using the DWPF CPC protocol for tank farm sludge feed were generated and analyzed for organic compounds using a variety of analytical techniques at the Savannah River National Laboratory (SRNL). These techniques included Ion Chromatography (IC), Gas Chromatography-Mass Spectrometry (GC-MS), Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES), and Nuclear Magnetic Resonance (NMR) Spectroscopy. A set of samples were also sent to the Catholic University of America Vitreous State Laboratory (VSL) for analysis by NMR Spectroscopy at the University of Maryland, College Park. Analytical methods developed and executed at SRNL collectively showed that glycolic acid was the most prevalent organic compound in the supernatants of Slurry Mix Evaporator (SME) products examined. Furthermore, the studies suggested that commercially available glycolic acid contained minor amounts of impurities such as formic and diglycolic acid that were then carried over in the SME products. Oxalic acid present in the simulated tank farm waste was also detected. Finally, numerous other compounds, at low concentrations, were observed present in etheric extracts of aqueous supernate solutions of the SME samples and are thought to be breakdown products of antifoam 747. The data collectively suggest that although addition of glycolic acid and antifoam 747 will introduce a number of impurities and breakdown products into the melter feed, the concentrations of these organics is expected to remain low and may not significantly impact REDOX or off-gas flammability predictions. In the SME products examined presently, which contained variant amounts of glycolic acid and antifoam 747, no unexpected organic degradation product was found at concentrations above 500 mg/kg, a reasonable threshold concentration for an organic compound to be taken into account in the REDOX modeling. This statement does not include oxalic or formic acid that were sometimes observed above 500 mg/kg and acetic acid that has an analytical detection limit of 1250 mg/kg due to high glycolate concentration in the SME products tested. Once a finalized REDOX equation has been developed and implemented, REDOX properties of known organic species will be determined and their impact assessed. Although no immediate concerns arose during the study in terms of a negative impact of organics present in SME products of the glycolic flowsheet, evidence of antifoam degradation suggest that an alternative antifoam to antifoam 747 is worth considering. The determination and implementation of an antifoam that is more hydrolysis resistant would have benefits such as increasing its effectiveness over time and reducing the generation of degradation products.« less

ACID EVAPORATION OF ULTIMA GOLD TM AB LIQUID SCINTILLATION COCKTAIL RESIDUE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kyser, E.; Fondeur, F.; Crump, S.

2011-12-21

Prior analyses of samples from the F/H Lab solutions showed the presence of diisopropylnapthalene (DIN), a major component of Ultima Gold{trademark} AB liquid scintillation cocktail (LSC). These solutions are processed through H-Canyon Tank 10.5 and ultimately through the 17.8E evaporator. Similar solutions originated in SRNL streams sent to the same H Canyon tanks. This study examined whether the presence of these organics poses a process-significant hazard for the evaporator. Evaporation and calorimetry testing of surrogate samples containing 2000 ppm of Ultima Gold{trademark} AB LSC in 8 M nitric acid have been completed. These experiments showed that although reactions between nitricmore » acid and the organic components do occur, they do not appear to pose a significant hazard for runaway reactions or generation of energetic compounds in canyon evaporators. The amount of off-gas generated was relatively modest and appeared to be well within the venting capacity of the H-Canyon evaporators. A significant fraction of the organic components likely survives the evaporation process primarily as non-volatile components that are not expected to represent any new process concerns during downstream operations such as neutralization. Laboratory Waste solutions containing minor amounts of DIN can be safely received, stored, transferred, and processed through the canyon waste evaporator.« less

DISTRIBUTION COEFICIENTS (KD) GENERATED FROM A CORE SAMPLE COLLECTED FROM THE SALTSTONE DISPOSAL FACILITY

DOE Office of Scientific and Technical Information (OSTI.GOV)

Almond, P.; Kaplan, D.

Core samples originating from Vault 4, Cell E of the Saltstone Disposal Facility (SDF) were collected in September of 2008 (Hansen and Crawford 2009, Smith 2008) and sent to SRNL to measure chemical and physical properties of the material including visual uniformity, mineralogy, microstructure, density, porosity, distribution coefficients (K{sub d}), and chemical composition. Some data from these experiments have been reported (Cozzi and Duncan 2010). In this study, leaching experiments were conducted with a single core sample under conditions that are representative of saltstone performance. In separate experiments, reducing and oxidizing environments were targeted to obtain solubility and Kd valuesmore » from the measurable species identified in the solid and aqueous leachate. This study was designed to provide insight into how readily species immobilized in saltstone will leach from the saltstone under oxidizing conditions simulating the edge of a saltstone monolith and under reducing conditions, targeting conditions within the saltstone monolith. Core samples were taken from saltstone poured in December of 2007 giving a cure time of nine months in the cell and a total of thirty months before leaching experiments began in June 2010. The saltstone from Vault 4, Cell E is comprised of blast furnace slag, class F fly ash, portland cement, and Deliquification, Dissolution, and Adjustment (DDA) Batch 2 salt solution. The salt solution was previously analyzed from a sample of Tank 50 salt solution and characterized in the 4QCY07 Waste Acceptance Criteria (WAC) report (Zeigler and Bibler 2009). Subsequent to Tank 50 analysis, additional solution was added to the tank solution from the Effluent Treatment Project as well as from inleakage from Tank 50 pump bearings (Cozzi and Duncan 2010). Core samples were taken from three locations and at three depths at each location using a two-inch diameter concrete coring bit (1-1, 1-2, 1-3; 2-1, 2-2, 2-3; 3-1, 3-2, 3-3) (Hansen and Crawford 2009). Leaching experiments were conducted with a section of core sample 3-2. All cores from location 3 were drilled without using water. Core sample 3-2 was drilled from approximately six inches to a depth of approximately 13 inches. Approximately six inches of the core was removed but it broke into two pieces during removal from the bit. At the time of drilling, core material appeared olive green in color (Smith 2008). The fact that the samples were cored as olive green and were received after storage with a gray outer layer is indicative that some oxidation had occurred prior to leaching studies.« less

Chemical composition analysis and product consistency tests supporting refinement of the Nepheline model for the high aluminum Hanford Glass composition region

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fox, K. M.; Edwards, T. B.; Mcclane, D. L.

2016-02-17

In this report, SRNL provides chemical analyses and Product Consistency Test (PCT) results for a series of simulated HLW glasses fabricated by Pacific Northwest National Laboratory (PNNL) as part of an ongoing nepheline crystallization study. The results of these analyses will be used to improve the ability to predict crystallization of nepheline as a function of composition and heat treatment for glasses formulated at high alumina concentrations.

Verification of Sulfate Attack Penetration Rates for Saltstone Disposal Unit Modeling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Flach, G. P.

Recent Special Analysis modeling of Saltstone Disposal Units consider sulfate attack on concrete and utilize degradation rates estimated from Cementitious Barriers Partnership software simulations. This study provides an independent verification of those simulation results using an alternative analysis method and an independent characterization data source. The sulfate penetration depths estimated herein are similar to the best-estimate values in SRNL-STI-2013-00118 Rev. 2 and well below the nominal values subsequently used to define Saltstone Special Analysis base cases.

EFFECTS OF GAMMA IRRADIATION ON EPDM ELASTOMERS (REVISION 1)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Clark, E.

Two formulations of EPDM elastomer, one substituting a UV stabilizer for the normal antioxidant in this polymer, and the other the normal formulation, were synthesized and samples of each were exposed to gamma irradiation in initially pure deuterium gas to compare their radiation stability. Stainless steel containers having rupture disks were designed for this task. After 130 MRad dose of cobalt-60 radiation in the SRNL Gamma Irradiation Facility, a significant amount of gas was created by radiolysis; however the composition indicated by mass spectroscopy indicated an unexpected increase in the total amount deuterium in both formulations. The irradiated samples retainedmore » their ductility in a bend test. No change of sample weight, dimensions, or density was observed. No change of the glass transition temperature as measured by dynamic mechanical analysis was observed, and most of the other dynamic mechanical properties remained unchanged. There appeared to be an increase in the storage modulus of the irradiated samples containing the UV stabilizer above the glass transition, which may indicate hardening of the material by radiation damage. Revision 1 adds a comparison with results of a study of tritium exposed EPDM. The amount of gas produced by the gamma irradiation was found to be equivalent to about 280 days exposure to initially pure tritium gas at one atmosphere. The glass transition temperature of the tritium exposed EPDM rose about 10°C. over 280 days, while no glass transition temperature change was observed for gamma irradiated EPDM. This means that gamma irradiation in deuterium cannot be used as a surrogate for tritium exposure.« less

POTENTIAL IMPACT OF TANK F FLUSH SOLUTION ON H-CANYON EVAPORATOR OPERATION

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kyser, E.; Fondeur, F.; Fink, S.

2010-09-13

Previous chemical analysis of a sample from the liquid heel found in Tank F of the High Activity Drain (HAD) system in F/H laboratory revealed the presence of n-paraffin, tributyl phosphate (TBP), Modifier from the Modular Caustic-Side Solvent Extraction Unit (MCU) process and a vinyl ester resin that is very similar to the protective lining on Tank F. Subsequent analyses detected the presence of a small amount of diisopropylnaphthalene (DIN) (major component of Ultima Gold{trademark} AB liquid scintillation cocktail). Indications are that both vinyl ester resin and DIN are present in small amounts in the flush solution. The flush solutionmore » currently in the LR-56S trailer likely has an emulsion which is believed to contain a mixture of the reported organic species dominated by TBP. An acid treatment similar to that proposed to clear the HAD tank heel in F/H laboratory was found to allow separation of an organic phase from the cloudy sample tested by SRNL. Mixing of that clear sample did re-introduce some cloudiness that did not immediately clear but that cloudiness is attributed to the DIN in the matrix. An organic phase does quickly separate from the cloudy matrix allowing separation by a box decanter in H-Canyon prior to transfer to the evaporator feed tank. This separation should proceed normally as long as the emulsion is broken-up by acidification.« less

Traditional and Model Based Assay of Irregular Geometry Items

DOE Office of Scientific and Technical Information (OSTI.GOV)

MOORE, FRANK S.; SALAYMEH, SALEEM

The Analytical Development Section (ADS) of SRNL was requested to perform a waste disposal assay of two heater boxes which had been used in the HB Line dissolvers. They had been sent to SRNL for study to make recommendations on how to prevent future failure of the units when they were replaced. The study having been completed, the units needed to be characterized prior to sending to Solid Waste for disposal. An assay station consisting of a turntable, HPGe detector, CANBERRA Inspector, transmission source and a portable computer was set up to do the required assays. The assays indicate themore » presence of U-235, Pu-239 and Cs-137. No measurable amounts of U-235 or Pu-239 were found. Therefore the Minimum Detectable Activities for U-235 and Pu-239 were calculated. For Heater Box 1, 0.23 grams of U-235 and 0.24 grams of Pu-239. For Heater Box 2, the results were 0.21 grams of U-235 and 0.21 grams of Pu-239. This paper describes and documents the assays employed to determine the amount of U, Pu and Cs contents of the heater boxes. The paper provides results of SNM assays using traditional calibration of the system and on one based on modeling. It also provides the scientific community with data that will assist the user in determining the method of choice for assaying items with irregular geometries.« less

Analysis of an MCU HEPA filter

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.; Fondeur, F. F.

A series of direct analyses on three portions (inlet, center, and outlet) of the High Efficiency Particulate Air (HEPA) filter material from the Modular Caustic-Side Solvent Extraction Unit (MCU) have been performed; this includes x-ray methods such as X-Ray Diffraction (XRD), Contained Scanning Electron Microscopy (CSEM) and X-Ray Fluorescence (XRF), as well as Fourier Transform InfraRed spectroscopy (FTIR). Additionally, two leaching studies (one with water, one with dichloromethane) have been performed on three portions (inlet, center, and outlet) of the HEPA filter material, with the leachates being analyzed by Inductively-coupled plasma emission spectroscopy (ICPES), Semi-Volatile Organic Analysis (SVOA) and gammascan.more » From the results of the analyses, SRNL feels that cesium-depleted solvent is being introduced into the HEPA filter. The most likely avenue for this is mechanical aerosolization of solvent, where the aerosol is then carried along an airstream into the HEPA filter. Once introduced into the HEPA filter media, the solvent wicks throughout the material, and migrates towards the outlet end. Once on the outlet end, continual drying could cause particulate flakes to exit the filter and travel farther down the airstream path.« less

SUMMARY OF 2010 DOE EM INTERNATIONAL PROGRAM STUDIES OF WASTE GLASS STRUCTURE AND PROPERTIES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fox, K.; Choi, A.; Marra, J.

2011-02-07

Collaborative work between the Savannah River National Laboratory (SRNL) and SIA Radon in Russia was divided among three tasks for calendar year 2010. The first task focused on the study of simplified high level waste glass compositions with the objective of identifying the compositional drivers that lead to crystallization and poor chemical durability. The second task focused on detailed characterization of more complex waste glass compositions with unexpectedly poor chemical durabilities. The third task focused on determining the structure of select high level waste glasses made with varying frit compositions in order to improve models under development for predicting themore » melt rate of the Defense Waste Processing Facility (DWPF) glasses. The majority of these tasks were carried out at SIA Radon. Selection and fabrication of the glass compositions, along with chemical composition measurements and evaluations of durability were carried out at SRNL and are described in this report. SIA Radon provided three summary reports based on the outcome of the three tasks. These reports are included as appendices to this document. Briefly, the result of characterization of the Task 1 glasses may indicate that glass compositions where iron is predominantly tetrahedrally coordinated have more of a tendency to crystallize nepheline or nepheline-like phases. For the Task 2 glasses, the results suggested that the relatively low fraction of tetrahedrally coordinated boron and the relatively low concentrations of Al{sub 2}O{sub 3} available to form [BO{sub 4/2}]{sup -}Me{sup +} and [AlO{sub 4/2}]{sup -}Me{sup +} tetrahedral units are not sufficient to consume all of the alkali ions, and thus these alkali ions are easily leached from the glasses. All of the twelve Task 3 glass compositions were determined to be mainly amorphous, with some minor spinel phases. Several key structural units such as metasilicate chains and rings were identified, which confirms the current modeling approach for the silicate phase. The coordination of aluminum and iron was found to be mainly tetrahedral, with some octahedral iron ions. In all samples, trigonally-coordinated boron was determined to dominate over tetrahedrally-coordinated boron. The results further suggested that BO{sub 4} tetrahedra and BO{sub 3} triangles form complex borate units and may be present as separate constituents. However, no quantification of tetrahedral-to-trigonal boron ratio was made.« less

APPLICATION OF VACUUM SALT DISTILLATION TECHNOLOGY FOR THE REMOVAL OF FLUORIDE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pierce, R.; Pak, D.

2011-08-10

Vacuum distillation of chloride salts from plutonium oxide (PuO{sub 2}) and simulant PuO{sub 2} has been previously demonstrated at Department of Energy (DOE) sites using kilogram quantities of chloride salt. The apparatus for vacuum distillation contains a zone heated using a furnace and a zone actively cooled using either recirculated water or compressed air. During a vacuum distillation operation, a sample boat containing the feed material is placed into the apparatus while it is cool, and the system is sealed. The system is evacuated using a vacuum pump. Once a sufficient vacuum is attained, heating begins. Volatile salts distill frommore » the heated zone to the cooled zone where they condense, leaving behind the non-volatile materials in the feed boat. The application of vacuum salt distillation (VSD) is of interest to the HB-Line Facility and the MOX Fuel Fabrication Facility (MFFF) at the Savannah River Site (SRS). Both facilities are involved in efforts to disposition excess fissile materials. Many of these materials contain chloride and fluoride salt concentrations which make them unsuitable for dissolution without prior removal of the chloride and fluoride salts. Between September 2009 and January 2011, the Savannah River National Laboratory (SRNL) and HB-Line designed, developed, tested, and successfully deployed a system for the distillation of chloride salts. Subsequent efforts are attempting to adapt the technology for the removal of fluoride. Fluoride salts of interest are less-volatile than the corresponding chloride salts. Consequently, an alternate approach is required for the removal of fluoride without significantly increasing the operating temperature. HB-Line Engineering requested SRNL to evaluate and demonstrate the feasibility of an alternate approach using both non-radioactive simulants and plutonium-bearing materials. Whereas the earlier developments targeted the removal of sodium chloride (NaCl) and potassium chloride (KCl), the current activities are concerned with the removal of the halide ions associated with plutonium trifluoride (PuF{sub 3}), plutonium tetrafluoride (PuF{sub 4}), calcium fluoride (CaF{sub 2}), and calcium chloride (CaCl{sub 2}). This report discusses non-radioactive testing of small-scale and pilot-scale systems and radioactive testing of a small-scale system. Experiments focused on demonstrating the chemistry for halide removal and addressing the primary engineering questions associated with a change in the process chemistry.« less

ROBOTICS IN HAZARDOUS ENVIRONMENTS - REAL DEPLOYMENTS BY THE SAVANNAH RIVER NATIONAL LABORATORY

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kriikku, E.; Tibrea, S.; Nance, T.

The Research & Development Engineering (R&DE) section in the Savannah River National Laboratory (SRNL) engineers, integrates, tests, and supports deployment of custom robotics, systems, and tools for use in radioactive, hazardous, or inaccessible environments. Mechanical and electrical engineers, computer control professionals, specialists, machinists, welders, electricians, and mechanics adapt and integrate commercially available technology with in-house designs, to meet the needs of Savannah River Site (SRS), Department of Energy (DOE), and other governmental agency customers. This paper discusses five R&DE robotic and remote system projects.

Integration of the Uncertainties of Anion and TOC Measurements into the Flammability Control Strategy for Sludge Batch 8 at the DWPF

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edwards, T. B.

2013-03-14

The Savannah River National Laboratory (SRNL) has been working with the Savannah River Remediation (SRR) Defense Waste Processing Facility (DWPF) in the development and implementation of a flammability control strategy for DWPF’s melter operation during the processing of Sludge Batch 8 (SB8). SRNL’s support has been in response to technical task requests that have been made by SRR’s Waste Solidification Engineering (WSE) organization. The flammability control strategy relies on measurements that are performed on Slurry Mix Evaporator (SME) samples by the DWPF Laboratory. Measurements of nitrate, oxalate, formate, and total organic carbon (TOC) standards generated by the DWPF Laboratory aremore » presented in this report, and an evaluation of the uncertainties of these measurements is provided. The impact of the uncertainties of these measurements on DWPF’s strategy for controlling melter flammability also is evaluated. The strategy includes monitoring each SME batch for its nitrate content and its TOC content relative to the nitrate content and relative to the antifoam additions made during the preparation of the SME batch. A linearized approach for monitoring the relationship between TOC and nitrate is developed, equations are provided that integrate the measurement uncertainties into the flammability control strategy, and sample calculations for these equations are shown to illustrate the impact of the uncertainties on the flammability control strategy.« less

CHARACTERIZATION OF TANK 5F VERTICAL COOLING COIL LEACHATES FOR SELECT RADIONUCLIDES 2011

DOE Office of Scientific and Technical Information (OSTI.GOV)

Oji, L.; Diprete, D.

2001-08-17

Two twenty-four inch samples of vertical sections of the cooling coils from Tank 5F, taken from Riser 1, were made available to SRNL by SRR for leaching and characterization of the leachates for select radionuclide trapped in the corrosion layer on the exterior of the cooling coils. One piece of cooling coil sample was obtained from a section of a vertical cooling coil located above the 45-inch elevation from the tank floor and the other also from a vertical section of a cooling coil located below the 45-inch elevation from the tank floor of Tank 5F. Analysis results from bothmore » cooling coils show that the predominant radionuclides contributing to the activity in both coils are strontium-90 and cesium-137. The activities for strontium-90 and cesium-137 in the Tank 5F vertical cooling coil located above the 45-inch elevation of the tank and designated as sample 5-R1-A45 averaged 1.34E-02 {+-} 1.12E-03 and 7.27E-04 {+-} 4.46E-05 Ci/ft{sup 2}, respectively, while the activities for the vertical cooling coil located below the 45-inch elevation of the tank and designated as sample 5-R1-B45 averaged 8.93E-03 {+-} 8.25E-04 for Sr-90 and 8.10E-04 {+-} 6.36E-05 Ci/ft{sup 2} for Cs-137. Other significant activity contributing radionuclides are americium-241 and europium-154/155. With the exception of the analysis result for Pu-241 in the 5-R1-A45 cooling coils samples, the target detection limits for the other radionuclides were met in both cooling coil samples. The detection limits for Pu-241 analyses result in coil sample 5-R1-A45 were not met consistently because of possible background changes during counting.« less

HLW Flexible jumper materials compatibility evaluation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Skidmore, T. E.

H-Tank Farm Engineering tasked SRNL/Materials Science & Technology (MS&T) to evaluate the compatibility of Goodyear Viper® chemical transfer hose with HLW solutions. The hose is proposed as a flexible Safety Class jumper for up to six months service. SRNL/MS&T performed various tests to evaluate the effects of radiation, high pH chemistry and elevated temperature on the hose, particularly the inner liner. Test results suggest an upper dose limit of 50 Mrad for the hose. Room temperature burst pressure values at 50 Mrad are estimated at 600- 800 psi, providing a safety factor of 4.0-5.3X over the anticipated operating pressure ofmore » 150 psi and a safety factor of 3.0-4.0X over the working pressure of the hose (200 psi), independent of temperature effects. Radiation effects are minimal at doses less than 10 Mrad. Doses greater than 50 Mrad may be allowed, depending on operating conditions and required safety factors, but cannot be recommended at this time. At 250 Mrad, burst pressure values are reduced to the hose working pressure. At 300 Mrad, burst pressures are below 150 psi. At a bounding continuous dose rate of 57,870 rad/hr, the 50 Mrad dose limit is reached within 1.2 months. Actual dose rates may be lower, particularly during non-transfer periods. Refined dose calculations are therefore recommended to justify longer service. This report details the tests performed and interpretation of the results. Recommendations for shelf-life/storage, component quality verification, and post-service examination are provided.« less

SIMULATION OF THE ICELAND VOLCANIC ERUPTION OF APRIL 2010 USING THE ENSEMBLE SYSTEM

DOE Office of Scientific and Technical Information (OSTI.GOV)

Buckley, R.

2011-05-10

The Eyjafjallajokull volcanic eruption in Iceland in April 2010 disrupted transportation in Europe which ultimately affected travel plans for many on a global basis. The Volcanic Ash Advisory Centre (VAAC) is responsible for providing guidance to the aviation industry of the transport of volcanic ash clouds. There are nine such centers located globally, and the London branch (headed by the United Kingdom Meteorological Office, or UKMet) was responsible for modeling the Iceland volcano. The guidance provided by the VAAC created some controversy due to the burdensome travel restrictions and uncertainty involved in the prediction of ash transport. The Iceland volcanicmore » eruption provides a useful exercise of the European ENSEMBLE program, coordinated by the Joint Research Centre (JRC) in Ispra, Italy. ENSEMBLE, a decision support system for emergency response, uses transport model results from a variety of countries in an effort to better understand the uncertainty involved with a given accident scenario. Model results in the form of airborne concentration and surface deposition are required from each member of the ensemble in a prescribed format that may then be uploaded to a website for manipulation. The Savannah River National Laboratory (SRNL) is the lone regular United States participant throughout the 10-year existence of ENSEMBLE. For the Iceland volcano, four separate source term estimates have been provided to ENSEMBLE participants. This paper focuses only on one of those source terms. The SRNL results in relation to other modeling agency results along with useful information obtained using an ensemble of transport results will be discussed.« less

Development and Demonstration of Material Properties Database and Software for the Simulation of Flow Properties in Cementitious Materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, F.; Flach, G.

This report describes work performed by the Savannah River National Laboratory (SRNL) in fiscal year 2014 to develop a new Cementitious Barriers Project (CBP) software module designated as FLOExcel. FLOExcel incorporates a uniform database to capture material characterization data and a GoldSim model to define flow properties for both intact and fractured cementitious materials and estimate Darcy velocity based on specified hydraulic head gradient and matric tension. The software module includes hydraulic parameters for intact cementitious and granular materials in the database and a standalone GoldSim framework to manipulate the data. The database will be updated with new data asmore » it comes available. The software module will later be integrated into the next release of the CBP Toolbox, Version 3.0. This report documents the development efforts for this software module. The FY14 activities described in this report focused on the following two items that form the FLOExcel package; 1) Development of a uniform database to capture CBP data for cementitious materials. In particular, the inclusion and use of hydraulic properties of the materials are emphasized; and 2) Development of algorithms and a GoldSim User Interface to calculate hydraulic flow properties of degraded and fractured cementitious materials. Hydraulic properties are required in a simulation of flow through cementitious materials such as Saltstone, waste tank fill grout, and concrete barriers. At SRNL these simulations have been performed using the PORFLOW code as part of Performance Assessments for salt waste disposal and waste tank closure.« less

Impacts of glycolate and formate radiolysis and thermolysis on hydrogen generation rate calculations for the Savannah River Site tank farm

DOE Office of Scientific and Technical Information (OSTI.GOV)

Crawford, C. L.; King, W. D.

Savannah River Remediation (SRR) personnel requested that the Savannah River National Laboratory (SRNL) evaluate available data and determine its applicability to defining the impact of planned glycolate anion additions to Savannah River Site (SRS) High Level Waste (HLW) on Tank Farm flammability (primarily with regard to H 2 production). Flammability evaluations of formate anion, which is already present in SRS waste, were also needed. This report describes the impacts of glycolate and formate radiolysis and thermolysis on Hydrogen Generation Rate (HGR) calculations for the SRS Tank Farm.

PROPERTIES IMPORTANT TO MIXING FOR WTP LARGE SCALE INTEGRATED TESTING

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koopman, D.; Martino, C.; Poirier, M.

2012-04-26

Large Scale Integrated Testing (LSIT) is being planned by Bechtel National, Inc. to address uncertainties in the full scale mixing performance of the Hanford Waste Treatment and Immobilization Plant (WTP). Testing will use simulated waste rather than actual Hanford waste. Therefore, the use of suitable simulants is critical to achieving the goals of the test program. External review boards have raised questions regarding the overall representativeness of simulants used in previous mixing tests. Accordingly, WTP requested the Savannah River National Laboratory (SRNL) to assist with development of simulants for use in LSIT. Among the first tasks assigned to SRNL wasmore » to develop a list of waste properties that matter to pulse-jet mixer (PJM) mixing of WTP tanks. This report satisfies Commitment 5.2.3.1 of the Department of Energy Implementation Plan for Defense Nuclear Facilities Safety Board Recommendation 2010-2: physical properties important to mixing and scaling. In support of waste simulant development, the following two objectives are the focus of this report: (1) Assess physical and chemical properties important to the testing and development of mixing scaling relationships; (2) Identify the governing properties and associated ranges for LSIT to achieve the Newtonian and non-Newtonian test objectives. This includes the properties to support testing of sampling and heel management systems. The test objectives for LSIT relate to transfer and pump out of solid particles, prototypic integrated operations, sparger operation, PJM controllability, vessel level/density measurement accuracy, sampling, heel management, PJM restart, design and safety margin, Computational Fluid Dynamics (CFD) Verification and Validation (V and V) and comparison, performance testing and scaling, and high temperature operation. The slurry properties that are most important to Performance Testing and Scaling depend on the test objective and rheological classification of the slurry (i.e., Newtonian or non-Newtonian). The most important properties for testing with Newtonian slurries are the Archimedes number distribution and the particle concentration. For some test objectives, the shear strength is important. In the testing to collect data for CFD V and V and CFD comparison, the liquid density and liquid viscosity are important. In the high temperature testing, the liquid density and liquid viscosity are important. The Archimedes number distribution combines effects of particle size distribution, solid-liquid density difference, and kinematic viscosity. The most important properties for testing with non-Newtonian slurries are the slurry yield stress, the slurry consistency, and the shear strength. The solid-liquid density difference and the particle size are also important. It is also important to match multiple properties within the same simulant to achieve behavior representative of the waste. Other properties such as particle shape, concentration, surface charge, and size distribution breadth, as well as slurry cohesiveness and adhesiveness, liquid pH and ionic strength also influence the simulant properties either directly or through other physical properties such as yield stress.« less

CHEMICAL ANALYSIS OF SIMULATED HIGH LEVEL WASTE GLASSES TO SUPPORT SULFATE SOLUBILITY MODELING

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fox, K.; Marra, J.

2014-08-14

The U.S. Department of Energy (DOE), Office of Environmental Management (EM) is sponsoring an international, collaborative project to develop a fundamental model for sulfate solubility in nuclear waste glass. The solubility of sulfate has a significant impact on the achievable waste loading for nuclear waste forms both within the DOE complex and to some extent at U.K. sites. The development of enhanced borosilicate glass compositions with improved sulfate solubility will allow for higher waste loadings and accelerated cleanup missions. Much of the previous work on improving sulfate retention in waste glasses has been done on an empirical basis, making itmore » difficult to apply the findings to future waste compositions despite the large number of glass systems studied. A more fundamental, rather than empirical, model of sulfate solubility in glass, under development at Sheffield Hallam University (SHU), could provide a solution to the issues of sulfate solubility. The model uses the normalized cation field strength index as a function of glass composition to predict sulfate capacity, and has shown early success for some glass systems. The objective of the current scope is to mature the sulfate solubility model to the point where it can be used to guide glass composition development for DOE waste vitrification efforts, allowing for enhanced waste loadings and waste throughput. A series of targeted glass compositions was selected to resolve data gaps in the current model. SHU fabricated these glasses and sent samples to the Savannah River National Laboratory (SRNL) for chemical composition analysis. SHU will use the resulting data to enhance the sulfate solubility model and resolve any deficiencies. In this report, SRNL provides chemical analyses for simulated waste glasses fabricated SHU in support of sulfate solubility model development. A review of the measured compositions revealed that there are issues with the B{sub 2}O{sub 3} and Fe{sub 2}O{sub 3} concentrations missing their targeted values by a significant amount for several of the study glasses. SHU is reviewing the fabrication of these glasses and the chemicals used in batching them to identify the source of these issues. The measured sulfate concentrations were all below their targeted values. This is expected, as the targeted concentrations likely exceeded the solubility limit for sulfate in these glass compositions. Some volatilization of sulfate may also have occurred during fabrication of the glasses. Measurements of the other oxides in the study glasses were reasonably close to their targeted values« less

Actual Waste Demonstration of the Nitric-Glycolic Flowsheet for Sludge Batch 9 Qualification

DOE Office of Scientific and Technical Information (OSTI.GOV)

J. D. Newell; Pareizs, J. M.; Martino, C. J.

For each sludge batch that is processed in the Defense Waste Processing Facility (DWPF), the Savannah River National Laboratory (SRNL) performs qualification testing to demonstrate that the sludge batch is processable. Testing performed by the Savannah River National Laboratory has shown glycolic acid to be effective in replacing the function of formic acid in the DWPF chemical process. The nitric-glycolic flowsheet reduces mercury, significantly lowers the catalytic generation of hydrogen and ammonia which could allow purge reduction in the Sludge Receipt and Adjustment Tank (SRAT), stabilizes the pH and chemistry in the SRAT and the Slurry Mix Evaporator (SME), allowsmore » for effective rheology adjustment, and is favorable with respect to melter flammability. In order to implement the new flowsheet, SRAT and SME cycles, designated SC-18, were performed using a Sludge Batch (SB) 9 slurry blended from SB8 Tank 40H and Tank 51H samples. The SRAT cycle involved adding nitric and glycolic acids to the sludge, refluxing to steam strip mercury, and dewatering to a targeted solids concentration. Data collected during the SRAT cycle included offgas analyses, process temperatures, heat transfer, and pH measurements. The SME cycle demonstrated the addition of glass frit and the replication of six canister decontamination additions. The demonstration concluded with dewatering to a targeted solids concentration. Data collected during the SME cycle included offgas analyses, process temperatures, heat transfer, and pH measurements. Slurry and condensate samples were collected for subsequent analysis« less

DOE-EM-45 PACKAGING OPERATIONS AND MAINTENANCE COURSE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Watkins, R.; England, J.

2010-05-28

Savannah River National Laboratory - Savannah River Packaging Technology (SRNL-SRPT) delivered the inaugural offering of the Packaging Operations and Maintenance Course for DOE-EM-45's Packaging Certification Program (PCP) at the University of South Carolina Aiken on September 1 and 2, 2009. Twenty-nine students registered, attended, and completed this training. The DOE-EM-45 Packaging Certification Program (PCP) sponsored the presentation of a new training course, Packaging Maintenance and Operations, on September 1-2, 2009 at the University of South Carolina Aiken (USC-Aiken) campus in Aiken, SC. The premier offering of the course was developed and presented by the Savannah River National Laboratory, and attendedmore » by twenty-nine students across the DOE, NNSA and private industry. This training informed package users of the requirements associated with handling shipping containers at a facility (user) level and provided a basic overview of the requirements typically outlined in Safety Analysis Report for Packaging (SARP) Chapters 1, 7, and 8. The course taught packaging personnel about the regulatory nature of SARPs to help reduce associated and often costly packaging errors. Some of the topics covered were package contents, loading, unloading, storage, torque requirements, maintaining records, how to handle abnormal conditions, lessons learned, leakage testing (including demonstration), and replacement parts. The target audience for this course was facility operations personnel, facility maintenance personnel, and field quality assurance personnel who are directly involved in the handling of shipping containers. The training also aimed at writers of SARP Chapters 1, 7, and 8, package designers, and anyone else involved in radioactive material packaging and transportation safety. Student feedback and critiques of the training were very positive. SRNL will offer the course again at USC Aiken in September 2010.« less

242-16H 2H EVAPORATOR POT SAMPLING FINAL REPORT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Krementz, D; William Cheng, W

2008-06-11

Due to the materials that are processed through 2H Evaporator, scale is constantly being deposited on the surfaces of the evaporator pot. In order to meet the requirements of the Nuclear Criticality Safety Analysis/Evaluation (NCSA/NCSE) for 2H Evaporator, inspections of the pot are performed to determine the extent of scaling. Once the volume of scale reaches a certain threshold, the pot must be chemically cleaned to remove the scale. Prior to cleaning the pot, samples of the scale are obtained to determine the concentration of uranium and plutonium and also to provide information to assist with pot cleaning. Savannah Rivermore » National Laboratory (SRNL) was requested by Liquid Waste Organization (LWO) Engineering to obtain these samples from two locations within the evaporator. Past experience has proven the difficulty of successfully obtaining solids samples from the 2H Evaporator pot. To mitigate this risk, a total of four samplers were designed and fabricated to ensure that two samples could be obtained. Samples had previously been obtained from the cone surface directly below the vertical access riser using a custom scraping tool. This tool was fabricated and deployed successfully. A second scraper was designed to obtain sample from the nearby vertical thermowell and a third scraper was designed to obtain sample from the vertical pot wall. The newly developed scrapers both employed a pneumatically actuated elbow. The scrapers were designed to be easily attached/removed from the elbow assembly. These tools were fabricated and deployed successfully. A fourth tool was designed to obtain sample from the opposite side of the pot under the tube bundle. This tool was fabricated and tested, but the additional modifications required to make the tool field-ready could not be complete in time to meet the aggressive deployment schedule. Two samples were obtained near the pot entry location, one from the pot wall and the other from the evaporator feed pipe. Since a third sampler was available and all of the radiological controls were in place, the decision was made to obtain a third sample. The third sampler dropped directly below the riser to obtain a scrape sample from the evaporator cone. Samples were obtained from all of these locations in sufficient quantities to perform the required analysis.« less

Low temperature dissolution flowsheet for plutonium metal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Daniel, W. E.; Almond, P. M.; Rudisill, T. S.

2016-05-01

The H-Canyon flowsheet used to dissolve Pu metal for PuO 2 production utilizes boiling HNO 3. SRNL was requested to develop a complementary dissolution flowsheet at two reduced temperature ranges. The dissolution and H 2 generation rates of Pu metal were investigated using a dissolving solution at ambient temperature (20-30 °C) and for an intermediate temperature of 50-60 °C. Additionally, the testing included an investigation of the dissolution rates and characterization of the off-gas generated from the ambient temperature dissolution of carbon steel cans and the nylon bags that contain the Pu metal when charged to the dissolver.

Test report dot 7A type a liquid packaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ketusky, E. T.; Brandjes, C.; Benoit, T. J.

This test report documents the performance of Savannah River National Laboratory’s (SRNL’s) U.S. Department of Transportation (DOT) Specification 7A; General Packaging, Type A shielded liquid shipping packaging and compliance with the regulatory requirements of Title 49 of the Code of Federal Regulations (CFR). The primary use of this packaging design is for the transport of radioactive liquids of up to 1.3 liters in an unshielded configuration and up to 113 mL of radioactive liquids in a shielded configuration, with no more than an A2 quantity in either configuration, over public highways and/or commercial aircraft. The contents are liquid radioactive materialsmore » sufficiently shielded and within the activity limits specified in173.435 or 173.433 for A2 (normal form) materials, as well as within the analyzed thermal heat limits. Any contents must be compatibly packaged and must be compatible with the packaging. The basic packaging design is based on the U.S. Department of Energy’s (DOE’s) Model 9979 Type A fissile shipping packaging designed and tested by SRNL. The shielded liquid configuration consists of the outer and inner drums of the 9979 package with additional low density polyethylene (LDPE) dunnage nesting a tungsten shielded cask assembly (WSCA) within the 30-gallon inner drum. The packaging model for the DOT Specification 7A, Type A liquids packaging is HVYTAL.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Raszewski, F; Tommy Edwards, T; David Peeler, D

Sludge Batch 4 (SB4) is currently being processed in the Defense Waste Processing Facility (DWPF) using Frit 510. The slurry pumps in Tank 40 are experiencing in-leakage of bearing water, which is causing the sludge slurry feed in Tank 40 to become dilute at a rapid rate. Currently, the DWPF is removing this dilution water by performing caustic boiling during the Sludge Receipt and Adjustment Tank (SRAT) cycle. In order to alleviate prolonged SRAT cycle times that may eventually impact canister production rates, decant scenarios of 100, 150, and 200 kilogallons of supernate were proposed for Tank 40 during themore » DWPF March outage. Based on the results of the preliminary assessment issued by the Savannah River National Laboratory (SRNL), the Liquid Waste Organization (LWO) issued a Technical Task Request (TTR) for SRNL to (1) perform a more detailed evaluation using updated SB4 compositional information and (2) assess the viability of Frit 510 and determine any potential impacts on the SB4 system. As defined in the TTR, LWO requested that SRNL validate the sludge--only SB4 flowsheet and the coupled operations flowsheet using the 100K gallon decant volume as well as the addition of 3 wt% sodium on a calcined oxide basis. Approximately 12 historical glasses were identified during a search of the ComProTM database that are located within at least one of the five glass regions defined by the proposed SB4 flowsheet options. While these glasses meet the requirements of a variability study there was some concern that the compositional coverage did not adequately bound all cases. Therefore, SRNL recommended that a supplemental experimental variability study be performed to support the various SB4 flowsheet options that may be implemented for future SB4 operations in DWPF. Eighteen glasses were selected based on nominal sludge projections representing the current as well as the proposed flowsheets over a WL interval of interest to DWPF (32-42%). The intent of the experimental portion of the variability study is to demonstrate that the glasses of the Frit 510-modified SB4 compositional region (Cases No.1-5) are both acceptable relative to the Environmental Assessment (EA) reference glass and predictable by the current DWPF process control models for durability. Frit 510 is a viable option for the processing of SB4 after a Tank 40 decant and the addition of products from the Actinide Removal Process (ARP). The addition of ARP did not have any negative impacts on the acceptability and predictability of the variability study glasses. The results of the variability study indicate that all of the study glasses (both quenched and centerline canister cooled (ccc)) have normalized releases for boron that are well below the reference EA glass (16.695 g/L). The durabilities of all of the study glasses are predictable using the current Product Composition Control System (PCCS) durability models with the exception of SB4VAR24ccc (Case No.2 at 41%). PCCS is not applicable to non-homogeneous glasses (i.e. glasses containing crystals such as acmite and nepheline), thus SB4VAR24ccc should not be predictable as it contains nepheline. The presence of nepheline has been confirmed in both SB4VAR13ccc and SB4VAR24ccc by X-ray diffraction (XRD). These two glasses are the first results which indicate that the current nepheline discriminator value of 0.62 is not conservative. The nepheline discriminator was implemented into PCCS for SB4 based on the fact that all of the historical glasses evaluated with nepheline values of 0.62 or greater did not contain nepheline via XRD analysis. Although these two glasses do cause some concern over the use of the 0.62 nepheline value for future DWPF glass systems, the impact to the current SB4 system is of little concern. More specifically, the formation of nepheline was observed in glasses targeting 41 or 42% WL. Current processing of the Frit 510-SB4 system in DWPF has nominally targeted 34% WL. For the SB4 variability study glasses targeting these lower WLs, nepheline formation was not observed and the minimal difference in PCT response between quenched and ccc versions supported its absence.« less

Analysis of Monolith Cores from an Engineering Scale Demonstration of a Prospective Cast Stone Process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Crawford, C. L.; Cozzi, A. D.; Hill, K. A.

2016-06-01

The primary disposition path of Low Activity Waste (LAW) at the DOE Hanford Site is vitrification. A cementitious waste form is one of the alternatives being considered for the supplemental immobilization of the LAW that will not be treated by the primary vitrification facility. Washington River Protection Solutions (WRPS) has been directed to generate and collect data on cementitious or pozzolanic waste forms such as Cast Stone. This report documents the coring and leach testing of monolithic samples cored from an engineering-scale demonstration (ES Demo) with non-radioactive simulants. The ES Demo was performed at SRNL in October of 2013 usingmore » the Scaled Continuous Processing Facility (SCPF) to fill an 8.5 ft. diameter x 3.25 ft. high container with simulated Cast Stone grout. The Cast Stone formulation was chosen from the previous screening tests. Legacy salt solution from previous Hanford salt waste testing was adjusted to correspond to the average LAW composition generated from the Hanford Tank Waste Operation Simulator (HTWOS). The dry blend materials, ordinary portland cement (OPC), Class F fly ash, and ground granulated blast furnace slag (GGBFS or BFS), were obtained from Lafarge North America in Pasco, WA. In 2014 core samples originally obtained approximately six months after filling the ES Demo were tested along with bench scale molded samples that were collected during the original pour. A latter set of core samples were obtained in late March of 2015, eighteen months after completion of the original ES Demo. Core samples were obtained using a 2” diameter x 11” long coring bit. The ES Demo was sampled in three different regions consisting of an outer ring, a middle ring and an inner core zone. Cores from these three lateral zones were further segregated into upper, middle and lower vertical segments. Monolithic core samples were tested using the Environmental Protection Agency (EPA) Method 1315, which is designed to provide mass transfer rates (release rates) of inorganic analytes contained in monolithic material under diffusion controlled release conditions as a function of leaching time. Compressive strength measurements and drying tests were also performed on the 2015 samples. Leachability indices reported are based on analyte concentrations determined from dissolution of the dried samples.« less

RESULTS OF THE FY09 ENHANCED DOE HIGH LEVEL WASTE MELTER THROUGHPUT STUDIES AT SRNL

DOE Office of Scientific and Technical Information (OSTI.GOV)

Johnson, F.; Edwards, T.

2010-06-23

High-level waste (HLW) throughput (i.e., the amount of waste processed per unit time) is a function of two critical parameters: waste loading (WL) and melt rate. For the Waste Treatment and Immobilization Plant (WTP) at the Hanford Site and the Defense Waste Processing Facility (DWPF) at the Savannah River Site (SRS), increasing HLW throughput would significantly reduce the overall mission life cycle costs for the Department of Energy (DOE). The objective of this task is to develop data, assess property models, and refine or develop the necessary models to support increased WL of HLW at SRS. It is a continuationmore » of the studies initiated in FY07, but is under the specific guidance of a Task Change Request (TCR)/Work Authorization received from DOE headquarters (Project Number RV071301). Using the data generated in FY07, FY08 and historical data, two test matrices (60 glasses total) were developed at the Savannah River National Laboratory (SRNL) in order to generate data in broader compositional regions. These glasses were fabricated and characterized using chemical composition analysis, X-ray Diffraction (XRD), viscosity, liquidus temperature (TL) measurement and durability as defined by the Product Consistency Test (PCT). The results of this study are summarized below: (1) In general, the current durability model predicts the durabilities of higher waste loading glasses quite well. A few of the glasses exhibited poorer durability than predicted. (2) Some of the glasses exhibited anomalous behavior with respect to durability (normalized leachate for boron (NL [B])). The quenched samples of FY09EM21-02, -07 and -21 contained no nepheline or other wasteform affecting crystals, but have unacceptable NL [B] values (> 10 g/L). The ccc sample of FY09EM21-07 has a NL [B] value that is more than one half the value of the quenched sample. These glasses also have lower concentrations of Al{sub 2}O{sub 3} and SiO{sub 2}. (3) Five of the ccc samples (EM-13, -14, -15, -29 and -30) completely crystallized with both magnetite and nepheline, and still had extremely low NL [B] values. These particular glasses have more CaO present than any of the other glasses in the matrix. It appears that while all of the glasses contain nepheline, the NL [B] values decrease as the CaO concentration increases from 2.3 wt% to 4.3 wt%. A different form of nepheline may be created at higher concentrations of CaO that does not significantly reduce glass durability. (4) The T{sub L} model appears to be under-predicting the measured values of higher waste loading glasses. Trends in T{sub L} with composition are not evident in the data from these studies. (5) A small number of glasses in the FY09 matrix have measured viscosities that are much lower than the viscosity range over which the current model was developed. The decrease in viscosity is due to a higher concentration of non-bridging oxygens (NBO). A high iron concentration is the cause of the increase in NBO. Durability, viscosity and T{sub L} data collected during FY07 and FY09 that specifically targeted higher waste loading glasses was compiled and assessed. It appears that additional data may be required to expand the coverage of the T{sub L} and viscosity models for higher waste loading glasses. In general, the compositional regions of the higher waste loading glasses are very different than those used to develop these models. On the other hand, the current durability model seems to be applicable to the new data. At this time, there is no evidence to modify this model; however additional experimental studies should be conducted to determine the cause of the anomalous durability data.« less

DEVELOPMENT OF AN ANTIFOAM TRACKING SYSTEM AS AN OPTION TO SUPPORT THE MELTER OFF-GAS FLAMMABILITY CONTROL STRATEGY AT THE DWPF

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edwards, T.; Lambert, D.

The Savannah River National Laboratory (SRNL) has been working with the Savannah River Remediation (SRR) Defense Waste Processing Facility (DWPF) in the development and implementation of an additional strategy for confidently satisfying the flammability controls for DWPF’s melter operation. An initial strategy for implementing the operational constraints associated with flammability control in DWPF was based upon an analytically determined carbon concentration from antifoam. Due to the conservative error structure associated with the analytical approach, its implementation has significantly reduced the operating window for processing and has led to recurrent Slurry Mix Evaporator (SME) and Melter Feed Tank (MFT) remediation. Tomore » address the adverse operating impact of the current implementation strategy, SRR issued a Technical Task Request (TTR) to SRNL requesting the development and documentation of an alternate strategy for evaluating the carbon contribution from antifoam. The proposed strategy presented in this report was developed under the guidance of a Task Technical and Quality Assurance Plan (TTQAP) and involves calculating the carbon concentration from antifoam based upon the actual mass of antifoam added to the process assuming 100% retention. The mass of antifoam in the Additive Mix Feed Tank (AMFT), in the Sludge Receipt and Adjustment Tank (SRAT), and in the SME is tracked by mass balance as part of this strategy. As these quantities are monitored, the random and bias uncertainties affecting their values are also maintained and accounted for. This report documents: 1) the development of an alternate implementation strategy and associated equations describing the carbon concentration from antifoam in each SME batch derived from the actual amount of antifoam introduced into the AMFT, SRAT, and SME during the processing of the batch. 2) the equations and error structure for incorporating the proposed strategy into melter off-gas flammability assessments. Sample calculations of the system are also included in this report. Please note that the system developed and documented in this report is intended as an alternative to the current, analytically-driven system being utilized by DWPF; the proposed system is not intended to eliminate the current system. Also note that the system developed in this report to track antifoam mass in the AMFT, SRAT, and SME will be applicable beyond just Sludge Batch 8. While the model used to determine acceptability of the SME product with respect to melter off-gas flammability controls must be reassessed for each change in sludge batch, the antifoam mass tracking methodology is independent of sludge batch composition and as such will be transferable to future sludge batches.« less

RADIOLOGICAL SURVEY STATION DEVELOPMENT FOR THE PIT DISASSEMBLY AND CONVERSION PROJECT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dalmaso, M.; Gibbs, K.; Gregory, D.

2011-05-22

The Savannah River National Laboratory (SRNL) has developed prototype equipment to demonstrate remote surveying of Inner and Outer DOE Standard 3013 containers for fixed and transferable contamination in accordance with DOE Standard 3013 and 10 CFR 835 Appendix B. When fully developed the equipment will be part of a larger suite of equipment used to package material in accordance with DOE Standard 3013 at the Pit Disassembly and Conversion Project slated for installation at the Savannah River Site. The prototype system consists of a small six-axis industrial robot with an end effector consisting of a force sensor, vacuum gripper andmore » a three fingered pneumatic gripper. The work cell also contains two alpha survey instruments, swipes, swipe dispenser, and other ancillary equipment. An external controller interfaces with the robot controller, survey instruments and other ancillary equipment to control the overall process. SRNL is developing automated equipment for the Pit Disassembly and Conversion (PDC) Project that is slated for the Savannah River Site (SRS). The equipment being developed is automated packaging equipment for packaging plutonium bearing materials in accordance with DOE-STD-3013-2004. The subject of this paper is the development of a prototype Radiological Survey Station (RSS). Other automated equipment being developed for the PDC includes the Bagless transfer System, Outer Can Welder, Gantry Robot System (GRS) and Leak Test Station. The purpose of the RSS is to perform a frisk and swipe of the DOE Standard 3013 Container (either inner can or outer can) to check for fixed and transferable contamination. This is required to verify that the contamination levels are within the limits specified in DOE-STD-3013-2004 and 10 CFR 835, Appendix D. The surface contamination limit for the 3013 Outer Can (OC) is 500 dpm/100 cm2 (total) and 20 dpm/100 cm2 (transferable). This paper will concentrate on the RSS developments for the 3013 OC but the system for the 3013 Inner Can (IC) is nearly identical.« less

Evaluation and Mitigation of the Risk Due to Climate Change at the Department of Energy's Savannah River Site

NASA Astrophysics Data System (ADS)

Werth, D. W.

2016-12-01

The state of South Carolina, home to the Department of Energy's (DOE) Savannah River Site (SRS), has been identified as facing an `above average' risk due to extreme heat, and the threat due to wildfire is expected to nearly double by 2050. To comply with DOE requirements that each of its sites prepares for climate change, the Savannah River National Laboratory (SRNL) is involved in an ongoing process to evaluate the site vulnerability and establish policies to mitigate those effects. This requires close cooperation between the managers of various site facilities and on-site climate researchers. The Atmospheric Technologies Group at SRNL currently provides short-term weather forecasts to support outdoor activities on site, but is also now working with site decision-makers to achieve DOE's goals of climate change mitigation and adaptation. We will discuss the results of our climate vulnerability assessment, which includes the effects of climate change on the energy requirements for mission critical infrastructure, the health, safety and productivity of the outdoor workforce, the danger of fire in the SRS forest, and the levels of surface water impoundments. (The latter of which must be maintained to avoid the release of radioactive contaminants sequestered beneath them). For each of these, existing climate change projections were carefully studied and `translated' into numerical indices relevant to facility personnel at SRS, along with a vulnerability rating (also based on conversations with site workers) to estimate the most endangered `assets'. We will also explain the process we have developed to facilitate effective communication between researchers and managers - involving them both in the development of the climate vulnerability assessment and the next steps toward planning, resource allocation, actions to mitigate rising costs, and safety considerations as well as helping the site remain sustainable throughout the future of its missions.

ANNUAL RADIOACTIVE WASTE TANK INSPECTION PROGRAM 2009

DOE Office of Scientific and Technical Information (OSTI.GOV)

West, B.; Waltz, R.

2010-06-21

Aqueous radioactive wastes from Savannah River Site (SRS) separations and vitrification processes are contained in large underground carbon steel tanks. Inspections made during 2009 to evaluate these vessels and other waste handling facilities along with evaluations based on data from previous inspections are the subject of this report. The 2009 inspection program revealed that the structural integrity and waste confinement capability of the Savannah River Site waste tanks were maintained. All inspections scheduled per LWO-LWE-2008-00423, HLW Tank Farm Inspection Plan for 2009, were completed. All Ultrasonic measurements (UT) performed in 2009 met the requirements of C-ESG-00006, In-Service Inspection Program formore » High Level Waste Tanks, Rev. 1, and WSRC-TR-2002-00061, Rev.4. UT inspections were performed on Tank 29 and the findings are documented in SRNL-STI-2009-00559, Tank Inspection NDE Results for Fiscal Year 2009, Waste Tank 29. Post chemical cleaning UT measurements were made in Tank 6 and the results are documented in SRNL-STI-2009-00560, Tank Inspection NDE Results Tank 6, Including Summary of Waste Removal Support Activities in Tanks 5 and 6. A total of 6669 photographs were made and 1276 visual and video inspections were performed during 2009. Twenty-Two new leaksites were identified in 2009. The locations of these leaksites are documented in C-ESR-G-00003, SRS High Level Waste Tank Leaksite Information, Rev.4. Fifteen leaksites at Tank 5 were documented during tank wall/annulus cleaning activities. Five leaksites at Tank 6 were documented during tank wall/annulus cleaning activities. Two new leaksites were identified at Tank 19 during waste removal activities. Previously documented leaksites were reactivated at Tanks 5 and 12 during waste removal activities. Also, a very small amount of additional leakage from a previously identified leaksite at Tank 14 was observed.« less

VALIDATION OF ANSI N42.34 AMERICAN NATIONAL STANDARD PERFORMANCE CRITERIA FOR HAND-HELD INSTRUMENTS FOR THE DETECTION AND IDENTIFICATION OF RADIONUCLIDES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lorier, T.

2014-09-03

SRNL’s validation of ANSI N42.34-D6 for the Domestic Nuclear Detection Office (DNDO) was performed utilizing one hand-held instrument (or RID) – the FLIR identiFINDER 2. Each section of the standard was evaluated via a walk-through or test. NOTE: In Table 1, W = walk-through and T = test, as directed by the Domestic Nuclear Detection Office (DNDO). For a walk-through, the experiment was either setup or reviewed for setup; for a test, the N42.34-D6 procedures were followed with some exceptions and comments noted. SRNL is not fully able to evaluate a RID against Sections 7 (Environmental), 8 (Electromagnetic), and 9more » (Mechanical) of N42.34, so those portions of this validation were done in collaboration with Qualtest, Inc. in Orlando, Florida. The walk-throughs and tests of Sections 7, 8, and 9 were performed in Qualtest, Inc. facilities with SRNL providing radiological sources as necessary. Where applicable, assessment results and findings of the walk-throughs and tests were recorded on datasheets and a validation summary is provided. A general comment pertained to test requirements found in another standard and referenced in N42.34-D6. For example, step 1 of the test method in section 8.1.2 states “RF test set up information can be found in IEC 61000-4-3.” It is recommended that any information from other standards necessary for conducting the tests within N42.34 should be posted in N42.34 for simplicity and to prevent the user from having to peruse other documents. Another general comment, as noted by Qualtest, is that a tolerance reference is not listed for each test in sections 7-9. Overall, the N42.34-D6 was proven to be practicable, but areas for improvement and recommendations were identified for consideration prior to final ballot submittal.« less

A BASIS FOR MODIFYING THE TANK 12 COMPOSITE SAMPLING DESIGN

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shine, G.

The SRR sampling campaign to obtain residual solids material from the Savannah River Site (SRS) Tank Farm Tank 12 primary vessel resulted in obtaining appreciable material in all 6 planned source samples from the mound strata but only in 5 of the 6 planned source samples from the floor stratum. Consequently, the design of the compositing scheme presented in the Tank 12 Sampling and Analysis Plan, Pavletich (2014a), must be revised. Analytical Development of SRNL statistically evaluated the sampling uncertainty associated with using various compositing arrays and splitting one or more samples for compositing. The variance of the simple meanmore » of composite sample concentrations is a reasonable standard to investigate the impact of the following sampling options. Composite Sample Design Option (a). Assign only 1 source sample from the floor stratum and 1 source sample from each of the mound strata to each of the composite samples. Each source sample contributes material to only 1 composite sample. Two source samples from the floor stratum would not be used. Composite Sample Design Option (b). Assign 2 source samples from the floor stratum and 1 source sample from each of the mound strata to each composite sample. This infers that one source sample from the floor must be used twice, with 2 composite samples sharing material from this particular source sample. All five source samples from the floor would be used. Composite Sample Design Option (c). Assign 3 source samples from the floor stratum and 1 source sample from each of the mound strata to each composite sample. This infers that several of the source samples from the floor stratum must be assigned to more than one composite sample. All 5 source samples from the floor would be used. Using fewer than 12 source samples will increase the sampling variability over that of the Basic Composite Sample Design, Pavletich (2013). Considering the impact to the variance of the simple mean of the composite sample concentrations, the recommendation is to construct each sample composite using four or five source samples. Although the variance using 5 source samples per composite sample (Composite Sample Design Option (c)) was slightly less than the variance using 4 source samples per composite sample (Composite Sample Design Option (b)), there is no practical difference between those variances. This does not consider that the measurement error variance, which is the same for all composite sample design options considered in this report, will further dilute any differences. Composite Sample Design Option (a) had the largest variance for the mean concentration in the three composite samples and should be avoided. These results are consistent with Pavletich (2014b) which utilizes a low elevation and a high elevation mound source sample and two floor source samples for each composite sample. Utilizing the four source samples per composite design, Pavletich (2014b) utilizes aliquots of Floor Sample 4 for two composite samples.« less

ANNULUS CLOSURE TECHNOLOGY DEVELOPMENT INSPECTION/SALT DEPOSIT CLEANING MAGNETIC WALL CRAWLER

DOE Office of Scientific and Technical Information (OSTI.GOV)

Minichan, R; Russell Eibling, R; James Elder, J

2008-06-01

The Liquid Waste Technology Development organization is investigating technologies to support closure of radioactive waste tanks at the Savannah River Site (SRS). Tank closure includes removal of the wastes that have propagated to the tank annulus. Although amounts and types of residual waste materials in the annuli of SRS tanks vary, simple salt deposits are predominant on tanks with known leak sites. This task focused on developing and demonstrating a technology to inspect and spot clean salt deposits from the outer primary tank wall located in the annulus of an SRS Type I tank. The Robotics, Remote and Specialty Equipmentmore » (RRSE) and Materials Science and Technology (MS&T) Sections of the Savannah River National Laboratory (SRNL) collaborated to modify and equip a Force Institute magnetic wall crawler with the tools necessary to demonstrate the inspection and spot cleaning in a mock-up of a Type I tank annulus. A remote control camera arm and cleaning head were developed, fabricated and mounted on the crawler. The crawler was then tested and demonstrated on a salt simulant also developed in this task. The demonstration showed that the camera is capable of being deployed in all specified locations and provided the views needed for the planned inspection. It also showed that the salt simulant readily dissolves with water. The crawler features two different techniques for delivering water to dissolve the salt deposits. Both water spay nozzles were able to dissolve the simulated salt, one is more controllable and the other delivers a larger water volume. The cleaning head also includes a rotary brush to mechanically remove the simulated salt nodules in the event insoluble material is encountered. The rotary brush proved to be effective in removing the salt nodules, although some fine tuning may be required to achieve the best results. This report describes the design process for developing technology to add features to a commercial wall crawler and the results of the demonstration testing performed on the integrated system. The crawler was modified to address the two primary objectives of the task (inspection and spot cleaning). SRNL recommends this technology as a viable option for annulus inspection and salt removal in tanks with minimal salt deposits (such as Tanks 5 and 6.) This report further recommends that the technology be prepared for field deployment by: (1) developing an improved mounting system for the magnetic idler wheel, (2) improving the robustness of the cleaning tool mounting, (3) resolving the nozzle selection valve connections, (4) determining alternatives for the brush and bristle assembly, and (5) adding a protective housing around the motors to shield them from water splash. In addition, SRNL suggests further technology development to address annulus cleaning issues that are apparent on other tanks that will also require salt removal in the future such as: (1) Developing a duct drilling device to facilitate dissolving salt inside ventilation ducts and draining the solution out the bottom of the ducts. (2) Investigating technologies to inspect inside the vertical annulus ventilation duct.« less

In-Tank Elutriation Test Report And Independent Assessment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Burns, H. H.; Adamson, D. J.; Qureshi, Z. H.

2011-04-13

The Department of Energy (DOE) Office of Environmental Management (EM) funded Technology Development and Deployment (TDD) to solve technical problems associated with waste tank closure for sites such as Hanford Site and Savannah River Site (SRS). One of the tasks supported by this funding at Savannah River National Laboratory (SRNL) and Pacific Northwest Laboratory (PNNL) was In-Tank Elutriation. Elutriation is the process whereby physical separation occurs based on particle size and density. This report satisfies the first phase of Task WP_1.3.1.1 In-Tank Elutriation, which is to assess the feasibility of this method of separation in waste tanks at Hanford Sitemore » and SRS. This report includes an analysis of scoping tests performed in the Engineering Development Laboratory of SRNL, analysis of Hanford's inadvertent elutriation, the viability of separation methods such as elutriation and hydrocyclones and recommendations for a path forward. This report will demonstrate that the retrieval of Hanford salt waste tank S-112 very successfully decreased the tank's inventories of radionuclides. Analyses of samples collected from the tank showed that concentrations of the major radionuclides Cs-136 and Sr-90 were decreased by factors of 250 and 6 and their total curie tank inventories decreased by factors of 60,000 and 2000. The total tank curie loading decreased from 300,000 Ci to 55 Ci. The remaining heel was nearly all innocuous gibbsite, Al(OH){sub 3}. However, in the process of tank retrieval approximately 85% of the tank gibbsite was also removed. Significant amounts of money and processing time could be saved if more gibbsite could be left in tanks while still removing nearly all of the radionuclides. There were factors which helped to make the elutriation of Tank S-112 successful which would not necessarily be present in all salt tanks. 1. The gibbsite particles in the tank were surprisingly large, as much as 200 {micro}m. The gibbsite crystals had probably grown in size over a period of decades. 2. The radionuclides were apparently either in the form of soluble compounds, like cesium, or micrometer sized particles of actinide oxides or hydroxides. 3. After the initial tank retrieval the tank contained cobble which is not conducive to elutriation. Only after the tank contents were treated with thousands of gallons of 50 wt% caustic, were the solids converted to sand which is compatible with elutriation. Discussions between SRNL and PNNL resulted in plans to test elutriation in two phases; in Phase 1 particles would be separated by differences in settling velocity in an existing scaled tank with its associated hardware and in Phase 2 additional hardware, such as a hydrocyclone, would be added downstream to separate slow settling partciels from liquid. Phase 1 of in-tank elutriation was tested for Proof of Principle in theEngineering Development Laboratory of SRNL in a 41" diameter, 87 gallon tank. The tank had been previously used as a 1/22 scale model of Hanford Waste Tank AY-102. The objective of the testing was to determine which tank operating parameters achieved the best separation between fast- and slow-settling particles. For Phase 1 testing a simulated waste tank supernatant, slow-settling particles and fast-settling particles were loaded to the scaled tank. Because this was a Proof of Principle test, readily available solids particles were used that represented fast-settling and slow-settling particles. The tank contents were agitated using rotating mixer jet pumps (MJP) which suspended solids while liquids and solids were drawn out of the tank with a suction tube. The goal was to determine the optimum hydraulic operating conditions to achieve clean separation in which the residual solids in the tank were nearly all fast-settling particles and the solids transferred out of the tank were nearly all slow-settling particles. Tests were conducted at different pump jet velocities, suction tube diameters and suction tube elevations. Testing revealed that the most important variable was jet velocity which translates to a downstream fluid velocity in the vicinity of the suction tube which can suspend particles and potentially allow their removal from the tank. The optimum jet velocity in the vicinity of the sucti9on tube was between 1.5 and 2 ft/s (4-5 gpm). During testing at lower velocities a significant amount of slow-settling particles remained in the tank. At higher velocities a significant amount of fast-settling particles were elutriated from the tank. It should be noted that this range of velocities is appropriate for this particular geometry and particles. However, the principle of In-Tank Elutriation was proved. In-tank elutriation has the potential to save much money in tank closure. However, more work, both analytical and experimental, must be done before an improved version of the process could be applied to actual waste tanks. It is recommended that testing with more prototypic simulants be conducted. Also, scale-up criteria for elutriation and the resulting size of pilot scale test equipment require investigation during future research. In addition, it is recommended that the use of hydrocyclones be pursued in Phase 2 testing. Hydrocyclones are a precise and efficient separation tool that are frequently used in industry.« less

DIissolution of low enriched uranium from the experimental breeder reactor-II fuel stored at the Idaho National Laboratory

DOE Office of Scientific and Technical Information (OSTI.GOV)

Daniel, G.; Rudisill, T.; Almond, P.

The Idaho National Laboratory (INL) is actively engaged in the development of electrochemical processing technology for the treatment of fast reactor fuels using irradiated fuel from the Experimental Breeder Reactor-II (EBR-II) as the primary test material. The research and development (R&D) activities generate a low enriched uranium (LEU) metal product from the electrorefining of the EBR-II fuel and the subsequent consolidation and removal of chloride salts by the cathode processor. The LEU metal ingots from past R&D activities are currently stored at INL awaiting disposition. One potential disposition pathway is the shipment of the ingots to the Savannah River Sitemore » (SRS) for dissolution in H-Canyon. Carbon steel cans containing the LEU metal would be loaded into reusable charging bundles in the H-Canyon Crane Maintenance Area and charged to the 6.4D or 6.1D dissolver. The LEU dissolution would be accomplished as the final charge in a dissolver batch (following the dissolution of multiple charges of spent nuclear fuel (SNF)). The solution would then be purified and the 235U enrichment downblended to allow use of the U in commercial reactor fuel. To support this potential disposition path, the Savannah River National Laboratory (SRNL) developed a dissolution flowsheet for the LEU using samples of the material received from INL.« less

A Module for Graphical Display of Model Results with the CBP Toolbox

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, F.

2015-04-21

This report describes work performed by the Savannah River National Laboratory (SRNL) in fiscal year 2014 to add enhanced graphical capabilities to display model results in the Cementitious Barriers Project (CBP) Toolbox. Because Version 2.0 of the CBP Toolbox has just been released, the graphing enhancements described in this report have not yet been integrated into a new version of the Toolbox. Instead they have been tested using a standalone GoldSim model and, while they are substantially complete, may undergo further refinement before full implementation. Nevertheless, this report is issued to document the FY14 development efforts which will provide amore » basis for further development of the CBP Toolbox.« less

Evaluation and Uncertainty of a New Method to Detect Suspected Nuclear and WMD Activity: Project Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kurzeja, R.; Werth, D.; Buckley, R.

The Atmospheric Technology Group at SRNL developed a new method to detect signals from Weapons of Mass Destruction (WMD) activities in a time series of chemical measurements at a downwind location. This method was tested with radioxenon measured in Russia and Japan after the 2013 underground test in North Korea. This LDRD calculated the uncertainty in the method with the measured data and also for a case with the signal reduced to 1/10 its measured value. The research showed that the uncertainty in the calculated probability of origin from the NK test site was small enough to confirm the test.more » The method was also wellbehaved for small signal strengths.« less

Characterization of DWPF recycle condensate tank materials

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bannochie, C. J.

2015-01-01

A Defense Waste Processing Facility (DWPF) Recycle Condensate Tank (RCT) sample was delivered to the Savannah River National Laboratory (SRNL) for characterization with particular interest in the concentration of I-129, U-233, U-235, total U, and total Pu. Since a portion of Salt Batch 8 will contain DWPF recycle materials, the concentration of I-129 is important to undertand for salt batch planning purposes. The chemical and physical characterizations are also needed as input to the interpretation of future work aimed at determining the propensity of the RCT material to foam, and methods to remediate any foaming potential. According to DWPF themore » Tank Farm 2H evaporator has experienced foaming while processing DWPF recycle materials. The characterization work on the RCT samples has been completed and is reported here. The composition of the Sludge Batch 8 (SB8) RCT material is largely a low base solution of 0.2M NaNO 2 and 0.1M NaNO 3 with a small amount of formate present. Insoluble solids comprise only 0.05 wt.% of the slurry. The solids appear to be largely sludge-like solids based on elemental composition and SEM-EDS analysis. The sample contains an elevated concentration of I-129 (38x) and substantial 59% fraction of Tc-99, as compared to the incoming SB8 Tank 40 feed material. The Hg concentration is 5x, when compared to Fe, of that expected based on sludge carryover. The total U and Pu concentrations are reduced significantly, 0.536 wt.% TS and 2.42E-03 wt.% TS, respectively, with the fissile components, U-233, U-235, Pu-239, and Pu-241, an order of magnitude lower in concentration than those in the SB8 Tank 40 DWPF feed material. This report will be revised to include the foaming study requested in the TTR and outlined in the TTQAP when that work is concluded.« less

SLURRY MIX EVAPORATOR BATCH ACCEPTABILITY AND TEST CASES OF THE PRODUCT COMPOSITION CONTROL SYSTEM WITH THORIUM AS A REPORTABLE ELEMENT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Edwards, T.

2010-10-07

The Defense Waste Processing Facility (DWPF), which is operated by Savannah River Remediation, LLC (SRR), has recently begun processing Sludge Batch 6 (SB6) by combining it with Frit 418 at a nominal waste loading (WL) of 36%. A unique feature of the SB6/Frit 418 glass system, as compared to the previous glass systems processed in DWPF, is that thorium will be a reportable element (i.e., concentrations of elemental thorium in the final glass product greater than 0.5 weight percent (wt%)) for the resulting wasteform. Several activities were initiated based upon this unique aspect of SB6. One of these was anmore » investigation into the impact of thorium on the models utilized in DWPF's Product Composition and Control System (PCCS). While the PCCS is described in more detail below, for now note that it is utilized by Waste Solidification Engineering (WSE) to evaluate the acceptability of each batch of material in the Slurry Mix Evaporator (SME) before this material is passed on to the melter. The evaluation employs models that predict properties associated with processability and product quality from the composition of vitrified samples of the SME material. The investigation of the impact of thorium on these models was conducted by Peeler and Edwards [1] and led to a recommendation that DWPF can process the SB6/Frit 418 glass system with ThO{sub 2} concentrations up to 1.8 wt% in glass. Questions also arose regarding the handling of thorium in the SME batch acceptability process as documented by Brown, Postles, and Edwards [2]. Specifically, that document is the technical bases of PCCS, and while Peeler and Edwards confirmed the reliability of the models, there is a need to confirm that the current implementation of DWPF's PCCS appropriately handles thorium as a reportable element. Realization of this need led to a Technical Task Request (TTR) prepared by Bricker [3] that identified some specific SME-related activities that the Savannah River National Laboratory (SRNL) was requested to conduct. SRNL issued a Task Technical and Quality Assurance (TT&QA) plan [4] in response to the SRR request. The conclusions provided in this report are that no changes need to be made to the SME acceptability process (i.e., no modifications to WSRC-TR-95-00364, Revision 5, are needed) and no changes need to be made to the Product Composition Control System (PCCS) itself (i.e. the spreadsheet utilized by Waste Solidification Engineering (WSE) for acceptability decisions does not require modification) in response to thorium becoming a reportable element for DWPF operations. In addition, the inputs and results for the two test cases requested by WSE for use in confirming the successful activation of thorium as a reportable element for DWPF operations during the processing of SB6 are presented in this report.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zamecnik, J. R.; Edwards, T. B.

The conversions of nitrite to nitrate, the destruction of glycolate, and the conversion of glycolate to formate and oxalate were modeled for the Nitric-Glycolic flowsheet using data from Chemical Process Cell (CPC) simulant runs conducted by SRNL from 2011 to 2015. The goal of this work was to develop empirical correlations for these variables versus measureable variables from the chemical process so that these quantities could be predicted a-priori from the sludge composition and measurable processing variables. The need for these predictions arises from the need to predict the REDuction/OXidation (REDOX) state of the glass from the Defense Waste Processingmore » Facility (DWPF) melter. This report summarizes the initial work on these correlations based on the aforementioned data. Further refinement of the models as additional data is collected is recommended.« less

Vadose zone flow convergence test suite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Butcher, B. T.

Performance Assessment (PA) simulations for engineered disposal systems at the Savannah River Site involve highly contrasting materials and moisture conditions at and near saturation. These conditions cause severe convergence difficulties that typically result in unacceptable convergence or long simulation times or excessive analyst effort. Adequate convergence is usually achieved in a trial-anderror manner by applying under-relaxation to the Saturation or Pressure variable, in a series of everdecreasing RELAxation values. SRNL would like a more efficient scheme implemented inside PORFLOW to achieve flow convergence in a more reliable and efficient manner. To this end, a suite of test problems that illustratemore » these convergence problems is provided to facilitate diagnosis and development of an improved convergence strategy. The attached files are being transmitted to you describing the test problem and proposed resolution.« less

TYPE A FISSILE PACKAGING FOR AIR TRANSPORT PROJECT OVERVIEW

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eberl, K.; Blanton, P.

2013-10-11

This paper presents the project status of the Model 9980, a new Type A fissile packaging for use in air transport. The Savannah River National Laboratory (SRNL) developed this new packaging to be a light weight (<150-lb), drum-style package and prepared a Safety Analysis for Packaging (SARP) for submission to the DOE/EM. The package design incorporates unique features and engineered materials specifically designed to minimize packaging weight and to be in compliance with 10CFR71 requirements. Prototypes were fabricated and tested to evaluate the design when subjected to Normal Conditions of Transport (NCT) and Hypothetical Accident Conditions (HAC). An overview ofmore » the design details, results of the regulatory testing, and lessons learned from the prototype fabrication for the 9980 will be presented.« less

DEVELOPMENT OF A LAMINATED DISK FOR THE SPIN TEK ROTARY MICROFILTER

DOE Office of Scientific and Technical Information (OSTI.GOV)

Herman, D.

2011-06-03

Funded by the Department of Energy Office of Environmental Management, EM-31, the Savannah River National Laboratory (SRNL) partnered with SpinTek Filtration{trademark} to develop a filter disk that would withstand a reverse pressure or flow during operation of the rotary microfilter. The ability to withstand a reverse pressure and flow eliminates a potential accident scenario that could have resulted in damage to the filter membranes. While the original welded filter disks have been shown to withstand and reverse pressure/flow in the static condition, the filter disk design discussed in this report will allow a reverse pressure/flow while the disks are rotating.more » In addition, the laminated disk increases the flexibility during filter startup and cleaning operations. The new filter disk developed by SRNL and SpinTek is manufactured with a more open structure significantly reducing internal flow restrictions in the disk. The prototype was tested at the University of Maryland and demonstrated to withstand the reverse pressure due to the centrifugal action of the rotary filter. The tested water flux of the disk was demonstrated to be 1.34 gpm in a single disk test. By comparison, the water flux of the current disk was 0.49 gpm per disk during a 25 disk test. The disk also demonstrated rejection of solids by filtering a 5 wt % Strontium Carbonate slurry with a filtrate clarity of less the 1.4 Nephelometric Turbidity Units (NTU) throughout the two hour test. The Savannah River National Laboratory (SRNL) has been working with SpinTek Filtration{trademark} to adapt the rotary microfilter for radioactive service in the Department of Energy (DOE) Complex. One potential weakness is the loose nature of the membrane on the filter disks. The current disk is constructed by welding the membrane at the outer edge of the disk. The seal for the center of the membrane is accomplished by an o-ring in compression for the assembled stack. The remainder of the membrane is free floating on the disk. This construction requires that a positive pressure be applied to the rotary filter tank to prevent the membrane from rising from the disk structure and potentially contacting the filter turbulence promoter. In addition, one accident scenario is a reverse flow through the filtrate line due to mis-alignment of valves resulting in the membrane rising from the disk structure. The structural integrity of the current disk has been investigated, and shown that the disk can withstand a significant reverse pressure in a static condition. However, the disk will likely incur damage if the filter stack is rotated during a reverse pressure. The development of a laminated disk would have several significant benefits for the operation of the rotary filter including the prevention of a compromise in filter disk integrity during a reverse flow accident, increasing operational flexibility, and increasing the self cleaning ability of the filter. A laminated disk would allow the filter rotor operation prior to a positive pressure in the filter tank. This would prevent the initial dead-head of the filter and prevent the resulting initial filter cake buildup. The laminated disk would allow rotor operation with cleaning fluid, eliminating the need for a recirculation pump. Additionally, a laminated disk would allow a reverse flow of fluid through the membrane pores removing trapped particles.« less

Yield Stress Reduction of DWPF Melter Feed Slurries

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stone, M.E.; Smith, M.E.

2007-07-01

The Defense Waste Processing Facility (DWPF) at the Savannah River Site vitrifies High Level Waste for repository internment. The process consists of three major steps: waste pretreatment, vitrification, and canister decontamination/sealing. The HLW consists of insoluble metal hydroxides and soluble sodium salts. The pretreatment process acidifies the sludge with nitric and formic acids, adds the glass formers as glass frit, then concentrates the resulting slurry to approximately 50 weight percent (wt%) total solids. This slurry is fed to the joule-heated melter where the remaining water is evaporated followed by calcination of the solids and conversion to glass. The Savannah Rivermore » National Laboratory (SRNL) is currently assisting DWPF efforts to increase throughput of the melter. As part of this effort, SRNL has investigated methods to increase the solids content of the melter feed to reduce the heat load required to complete the evaporation of water and allow more of the energy available to calcine and vitrify the waste. The process equipment in the facility is fixed and cannot process materials with high yield stresses, therefore increasing the solids content will require that the yield stress of the melter feed slurries be reduced. Changing the glass former added during pretreatment from an irregularly shaped glass frit to nearly spherical beads was evaluated. The evaluation required a systems approach which included evaluations of the effectiveness of beads in reducing the melter feed yield stress as well as evaluations of the processing impacts of changing the frit morphology. Processing impacts of beads include changing the settling rate of the glass former (which effects mixing and sampling of the melter feed slurry and the frit addition equipment) as well as impacts on the melt behavior due to decreased surface area of the beads versus frit. Beads were produced from the DWPF process frit by fire polishing. The frit was allowed to free fall through a flame, then quenched with a water spray. Approximately 90% of the frit was converted to beads by this process. Yield stress reduction was measured by preparing melter feed slurries (using nonradioactive HLW simulants) that contain beads and comparing the yield stress with melter feed containing frit. A second set of tests was performed with beads of various diameters to determine if a decrease in diameter affected the results. Smaller particle size was shown to increase yield stress when frit is utilized. The settling rate of the beads was required to match the settling rate of the frit, therefore a decrease in particle size was anticipated. Settling tests were conducted in water, xanthan gum solutions, and in non-radioactive simulants of the HLW. The tests used time-lapse video-graphy as well as solids sampling to evaluate the settling characteristics of beads compared to frit of the same particle size. A preliminary melt rate evaluation was performed using a dry-fed Melt Rate Furnace (MRF) developed by SRNL. Preliminary evaluation of the impact of beading the frit on the frit addition system were completed by conducting flow loop testing. A recirculation loop was built with a total length of about 30 feet. Pump power, flow rate, outlet pressure, and observations of the flow in the horizontal upper section of the loop were noted. The recirculation flow was then gradually reduced and the above items recorded until settling was noted in the recirculation line. Overall, the data shows that the line pressure increased as the solids were increased for the same flow rate. In addition, the line pressure was higher for Frit 320 than the beads at the same solids level and flow. With the observations, a determination of minimum velocity to prevent settling could be done, but a graph of the line pressures versus velocity for the various tests was deemed to more objective. The graph shows that the inflection point in pressure drop is about the same for the beads and Frit 320. This indicates that the bead slurry would not require higher flows rates than frit slurry at DWPF during transfers. Another key finding was that the pump impeller was not significantly damaged by the bead slurry, while the Frit 320 slurry rapidly destroyed the impeller. Evidence of this was first observed when black particles were seen in the Frit 320 slurry being recirculated and then confirmed by a post-test inspection of the impeller. Finally, the pumping of bead slurry could be recovered even if flow is stopped. The Frit 320 slurry could not be restarted after stopping flow due to the nature of the frit to pack tightly when settled. Beads were shown to represent a significant process improvement versus frit for the DWPF process in lowering yield stress of the melter feed. Lower erosion of process equipment is another expected benefit.« less

Aging Behavior of the EPDM O-Rings in the H1616 Shipping Package

DOE Office of Scientific and Technical Information (OSTI.GOV)

Daugherty, W.; Stefek, T.; Skidmore, E.

The H1616 shipping package is used within the DOE complex for shipping tritium reservoirs. The annual recertification frequency can create logistical difficulties with other constraints on the timing of shipments; thus, a longer re-certification period is desirable. The ethylene propylene diene monomer (EPDM) O-rings used in the H1616 shipping package are being aged and tested at the Savannah River National Laboratory (SRNL) to provide a technical basis for extending the annual maintenance of the H1616 shipping package. H1616 EPDM O-rings are being aged at elevated temperature, and tested for degradation in mechanical properties, compression stress relaxation (CSR) behavior, and leakmore » performance. Mechanical properties of aged O-rings show significant degradation can occur, but an inert atmosphere (argon backfill) greatly reduces the rate of degradation. The CSR behavior of O-rings was evaluated in air at 79 to 177 °C. These collective data were used to develop a predictive model for extrapolation of CSR behavior to relevant service temperatures (<67 °C). O-rings were also aged in H1616 Containment Vessels (CV) in an inert atmosphere at 71 to 149 °C. The vessels are helium leak tested periodically to determine if they continue to remain leak-tight. The vessel tests provide a solid demonstration that the H1616 O-rings will remain leak-tight at temperatures up to 113 °C for up to approximately 2.3 years. Significantly longer periods of leak-tight service are expected at the lower temperatures actually experienced in service. The predictive model developed from the CSR data conservatively indicates a service life of ~5 years at 67 °C. Although the relationship between CSR behavior and leak-tight performance has not been established for this design, the CSR predictions for this O-ring are conservative relative to leak-tight performance. Based on the collective data developed to date, SRNL has recommended that the maintenance interval for the H1616 package be extended from 1 year to 2 years. Future recommendations in support of even longer maintenance intervals are expected, as additional aging data become available.« less

PERFORMANCE IMPROVEMENT OF CROSS-FLOW FILTRATION FOR HIGH LEVEL WASTE TREATMENT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Duignan, M.; Nash, C.; Poirier, M.

2011-01-12

In the interest of accelerating waste treatment processing, the DOE has funded studies to better understand filtration with the goal of improving filter fluxes in existing cross-flow equipment. The Savannah River National Laboratory (SRNL) was included in those studies, with a focus on start-up techniques, filter cake development, the application of filter aids (cake forming solid precoats), and body feeds (flux enhancing polymers). This paper discusses the progress of those filter studies. Cross-flow filtration is a key process step in many operating and planned waste treatment facilities to separate undissolved solids from supernate slurries. This separation technology generally has themore » advantage of self-cleaning through the action of wall shear stress created by the flow of waste slurry through the filter tubes. However, the ability of filter wall self-cleaning depends on the slurry being filtered. Many of the alkaline radioactive wastes are extremely challenging to filtration, e.g., those containing compounds of aluminum and iron, which have particles whose size and morphology reduce permeability. Unfortunately, low filter flux can be a bottleneck in waste processing facilities such as the Savannah River Modular Caustic Side Solvent Extraction Unit and the Hanford Waste Treatment Plant. Any improvement to the filtration rate would lead directly to increased throughput of the entire process. To date increased rates are generally realized by either increasing the cross-flow filter axial flowrate, limited by pump capacity, or by increasing filter surface area, limited by space and increasing the required pump load. SRNL set up both dead-end and cross-flow filter tests to better understand filter performance based on filter media structure, flow conditions, filter cleaning, and several different types of filter aids and body feeds. Using non-radioactive simulated wastes, both chemically and physically similar to the actual radioactive wastes, the authors performed several tests to demonstrate increases in filter performance. With the proper use of filter flow conditions and filter enhancers, filter flow rates can be increased over rates currently realized today.« less

Update to agency for toxic substances and disease registry 2012 report on assessment of biota exposure to mercury originating from Savannah River Site.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kuhne, W.

The purpose of this report is to 1) update previous Savannah River National Laboratory (SRNL) assessment reports (Kvartek et al. 1994 and Halverson et al. 2008) on the fate of mercury in the Savannah River Site (SRS) environment and 2) address comments and recommendations from the review of SRS by the Agency for Toxic Substances and Disease Registry (ATSDR) concerning the evaluation of exposures to contaminants in biota originating from the SRS. The ATSDR reviewed and evaluated data from SRS, South Carolina Department of Health & Environmental Control (SCDHEC) and the Georgia Department of Natural Resources (GDNR) concerning the non-radioactivemore » contaminant mercury. This report will provide a response and update to conclusions and recommendations made by the ATSDR.« less

Examination of Shipping Packages 9975-02694 and 9975-02729

DOE Office of Scientific and Technical Information (OSTI.GOV)

Daugherty, W.

SRNL has assisted in the examination of two 9975 shipping packages (9975-02694 and 9975-02729) following their use for storage of nuclear material in K-Area Complex (KAC). Both of these were targeted for examination because they were exposed to water from a leaking expansion joint during storage. When first opened in KAC, the axial gap was found to be in excess of the 1 inch maximum criterion, signaling the potential for degradation of the fiberboard overpack and drum. Within each package the highest fiberboard moisture levels were observed in the bottom layers, but no mold was observed in either package. Themore » fiberboard in each package appeared to retain good integrity consistent with non-degraded material. Minor corrosion was also observed on these drums along the lower stitch welds and on several closure bolts.« less

Examination of shipping packages 9975-01658, 9975-02075 and 9975-02738

DOE Office of Scientific and Technical Information (OSTI.GOV)

Daugherty, W. L.

SRNL has assisted in the examination of three 9975 shipping packages (9975-01658, 9975-02075 and 9975-02738) following their use for storage of nuclear material in K-Area Complex (KAC). Each of these was targeted for examination because the axial gap exceeded the 1 inch maximum criterion, signaling the potential for degradation of the fiberboard overpack and drum. Each package experienced a degree of compaction of the bottom fiberboard layers, and had elevated moisture levels toward the bottom. A small amount of mold was observed on the lower fiberboard assembly in 9975-02738. However, the majority of the fiberboard in each package appeared tomore » retain good integrity consistent with non-degraded material. Minor corrosion was observed on these drums, but is judged to have not compromised the drum integrity.« less

MIXING STUDY FOR JT-71/72 TANKS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, S.

2013-11-26

All modeling calculations for the mixing operations of miscible fluids contained in HBLine tanks, JT-71/72, were performed by taking a three-dimensional Computational Fluid Dynamics (CFD) approach. The CFD modeling results were benchmarked against the literature results and the previous SRNL test results to validate the model. Final performance calculations were performed by using the validated model to quantify the mixing time for the HB-Line tanks. The mixing study results for the JT-71/72 tanks show that, for the cases modeled, the mixing time required for blending of the tank contents is no more than 35 minutes, which is well below 2.5more » hours of recirculation pump operation. Therefore, the results demonstrate the adequacy of 2.5 hours’ mixing time of the tank contents by one recirculation pump to get well mixed.« less

EVALUATION OF THE DURABILITY OF THE STRUCTURAL CONCRETE OF REACTOR BUILDINGS AT SRS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Duncan, A.; Reigel, M.

2011-02-28

The Department of Energy (DOE) intends to close 100-150 facilities in the DOE complex using an in situ decommissioning (ISD) strategy that calls for grouting the below-grade interior volume of the structure and leaving the above-grade interior open or demolishing it and disposing of it in the slit trenches in E Area. These closures are expected to persist and remain stable for centuries, but there are neither facility-specific monitoring approaches nor studies on the rate of deterioration of the materials used in the original construction or on the ISD components added during closure (caps, sloped roofs, etc). This report willmore » focus on the evaluation of the actual aging/degradation of the materials of construction used in the ISD structures at Savannah River Site (SRS) above grade, specifically P & R reactor buildings. Concrete blocks (six 2 to 5 ton blocks) removed from the outer wall of the P Reactor Building were turned over to SRNL as the first source for concrete cores. Larger cores were received as a result of grouting activities in P and R reactor facilities. The cores were sectioned and evaluated using microscopy, x-ray diffraction (XRD), ion chromatography (IC) and thermal analysis. Scanning electron microscopy shows that the aggregate and cement phases present in the concrete are consistent with the mix design and no degradation mechanisms are evident at the aggregate-cement interfaces. Samples of the cores were digested and analyzed for chloride ingress as well as sulfate attack. The concentrations of chloride and sulfate ions did not exceed the limits of the mix design and there is no indication of any degradation due to these mechanisms. Thermal analysis on samples taken along the longitudinal axis of the cores show that there is a 1 inch carbonation layer (i.e., no portlandite) present in the interior wall of the reactor building and a negligible carbonation layer in the exterior wall. A mixed layer of carbonate and portlandite extends deeper into the interior (2-3 inches) and exterior (1-2 inches) walls. This is more extensive than measured in previous SRS structures. Once the completely carbonated layer reaches the rebar that is approximately 2-3 inches into the concrete wall, the steel is susceptible to corrosion. The growth rate of the carbonated layer was estimated from current observations and previous studies. Based on the estimated carbonation rate, the steel rebar should be protected from carbonation induced corrosion for at least another 100 years. If degradation of these structures is dominated by the carbonation mechanism, the length of time before water intrusion is expected into the process room of P-reactor is estimated to be between 425-675 years.« less

EFFECTS OF GAMMA IRRADIATION ON EPDM ELASTOMERS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Clark, E.

Two formulations of EPDM elastomer, one substituting a UV stabilizer for the normal antioxidant in this polymer, and the other the normal formulation, were synthesized and samples of each were exposed to gamma irradiation in initially pure deuterium gas to compare their radiation stability. Stainless steel containers having rupture disks were designed for this task. After 130 MRad dose of cobalt-60 radiation in the SRNL Gamma Irradiation Facility, a significant amount of gas was created by radiolysis; however the composition indicated by mass spectroscopy indicated an unexpected increase in the total amount deuterium in both formulations. The irradiated samples retainedmore » their ductility in a bend test. No change of sample weight, dimensions, or density was observed. No change of the glass transition temperature as measured by dynamic mechanical analysis was observed, and most of the other dynamic mechanical properties remained unchanged. There appeared to be an increase in the storage modulus of the irradiated samples containing the UV stabilizer above the glass transition, which may indicate hardening of the material by radiation damage. Polymeric materials become damaged by exposure over time to ionizing radiation. Despite the limited lifetime, polymers have unique engineering material properties and polymers continue to be used in tritium handling systems. In tritium handling systems, polymers are employed mainly in joining applications such as valve sealing surfaces (eg. Stem tips, valve packing, and O-rings). Because of the continued need to employ polymers in tritium systems, over the past several years, programs at the Savannah River National Laboratory have been studying the effect of tritium on various polymers of interest. In these studies, samples of materials of interest to the SRS Tritium Facilities (ultra-high molecular weight polyethylene (UHMW-PE), polytetrafluoroethylene (PTFE, Teflon{reg_sign}), Vespel{reg_sign} polyimide, and the elastomer ethylene propylene diene monomer (EPDM)) have been exposed in closed containers to tritium gas initially at 1 atmosphere pressure. These studies have demonstrated the degradation of properties when exposed to tritium gas. Also, the radiolytic production of significant amounts of hydrogen has been observed for UHMW-PE and EPDM. The study documented in this report exposes two similar formulations of EPDM elastomer to gamma irradiation in a closed container backfilled with deuterium. Deuterium is chemically identical to protium and tritium, but allows the identification of protium that is radiolytically produced from the samples. The goal of this program is to compare and contrast the response of EPDM exposure to two different types of ionizing radiation in a similar chemical environment.« less

TANKS 18 AND 19-F STRUCTURAL FLOWABLE GROUT FILL MATERIAL EVALUATION AND RECOMMENDATIONS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stefanko, D.; Langton, C.

2011-11-01

Cementitious grout will be used to close Tanks 18-F and 19-F. The functions of the grout are to: (1) physically stabilize the final landfill by filling the empty volume in the tanks with a non compressible material; (2) provide a barrier for inadvertent intrusion into the tank; (3) reduce contaminant mobility by (a) limiting the hydraulic conductivity of the closed tank and (b) reducing contact between the residual waste and infiltrating water; and (4) providing an alkaline, chemically reducing environment in the closed tank to control speciation and solubility of selected radionuclides. The objective of this work was to identifymore » a single (all-in-one) grout to stabilize and isolate the residual radionuclides in the tank, provide structural stability of the closed tank and serve as an inadvertent intruder barrier. This work was requested by V. A. Chander, High Level Waste (HLW) Tank Engineering, in HLW-TTR-2011-008. The complete task scope is provided in the Task Technical and QA Plan, SRNL-RP-2011-00587 Revision 0. The specific objectives of this task were to: (1) Identify new admixtures and dosages for formulating a zero bleed flowable tank fill material selected by HLW Tank Closure Project personnel based on earlier tank fill studies performed in 2007. The chemical admixtures used for adjusting the flow properties needed to be updated because the original admixture products are no longer available. Also, the sources of cement and fly ash have changed, and Portland cements currently available contain up to 5 wt. % limestone (calcium carbonate). (2) Prepare and evaluate the placement, compressive strength, and thermal properties of the selected formulation with new admixture dosages. (3) Identify opportunities for improving the mix selected by HLW Closure Project personnel and prepare and evaluate two potentially improved zero bleed flowable fill design concepts; one based on the reactor fill grout and the other based on a shrinkage compensating flowable fill mix design. (4) Prepare samples for hydraulic property measurements for comparison to the values in the F and H- Tank Farm Performance Assessments (PAs). (5) Identify a grout mix for the Tanks 18-F and 19-F Grout Procurement Specification [Forty, 2011 a, b, c]. Results for two flowable zero bleed structural fill concepts containing 3/8 inch gravel (70070 Series and LP-8 Series) and a sand only mix (SO Series) are provided in this report. Tank Farm Engineering and SRNL Project Management selected the 70070 mix as the base case for inclusion in Revision 0 of the Tanks 18-F and 19-F grout procurement specification [Forty 2011 a] and requested admixture recommendations and property confirmation for this formulation [Forty, 2011 b]. Lower cementitious paste mixes were formulated because the 70070 mix is over designed with respect to strength and generates more heat from hydration reactions than is desirable for mass pour application. Work was also initiated on a modification of the recommended mix which included shrinkage compensation to mitigate fast pathways caused by shrinkage cracking and poor physical bonding to the tank and ancillary equipment. Testing of this option was postponed to FY12.« less

Fuel Cycle Research & Development Technical Monthly-March 2012

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miller, Michael C.

2012-05-10

Several MPACT BCPs were executed in February, reflecting the shift in MPACT priorities directed late last year. Work continued on the FY2014 IPL, also bringing it in line with the new priorities. Preparations were made for the March MPACT Working Group meeting, in conjunction with Savannah River which is hosting the meeting. Steps were taken to initiate a new project with the World Institute for Nuclear Security, including discussions with WINS staff and preliminary work on the required procurement documentation. Several hardware issues were worked through. The newest detector array is working at LANL. A thorough analysis of previously collectedmore » Pu sample data using recently developed analysis code with improved spectral energy calibrations was completed. We now have a significantly better understanding of measurement uncertainties. Post-test analyses of the salt and sensor material for the first sensor test are almost complete. Sensor testing with different arrangements will continue and will be oriented based on post-test analysis of the first sensor test. Sensor materials for the next couple of tests are being fabricated. Materials with different annealing temperatures are being prepared for analysis. Fast Neutron Imaging to Quantify Nuclear Materials - The imager detectors repairs are complete and work with the imager is under way. The milestone requiring a report on LANSCE experiments was completed and submitted. Analysis of previous experiments and comparisons to simulations is near complete. Results are being compared with previous LANSCE-LSDS and RPI results. Additional data library (TENDL) is also being checked to see whether there are differences in the simulation results. The mid-year MIP Monitor project accomplishments and progress was presented at the MPACT meeting held in March at SRNL. Discussions around the meeting included inquiries into the feasibility of collecting process measurement data at H-Canyon, and it was explored further after the meeting. Kenneth Dayman, the graduate student from University of Texas, completed an initial draft of his master's thesis. His research will contribute to the multivariate classifier currently under development. Sarah Bender, the graduate student from Pennsylvania State University, presented her work on a poster and in a conference paper at the MARC IX meeting. A mass balance flowsheet for the fast reactor fuel was completed and a model simulation is scheduled to begin construction next month. The development of a mass balance flowsheet for light water reactor fuel will predict the behavior of the separation process using mathematical functions. The completed flowsheet will be utilized as the basis for constructing the model simulation for the electrochemical separations. Comments and review of the model from the MPACT Working Group meeting have been used to evaluate updates to the EChem model. A preliminary physical security layout has been developed in ATLAS. Thermal stability tests for high temperature microfluidic interconnections were completed on all compounds tested for bonding strength. An interconnection strategy was determined based on these results that we expect will allow for operation at 400C in the first generation of sampling systems. Design of the sampling system using the chosen interconnections was initiated, with handoff to an external foundry for fabrication based on ANL specified process conditions expected by the middle of the month. Monte Carlo simulations of the sampling system were conducted under conditions of realistic sampling size distributions, electrorefiner inhomogeneity distributions, and detector efficiencies. These simulations were used to establish a baseline limit of detection for system operation, assuming an on-line separation step is conducted before detection. Sensor for measuring density and depth of molten electrolyte - The procurement effort continued. 80% of the components ordered to assemble the double bubbler have arrived at the INL. Pratap Sadasivan, and his team have been working on the new metrics for proliferation and security. They have defined the basic structure and method, implementation strategy, needed data, and approach to application. Initial drafting of several sections of the milestone document was started. The MPACT Working Group meeting was hosted at SRS on March 13-15, 2012. Approximately 65 researchers from national labs, industry and universities attended the technical meetings at the Center for Hydrogen Research on March 13-14 with a working lunch each day. 37 persons participated in a site tour, including H-Canyon and the MOX Facility, on March 15. As part of the WG meeting, a presentation by SRNL was given on H-Canyon history, capabilities and opportunities for its use as an MPACT technology test bed. Used fuels storage security analysis, guidance and best practices - Coordination discussions continued for the MPACT used fuel security work packages.« less

9977 TYPE B PACKAGING INTERNAL DATA COLLECTION FEASIBILITY TESTING - MAGNETIC FIELD COMMUNICATIONS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shull, D.

2012-06-18

The objective of this report is to document the findings from proof-of-concept testing performed by the Savannah River National Laboratory (SRNL) R&D Engineering and Visible Assets, Inc. for the DOE Packaging Certification Program (PCP) to determine if RuBee (IEEE 1902.1) tags and readers could be used to provide a communication link from within a drum-style DOE certified Type B radioactive materials packaging. A Model 9977 Type B Packaging was used to test the read/write capability and range performance of a RuBee tag and reader. Testing was performed with the RuBee tags placed in various locations inside the packaging including insidemore » the drum on the outside of the lid of the containment vessel and also inside of the containment vessel. This report documents the test methods and results. A path forward will also be recommended.« less

Hanford Double Shell Waste Tank Corrosion Studies - Final Report FY2015

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fuentes, R. E.; Wyrwas, R. B.

2016-05-01

During FY15, SRNL performed corrosion testing that supported Washington River Protection Solutions (WRPS) with their double shell tank (DST) integrity program. The testing investigated six concerns including, 1) the possibility of corrosion of the exterior of the secondary tank wall; 2) the effect of ammonia on vapor space corrosion (VSC) above waste simulants; 3) the determination of the minimum required nitrite and hydroxide concentrations that prevent pitting in concentrated nitrate solutions (i.e., waste buffering); 4) the susceptibility to liquid air interface (LAI) corrosion at proposed stress corrosion cracking (SCC) inhibitor concentrations; 5) the susceptibility of carbon steel to pitting inmore » dilute solutions that contain significant quantities of chloride and sulfate; and 6) the effect of different heats of A537 carbon steel on the corrosion response. For task 1, 2, and 4, the effect of heat treating and/ or welding of the materials was also investigated.« less

Development of a Nanomaterial Anode for a Low-Voltage Proportional Counter for Neutron Detection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Craps, Matthew Greg

NanoTechLabs (NTL) in collaboration with the Savannah River National Laboratory (SRNL) and Clemson University have continued development of a next generation proportional counter (PC) for neutron detection utilizing robust, inexpensive nanostructured anodes while maximizing neutron capture. Neutron detectors are vital to national security as they can be used to detect illicit trafficking of radioactive materials, which could mean the presence of or planning of a dirty bomb attack. Typical PCs operate with high bias potentials that create electronic noise. Incorporating nanomaterials into the anode of PCs can theoretically operate at low voltages (eg. 10-300V) due to an increase in themore » electric field associated with a smaller diameter nano-scale anode. In addition to the lower operating voltage, typical high PC voltages (500-1200V) could be used to generate a larger electric field resulting in more electrons being collected, thus increasing the sensitivity of the PC. Other advantages of nano-PC include reduced platform size, weight, cost, and improved ruggedness. Clemson modeled the electric field around the CNT array tips. NTL grew many ordered CNT arrays as well as control samples and densified the arrays to improve the performance. The primary objective for this work is to provide evidence of a commercially viable technique for reducing the voltage of a parallel plate proportional counter using nanosized anodes. The parallel plate geometry has advantages over the typical cylindrical design based on more feasible placement of solid neutron absorbers and more geometrically practical windows for radiation capture and directional detection.« less

Defense Waste Processing Facility Simulant Chemical Processing Cell Studies for Sludge Batch 9

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, Tara E.; Newell, J. David; Woodham, Wesley H.

The Savannah River National Laboratory (SRNL) received a technical task request from Defense Waste Processing Facility (DWPF) and Saltstone Engineering to perform simulant tests to support the qualification of Sludge Batch 9 (SB9) and to develop the flowsheet for SB9 in the DWPF. These efforts pertained to the DWPF Chemical Process Cell (CPC). CPC experiments were performed using SB9 simulant (SB9A) to qualify SB9 for sludge-only and coupled processing using the nitric-formic flowsheet in the DWPF. Two simulant batches were prepared, one representing SB8 Tank 40H and another representing SB9 Tank 51H. The simulant used for SB9 qualification testing wasmore » prepared by blending the SB8 Tank 40H and SB9 Tank 51H simulants. The blended simulant is referred to as SB9A. Eleven CPC experiments were run with an acid stoichiometry ranging between 105% and 145% of the Koopman minimum acid equation (KMA), which is equivalent to 109.7% and 151.5% of the Hsu minimum acid factor. Three runs were performed in the 1L laboratory scale setup, whereas the remainder were in the 4L laboratory scale setup. Sludge Receipt and Adjustment Tank (SRAT) and Slurry Mix Evaporator (SME) cycles were performed on nine of the eleven. The other two were SRAT cycles only. One coupled flowsheet and one extended run were performed for SRAT and SME processing. Samples of the condensate, sludge, and off-gas were taken to monitor the chemistry of the CPC experiments.« less

DEVELOPMENT OF REMOTE HANFORD CONNECTOR GASKET REPLACEMENT TOOLING FOR DWPF

DOE Office of Scientific and Technical Information (OSTI.GOV)

Krementz, D.; Coughlin, Jeffrey

2009-05-05

The Defense Waste Processing Facility (DWPF) requested the Savannah River National Laboratory (SRNL) to develop tooling and equipment to remotely replace gaskets in mechanical Hanford connectors to reduce personnel radiation exposure as compared to the current hands-on method. It is also expected that radiation levels will continually increase with future waste streams. The equipment is operated in the Remote Equipment Decontamination Cell (REDC), which is equipped with compressed air, two master-slave manipulators (MSM's) and an electro-mechanical manipulator (EMM) arm for operation of the remote tools. The REDC does not provide access to electrical power, so the equipment must be manuallymore » or pneumatically operated. The MSM's have a load limit at full extension of ten pounds, which limited the weight of the installation tool. In order to remotely replace Hanford connector gaskets several operations must be performed remotely, these include: removal of the spent gasket and retaining ring (retaining ring is also called snap ring), loading the new snap ring and gasket into the installation tool and installation of the new gasket into the Hanford connector. SRNL developed and tested tools that successfully perform all of the necessary tasks. Removal of snap rings from horizontal and vertical connectors is performed by separate air actuated retaining ring removal tools and is manipulated in the cell by the MSM. In order install a new gasket, the snap ring loader is used to load a new snap ring into a groove in the gasket installation tool. A new gasket is placed on the installation tool and retained by custom springs. An MSM lifts the installation tool and presses the mounted gasket against the connector block. Once the installation tool is in position, the gasket and snap ring are installed onto the connector by pneumatic actuation. All of the tools are located on a custom work table with a pneumatic valve station that directs compressed air to the desired tool and vents the tools as needed. Extensive testing of tooling operation was performed in the DWPF manipulator repair shop. This testing allowed the operators to gain confidence before the equipment was exposed to radioactive contamination. The testing also led to multiple design improvements. On July 17 and 29, 2008 the Remote Gasket Replacement Tooling was successfully demonstrated in the REDC at the DWPF of The Savannah River Site.« less

Nucleation and crystal growth behavior of nepheline in simulated high-level waste glasses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fox, K.; Amoroso, J.; Mcclane, D.

The Savannah River National Laboratory (SRNL) has been tasked with supporting glass formulation development and process control strategies in key technical areas, relevant to the Department of Energy’s Office of River Protection (DOE-ORP) and related to high-level waste (HLW) vitrification at the Waste Treatment and Immobilization Plant (WTP). Of specific interest is the development of predictive models for crystallization of nepheline (NaAlSiO4) in HLW glasses formulated at high alumina concentrations. This report summarizes recent progress by researchers at SRNL towards developing a predicative tool for quantifying nepheline crystallization in HLW glass canisters using laboratory experiments. In this work, differential scanningmore » calorimetry (DSC) was used to obtain the temperature regions over which nucleation and growth of nepheline occur in three simulated HLW glasses - two glasses representative of WTP projections and one glass representative of the Defense Waste Processing Facility (DWPF) product. The DWPF glass, which has been studied previously, was chosen as a reference composition and for comparison purposes. Complementary quantitative X-ray diffraction (XRD) and optical microscopy confirmed the validity of the methodology to determine nucleation and growth behavior as a function of temperature. The nepheline crystallization growth region was determined to generally extend from ~ 500 to >850 °C, with the maximum growth rates occurring between 600 and 700 °C. For select WTP glass compositions (high Al2O3 and B2O3), the nucleation range extended from ~ 450 to 600 °C, with the maximum nucleation rates occurring at ~ 530 °C. For the DWPF glass composition, the nucleation range extended from ~ 450 to 750 °C with the maximum nucleation rate occurring at ~ 640 °C. The nepheline growth at the peak temperature, as determined by XRD, was between 35 - 75 wt.% /hour. A maximum nepheline growth rate of ~ 0.1 mm/hour at 700 °C was measured for the DWPF composition using optical microscopy. This research establishes a viable alternative to more traditional techniques for evaluating nepheline crystallization in large numbers of glasses, which are prohibitively time consuming or otherwise impractical. The ultimate objective is to combine the nucleation and growth information obtained from DSC, like that presented in this report, with computer simulations of glass cooling within the canister to accurately predict nepheline crystallization in HLW during processing through WTP.« less

CROSSFLOW FILTRATON: LITERATURE REVIEW

DOE Office of Scientific and Technical Information (OSTI.GOV)

Duignan, M.

2011-01-01

As part of the Filtration task EM-31, WP-2.3.6, which is a joint effort between Savannah River National Laboratory (SRNL) and the Pacific Northwest National Laboratory (PNNL), tests were planned to evaluate crossflow filtration in order to the improve the use of existing hardware in the waste treatment plants at both the Department of Energy (DOE) Savannah River Site (SRS) and Hanford Site. These tests included experiments to try different operating conditions and additives, such as filter aids, in order to create a more permeable filter cake and improve the permeate flux. To plan the SRNL tests a literature review wasmore » performed to provide information on previous experiments performed by DOE laboratories, and by academia. This report compliments PNNL report (Daniel, et al 2010), and is an attempt to try and capture crossflow filtration work performed in the past that provide a basis for future testing. However, not all sources on crossflow filtration could be reviewed due to the shear volume of information available. In this report various references were examined and a representative group was chosen to present the major factors that affect crossflow filtration. The information summarized in this review contains previous operating conditions studied and their influence on the rate of filtration. Besides operating conditions, other attempted improvements include the use of filter aids, a pre-filtration leaching process, the backpulse system, and various types of filter tubes and filter coatings. The results from past research can be used as a starting point for further experimentation that can result in the improvement in the performance of the crossflow filtration. The literature reviewed in this report indicates how complex the crossflow issues are with the results of some studies appearing to conflict results from other studies. This complexity implies that filtration of mobilized stored waste cannot be explained in a simple generic sense; meaning an empirical model develop from one waste-filter combination will more than likely not be applicable to another combination. It appears that filtration performance varies as wide as the range of the types of slurry wastes that exist. However, conclusions can be elicited from existing information so that filter performance can be better understood, and hopefully improved. Those conclusions and recommendations for the planned tests are listed.« less

Results Of Copper Catalyzed Peroxide Oxidation (CCPO) Of Tank 48H Simulants

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T. B.; Pareizs, J. M.; Newell, J. D.

2012-12-13

Savannah River National Laboratory (SRNL) performed a series of laboratory-scale experiments that examined copper-catalyzed hydrogen peroxide (H{sub 2}O{sub 2}) aided destruction of organic components, most notably tetraphenylborate (TPB), in Tank 48H simulant slurries. The experiments were designed with an expectation of conducting the process within existing vessels of Building 241-96H with minimal modifications to the existing equipment. Results of the experiments indicate that TPB destruction levels exceeding 99.9% are achievable, dependent on the reaction conditions. A lower reaction pH provides faster reaction rates (pH 7 > pH 9 > pH 11); however, pH 9 reactions provide the least quantity ofmore » organic residual compounds within the limits of species analyzed. Higher temperatures lead to faster reaction rates and smaller quantities of organic residual compounds. A processing temperature of 50°C as part of an overall set of conditions appears to provide a viable TPB destruction time on the order of 4 days. Higher concentrations of the copper catalyst provide faster reaction rates, but the highest copper concentration (500 mg/L) also resulted in the second highest quantity of organic residual compounds. The data in this report suggests 100-250 mg/L as a minimum. Faster rates of H{sub 2}O{sub 2} addition lead to faster reaction rates and lower quantities of organic residual compounds. An addition rate of 0.4 mL/hour, scaled to the full vessel, is suggested for the process. SRNL recommends that for pH adjustment, an acid addition rate 42 mL/hour, scaled to the full vessel, is used. This is the same addition rate used in the testing. Even though the TPB and phenylborates can be destroyed in a relative short time period, the residual organics will take longer to degrade to <10 mg/L. Low level leaching on titanium occurred, however, the typical concentrations of released titanium are very low (~40 mg/L or less). A small amount of leaching under these conditions is not surprising and is consistent with a previous study. Acidification with phosphoric and formic acids, in lieu of nitric acid, provides benefits in reducing the amount of benzene emitted over the lifetime of a reaction. Analyses of the post-reaction residual material indicate that slurry initially adjusted down to a pH 7 produced a greater degree of energetic material than material initially adjusted to a pH of 9. No more than 140 {micro}g/m{sup 3} of mercury was indicated in reactor head spaces at any time. An estimation of less than 1% of the initial mercury was vaporized in each experiment. A limited number of replicate tests were performed to determine experimental reproducibility. These tests indicate a reasonable degree of reproducibility. The conclusion of the simulant testing has provided a set of reaction conditions that can destroy the TPB and phenylborates quickly. While longer times will be required to degrade the residual organics, the reactions appear to perform in a consistent manner. A real waste test or tests are recommended and further investigation into the use of phosphoric or formic acid is warranted.« less

SOLVENT HOLD TANK SAMPLE RESULTS FOR MCU-11-1452, MCU-11-1453, MCU-11-1454, MCU-11-1455, MCU-11-1456 AND MCU-11-1457

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peters, T.; Fondeur, F.; Fink, S.

Solvent Hold Tank (SHT) samples are sent to Savannah River National Laboratory (SRNL) to examine solvent composition changes over time. On December 5, 2011, Operations personnel delivered six samples from the SHT (MCU-11-1452 through -1457) for analysis. These samples are intended to verify that the solvent is within the specified composition range. The results from the analyses are presented in this document. Samples were received in p-nut vials containing {approx}10 mL each. Once taken into the Shielded Cells, the samples were combined. Samples were removed for analysis by density, semi-volatile organic analysis (SVOA), high performance liquid chromatography (HPLC), and Fourier-Transformmore » Infra-Red spectroscopy (FTIR). Details for the work are contained in a controlled laboratory notebook. Each of the six p-nut vials contained a single phase, with no apparent solids contamination or cloudiness. Table 1 contains the results of the analyses for the combined samples. A duplicate density measurement of the organic phase gave a result of 0.844 g/mL (1.2% residual standard deviation - RSD). Using the density as a starting point, we know that the Isopar{reg_sign} L should be slightly higher than nominal and the other components should be slightly lower than nominal. The results as a whole are internally consistent. All measurements indicate Isopar{reg_sign} L higher than nominal, and Modifier lower than nominal. The extractant result is higher than expected - given the other results, the extractant concentration should be under nominal values. Using the measured density as well as the Isopar{reg_sign} L and Modifier concentrations from the FTIR results, we calculate an extractant concentration of 6888 mg/L. This value is outside the analytical uncertainty of the reported HPLC value. Given the other results, this most likely indicates that the HPLC extractant result was biased high. When compared to the MCU density target of 0.845 g/mL, there is no need to add an Isopar{reg_sign} L trim. However, it is advisable to add sufficient trioctylamine (TOA) to return the solvent composition to within specifications as that component has declined to about 64% the concentration since the last analysis. The TOA measurement was performed twice, so the result is not an analytical aberration. TOA has not been added to the system since the previous quarterly sample in October 2011. As with the previous solvent sample results, these analyses indicate that the solvent does not require Isopar{reg_sign} L trimming at this time. However, addition of TOA is warranted. These findings indicate that the new protocols for solvent monitoring and control are yielding favorable results. Nevertheless, the deviation in the TOA concentration since the last analysis indicates continued periodic (i.e., quarterly) monitoring is recommended.« less

Enhanced monitor system for water protection

DOEpatents

Hill, David E [Knoxville, TN; Rodriquez, Jr., Miguel [Oak Ridge, TN; Greenbaum, Elias [Knoxville, TN

2009-09-22

An automatic, self-contained device for detecting toxic agents in a water supply includes an analyzer for detecting at least one toxic agent in a water sample, introducing a means for introducing a water sample into the analyzer and discharging the water sample from the analyzer, holding means for holding a water sample for a pre-selected period of time before the water sample is introduced into the analyzer, and an electronics package that analyzes raw data from the analyzer and emits a signal indicating the presence of at least one toxic agent in the water sample.

Tanks 18 And 19-F Structural Flowable Grout Fill Material Evaluation And Recommendations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Langton, C. A.; Stefanko, D. B.

2013-04-23

Cementitious grout will be used to close Tanks 18-F and 19-F. The functions of the grout are to: 1) physically stabilize the final landfill by filling the empty volume in the tanks with a non-compressible material; 2) provide a barrier for inadvertent intrusion into the tank; 3) reduce contaminant mobility by a) limiting the hydraulic conductivity of the closed tank and b) reducing contact between the residual waste and infiltrating water; and 4) providing an alkaline, chemically reducing environment in the closed tank to control speciation and solubility of selected radionuclides. The objective of this work was to identify amore » single (all-in-one) grout to stabilize and isolate the residual radionuclides in the tank, provide structural stability of the closed tank and serve as an inadvertent intruder barrier. This work was requested by V. A. Chander, High Level Waste (HLW) Tank Engineering, in HLW-TTR-2011-008. The complete task scope is provided in the Task Technical and QA Plan, SRNL-RP-2011-00587 Revision 0. The specific objectives of this task were to: 1) Identify new admixtures and dosages for formulating a zero bleed flowable tank fill material selected by HLW Tank Closure Project personnel based on earlier tank fill studies performed in 2007. The chemical admixtures used for adjusting the flow properties needed to be updated because the original admixture products are no longer available. Also, the sources of cement and fly ash have changed, and Portland cements currently available contain up to 5 wt. % limestone (calcium carbonate). 2) Prepare and evaluate the placement, compressive strength, and thermal properties of the selected formulation with new admixture dosages. 3) Identify opportunities for improving the mix selected by HLW Closure Project personnel and prepare and evaluate two potentially improved zero bleed flowable fill design concepts; one based on the reactor fill grout and the other based on a shrinkage compensating flowable fill mix design. 4) Prepare samples for hydraulic property measurements for comparison to the values in the F and H- Tank Farm Performance Assessments (PAs). 5) Identify a grout mix for the Tanks 18-F and 19-F Grout Procurement Specification [Forty, 2011 a, b, c]. Results for two flowable zero bleed structural fill concepts containing 3/8 inch gravel (70070 Series and LP#8 Series) and a sand only mix (SO Series) are provided in this report. Tank Farm Engineering and SRNL Project Management selected the 70070 mix as the base case for inclusion in Revision 0 of the Tanks 18-F and 19-F grout procurement specification [Forty 2011 a] and requested admixture recommendations and property confirmation for this formulation [Forty, 2011 b]. Lower cementitious paste mixes were formulated because the 70070 mix is over designed with respect to strength and generates more heat from hydration reactions than is desirable for mass pour application. Work was also initiated on a modification of the recommended mix which included shrinkage compensation to mitigate fast pathways caused by shrinkage cracking and poor physical bonding to the tank and ancillary equipment. Testing of this option was postponed to FY12. Mix, LP#8-16 is recommended for inclusion in the specification for furnishing and delivering tank closure grout for Tanks 18-F and 19-F [Forty, 2011 c]. A shrinkage compensating variation of this mix, LP#16C, has not been fully developed and characterized at this time.« less

Alternative High-Performance Ceramic Waste Forms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sundaram, S. K.

This final report (M5NU-12-NY-AU # 0202-0410) summarizes the results of the project titled “Alternative High-Performance Ceramic Waste Forms,” funded in FY12 by the Nuclear Energy University Program (NEUP Project # 12-3809) being led by Alfred University in collaboration with Savannah River National Laboratory (SRNL). The overall focus of the project is to advance fundamental understanding of crystalline ceramic waste forms and to demonstrate their viability as alternative waste forms to borosilicate glasses. We processed single- and multiphase hollandite waste forms based on simulated waste streams compositions provided by SRNL based on the advanced fuel cycle initiative (AFCI) aqueous separation process developed in the Fuel Cycle Research and Development (FCR&D). For multiphase simulated waste forms, oxide and carbonate precursors were mixed together via ball milling with deionized water using zirconia media in a polyethylene jar for 2 h. The slurry was dried overnight and then separated from the media. The blended powders were then subjected to melting or spark plasma sintering (SPS) processes. Microstructural evolution and phase assemblages of these samples were studied using x-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersion analysis of x-rays (EDAX), wavelength dispersive spectrometry (WDS), transmission electron spectroscopy (TEM), selective area x-ray diffraction (SAXD), and electron backscatter diffraction (EBSD). These results showed that the processing methods have significant effect on the microstructure and thus the performance of these waste forms. The Ce substitution into zirconolite and pyrochlore materials was investigated using a combination of experimental (in situ XRD and x-ray absorption near edge structure (XANES)) and modeling techniques to study these single phases independently. In zirconolite materials, a transition from the 2M to the 4M polymorph was observed with increasing Ce content. The resulting powders were consolidated via SPS. Ce was reduced to the trivalent oxidation state and the zirconolite was converted into undesirable perovskite. The zirconolite polymorphs found in the synthesized powders were recovered after a post-SPS heat treatment in air. These results demonstrated the potential of processing in controlling the phase assemblage in these waste forms. Hollandites with Cr 3+ trivalent cations were identified as potential hosts for Cs immobilization and are being investigated for Cs retention properties. Series of compositions Ba 1.15-xCs 2xCr 2.3Ti 5.7O 16, with increasing Cs loadings, were prepared by sol-gel process and characterized for structural parameters. Structural characterization was performed by a combination of powder XRD and neutron powder diffraction. Phase pure hollandite adapting monoclinic symmetry (I2/m) was observed for 0 ≤ x ≤ 0.55. These results were used to develop a new structural model to interpret Cs immobilization in these hollandites. Performance of these waste forms were evaluated for chemical durability and radiation resistance. Product consistency testing (PCT) and vapor hydration testing (VHT) were used for testing of chemical durability. Radiation resistance was tested using He + ions to simulatemore » $$\\alpha$$ particles and heavy ions such as Au 3+ to simulate a recoil. These results showed that these waste forms were chemically durable. The waste forms also amorphized to various degrees on exposure to simulated radiation.« less

Operational cooling tower model (CTTOOL V1.0)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aleman, S.; LocalDomainServers, L.; Garrett, A.

2015-01-01

Mechanical draft cooling towers (MDCT’s) are widely used to remove waste heat from industrial processes, including suspected proliferators of weapons of mass destruction (WMD). The temperature of the air being exhausted from the MDCT is proportional to the amount of thermal energy being removed from the process cooling water, although ambient weather conditions and cooling water flow rate must be known or estimated to calculate the rate of thermal energy dissipation (Q). It is theoretically possible to derive MDCT air exhaust temperatures from thermal images taken from a remote sensor. A numerical model of a MDCT is required to translatemore » the air exhaust temperature to a Q. This report describes the MDCT model developed by the Problem Centered Integrated Analysis (PCIA) program that was designed to perform those computational tasks. The PCIA program is a collaborative effort between the Savannah River National Laboratory (SRNL), the Northrop-Grumman Corporation (NG) and the Aerospace Corporation (AERO).« less

Heat of Hydration of Low Activity Cementitious Waste Forms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nasol, D.

2015-07-23

During the curing of secondary waste grout, the hydraulic materials in the dry mix react exothermally with the water in the secondary low-activity waste (LAW). The heat released, called the heat of hydration, can be measured using a TAM Air Isothermal Calorimeter. By holding temperature constant in the instrument, the heat of hydration during the curing process can be determined. This will provide information that can be used in the design of a waste solidification facility. At the Savannah River National Laboratory (SRNL), the heat of hydration and other physical properties are being collected on grout prepared using three simulantsmore » of liquid secondary waste generated at the Hanford Site. From this study it was found that both the simulant and dry mix each had an effect on the heat of hydration. It was also concluded that the higher the cement content in the dry materials mix, the greater the heat of hydration during the curing of grout.« less

2014 SRNL LDRD Annual Report, Rev. 0

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mcwhorter, S.

2015-03-15

Laboratory Directed Research and Development is a congressionally authorized program that provides the ‘innovation inspiration’ from which many of the Laboratory’s multi-discipline advancements are made in both science and engineering technology. The program is the backbone for insuring that scientific, technical and engineering capabilities can meet current and future needs. It is an important tool in reducing the probability of technological surprise by allowing laboratory technical staff room to innovate and keep abreast of scientific breakthroughs. Drawing from the synergism among the EM and NNSA missions, and work from other federal agencies ensures that LDRD is the key element inmore » maintaining the vitality of SRNL’s technical programs. The LDRD program aims to position the Laboratory for new business in clean energy, national security, nuclear materials management and environmental stewardship by leveraging the unique capabilities of the Laboratory to yield foundational scientific research in core business areas, while aligning with SRS strategic initiatives and maintaining a vision for ultimate DOE applications.« less

Mercury Dispersion Modeling And Purge Ventilation Stack Height Determination For Tank 40H

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rivera-Giboyeaux, A.

2017-05-19

The SRNL Atmospheric Technologies Group performed an analysis for mercury emissions from H-Tank Farm - Tank 40 ventilation system exhaust in order to assess whether the Short Term Exposure Limit (STEL), or Threshold Limit Value (TLV) levels for mercury will be exceeded during bulk sludge slurry mixing and sludge removal operations. The American Meteorological Society/Environmental Protection Agency Regulatory Model (AERMOD) was used as the main dispersion modelling tool for this analysis. The results indicated that a 45-foot stack is sufficient to raise the plume centerline from the Tank 40 release to prevent mercury exposure problems for any of the stackmore » discharge scenarios provided. However, a 42-foot stack at Tank 40 is sufficient to prevent mercury exposure concerns in all emission scenarios except the 50 mg/m 3 release. At a 42-foot stack height, values exceeding the exposure standards are only measured on receptors located above 34 feet.« less

Defense Waste Processing Facility Nitric- Glycolic Flowsheet Chemical Process Cell Chemistry: Part 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zamecnik, J.; Edwards, T.

The conversions of nitrite to nitrate, the destruction of glycolate, and the conversion of glycolate to formate and oxalate were modeled for the Nitric-Glycolic flowsheet using data from Chemical Process Cell (CPC) simulant runs conducted by Savannah River National Laboratory (SRNL) from 2011 to 2016. The goal of this work was to develop empirical correlation models to predict these values from measureable variables from the chemical process so that these quantities could be predicted a-priori from the sludge or simulant composition and measurable processing variables. The need for these predictions arises from the need to predict the REDuction/OXidation (REDOX) statemore » of the glass from the Defense Waste Processing Facility (DWPF) melter. This report summarizes the work on these correlations based on the aforementioned data. Previous work on these correlations was documented in a technical report covering data from 2011-2015. This current report supersedes this previous report. Further refinement of the models as additional data are collected is recommended.« less

Radioactive Demonstrations Of Fluidized Bed Steam Reforming (FBSR) With Hanford Low Activity Wastes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jantzen, C. M.; Crawford, C. L.; Burket, P. R.

Several supplemental technologies for treating and immobilizing Hanford low activity waste (LAW) are being evaluated. One immobilization technology being considered is Fluidized Bed Steam Reforming (FBSR) which offers a low temperature (700-750?C) continuous method by which wastes high in organics, nitrates, sulfates/sulfides, or other aqueous components may be processed into a crystalline ceramic (mineral) waste form. The granular waste form produced by co-processing the waste with kaolin clay has been shown to be as durable as LAW glass. The FBSR granular product will be monolithed into a final waste form. The granular component is composed of insoluble sodium aluminosilicate (NAS)more » feldspathoid minerals such as sodalite. Production of the FBSR mineral product has been demonstrated both at the industrial, engineering, pilot, and laboratory scales on simulants. Radioactive testing at SRNL commenced in late 2010 to demonstrate the technology on radioactive LAW streams which is the focus of this study.« less

Evaluations of Mechanisms for Pu Uptake and Retention within Spherical Resorcinol-Formaldehyde Resin Columns

DOE Office of Scientific and Technical Information (OSTI.GOV)

Delegard, Calvin H.; Levitskaia, Tatiana G.; Fiskum, Sandra K.

The unexpected uptake and retention of plutonium (Pu) onto columns containing spherical resorcinol-formaldehyde (sRF) resin during ion exchange testing of Cs (Cs) removal from alkaline tank waste was observed in experiments at both the Pacific Northwest National Laboratory (PNNL) and the Savannah River National Laboratory (SRNL). These observations have raised concern regarding the criticality safety of the Cs removal unit operation within the low-activity waste pretreatment system (LAWPS). Accordingly, studies have been initiated at Washington River Protection Solutions (WRPS), who manages the operations of the Hanford Site tank farms, including the LAWPS, PNNL, and elsewhere to investigate these findings. Asmore » part of these efforts, PNNL has prepared the present report to summarize the laboratory testing observations, evaluate these phenomena in light of published and unpublished technical information, and outline future laboratory testing, as deemed appropriate based on the literature studies, with the goal to elucidate the mechanisms for the observed Pu uptake and retention.« less

Simulation of Flow and Long-Term Plutonium (Pu) Transport in the Vadose Zone at the Savannah River National Laboratory (SRNL)

NASA Astrophysics Data System (ADS)

Demirkanli, I.; Molz, F. J.; Kaplan, D. I.; Fjeld, R. A.; Serkiz, S. M.

2006-05-01

An improved understanding of flow and radionuclide transport in vadose zone sediments is fundamental to all types of future planning involving radioactive materials. One way to obtain such understanding is to perform long-term experimental studies of Pu transport in complex natural systems. With this in mind, a series of field experiments were initiated at the SRNL in the early 1980s. Lysimeters containing sources of different Pu oxidation states were placed in the shallow subsurface and left open to the natural environment for 2 to 11 years. At the end of the experiments, Pu activities were measured along vertical cores obtained from the lysimeters. Pu distributions were anomalous in nature, with transport from oxidized Pu sources being less than expected, and a small fraction of Pu from reduced sources moving more. Laboratory studies with lysimeter sediments suggested that surface-mediated, oxidation/reduction (redox) reactions could be responsible for the anomalous behavior, and this hypothesis is tested by performing both steady-state and transient Pu transport simulations that include retardation along with first-order redox reactions on mineral surfaces. Based on the simulations, we conclude that the surface-mediated, redox hypothesis is consistent with the observed downward Pu activity profiles in the experiments, and such profiles are captured well by a steady-state, net downward, flow model. (Discussion is presented as to why a steady model appears to work in a highly transient flow environment.) The redox model explains how Pu(V/VI) sources release activity that moves downward more slowly than expected based on adsorptive retardation alone, and how Pu(III/IV) sources result in a small fraction of activity that moves downward more rapidly than expected. The calibrated parameter values were robust and relatively well-defined throughout all four sets of simulations. Pu(V/VI) (i.e., oxidized Pu)retardation factors were about 15, and reduced Pu(III/IV) retardation factors were about 10,000. For these values, ko (1st order oxidation rate) averaged 2.4x10-7/hr with a standard deviation of 1.6x10-7, and kr (reduction rate)was 7.1x10-4/hr with a standard deviation of 1.6x10-4. Preliminary transient flow simulations showed a very slight increase in the fitted reaction rate constants, but otherwise reproduced the steady-state results. To date, neither approach is able to simulate the observed Pu movement above the source.

PDRD (SR13046) TRITIUM PRODUCTION FINAL REPORT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, P.; Sheetz, S.

Utilizing the results of Texas A&M University (TAMU) senior design projects on tritium production in four different small modular reactors (SMR), the Savannah River National Laboratory’s (SRNL) developed an optimization model evaluating tritium production versus uranium utilization under a FY2013 plant directed research development (PDRD) project. The model is a tool that can evaluate varying scenarios and various reactor designs to maximize the production of tritium per unit of unobligated United States (US) origin uranium that is in limited supply. The primary module in the model compares the consumption of uranium for various production reactors against the base case ofmore » Watts Bar I running a nominal load of 1,696 tritium producing burnable absorber rods (TPBARs) with an average refueling of 41,000 kg low enriched uranium (LEU) on an 18 month cycle. After inputting an initial year, starting inventory of unobligated uranium and tritium production forecast, the model will compare and contrast the depletion rate of the LEU between the entered alternatives. This is an annual tritium production rate of approximately 0.059 grams of tritium per kilogram of LEU (g-T/kg-LEU). To date, the Nuclear Regulatory Commission (NRC) license has not been amended to accept a full load of TPBARs so the nominal tritium production has not yet been achieved. The alternatives currently loaded into the model include the three light water SMRs evaluated in TAMU senior projects including, mPower, Holtec and NuScale designs. Initial evaluations of tritium production in light water reactor (LWR) based SMRs using optimized loads TPBARs is on the order 0.02-0.06 grams of tritium per kilogram of LEU used. The TAMU students also chose to model tritium production in the GE-Hitachi SPRISM, a pooltype sodium fast reactor (SFR) utilizing a modified TPBAR type target. The team was unable to complete their project so no data is available. In order to include results from a fast reactor, the SRNL Technical Advisory Committee (TAC) ran a Monte Carlo N-Particle (MCNP) model of a basic SFR for comparison. A 600MWth core surrounded by a lithium blanket produced approximately 1,000 grams of tritium annually with a 13% enriched, 6 year core. This is similar results to a mid-1990’s study where the Fast Flux Test Facility (FFTF), a 400 MWth reactor at the Idaho National Laboratory (INL), could produce about 1,000 grams with an external lithium target. Normalized to the LWRs values, comparative tritium production for an SFR could be approximately 0.31 g-T/kg LEU.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Peeler, D; Tommy Edwards, T; Kevin Fox, K

The Savannah River National Laboratory (SRNL) has developed, and continues to enhance, its integrated capability to evaluate the impact of proposed sludge preparation plans on the Defense Waste Processing Facility's (DWPF's) operation. One of the components of this integrated capability focuses on frit development which identifies a viable frit or frits for each sludge option being contemplated for DWPF processing. A frit is considered viable if its composition allows for economic fabrication and if, when it is combined with the sludge option under consideration, the DWPF property/composition models (the models of DWPF's Product Composition Control System (PCCS)) indicate that themore » combination has the potential for an operating window (a waste loading (WL) interval over which the sludge/frit glass system satisfies processability and durability constraints) that would allow DWPF to meet its goals for waste loading and canister production. This report documents the results of SRNL's efforts to identify candidate frit compositions and corresponding predicted operating windows (defined in terms of WL intervals) for the February 2007 compositional projection of Sludge Batch 4 (SB4) developed by the Liquid Waste Organization (LWO). The nominal compositional projection was used to assess projected operating windows (in terms of a waste loading interval over which all predicted properties were classified as acceptable) for various frits, evaluate the applicability of the 0.6 wt% SO{sub 4}{sup =} PCCS limit to the glass systems of interest, and determine the impact (or lack thereof) to the previous SB4 variability studies. It should be mentioned that the information from this report will be coupled with assessments of melt rate to recommend a frit for SB4 processing. The results of this paper study suggest that candidate frits are available to process the nominal SB4 composition over attractive waste loadings of interest to DWPF. Specifically, two primary candidate frits for SB4 processing, Frit 510 and Frit 418, have projected operating windows that should allow for successful processing at DWPF. While Frit 418 has been utilized at DWPF, Frit 510 is a higher B{sub 2}O{sub 3} based frit which could lead to improvements in melt rate. These frits provide relatively large operating windows and demonstrate robustness to possible sludge compositional variation while avoiding potential nepheline formation issues. In addition, assessments of SO{sub 4}{sup =} solubility indicate that the 0.6 wt% SO{sub 4}{sup =} limit in PCCS is applicable for the Frit 418 and the Frit 510 based SB4 glass systems.« less

Glycolic acid physical properties and impurities assessment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lambert, D. P.; Pickenheim, B. R.; Bibler, N. E.

This document has been revised due to recent information that the glycolic acid used in Savannah River National Laboratory (SRNL) experiments contains both formaldehyde and methoxyacetic acid. These impurities were in the glycolic acid used in the testing included in this report and in subsequent testing using DuPont (now called Chemours) supplied Technical Grade 70 wt% glycolic acid. However, these impurities were not reported in earlier revisions. Additional data concerning the properties of glycolic acid have also been added to this report. The Defense Waste Processing Facility (DWPF) is planning to implement a nitric-glycolic acid flowsheets to increase attainment tomore » meet closure commitment dates during Sludge Batch 9. In fiscal year 2009, SRNL was requested to determine the physical properties of formic and glycolic acid blends. Blends of formic acid in glycolic acid were prepared and their physical properties tested. Increasing amounts of glycolic acid led to increases in blend density, viscosity and surface tension as compared to the 90 wt% formic acid that is currently used at DWPF. These increases are small, however, and are not expected to present any difficulties in terms of processing. The effect of sulfur impurities in Technical Grade glycolic acid was studied for its impact on DWPF glass quality. While the glycolic acid specification allows for more sulfate than the current formic acid specification, the ultimate impact is expected to be on the order of 0.033 wt% sulfur in glass. Note that lower sulfur content glycolic acid could likely be procured at some increased cost if deemed necessary. A paper study on the effects of radiation on glycolic acid was performed. The analysis indicates that substitution of glycolic acid for formic acid would not increase the radiolytic production rate of H2 and cause an adverse effect in the Slurry Receipt and Adjustment Tank (SRAT) or Slurry Mix Evaporator (SME) process. It has been cited that glycolic acid solutions that are depleted of O2 when subjected to large radiation doses produced considerable quantities of a non-diffusive polymeric material. Considering a constant air purge is maintained in the SRAT and the solution is continuously mixed, oxygen depletion seems unlikely, however, if this polymer is formed in the SRAT solution, the rheology of the solution may be affected and pumping of the solution may be hindered. However, an irradiation test with a simulated SRAT product supernate containing glycolic acid in an oxygen depleted atmosphere found no evidence of polymerization.« less

LAB-SCALE DEMONSTRATION OF PLUTONIUM PURIFICATION BY ANION EXCHANGE, PLUTONIUM (IV) OXALATE PRECIPITATION, AND CALCINATION TO PLUTONIUM OXIDE TO SUPPORT THE MOX FEED MISSION

DOE Office of Scientific and Technical Information (OSTI.GOV)

Crowder, M.; Pierce, R.

2012-08-22

H-Canyon and HB-Line are tasked with the production of PuO{sub 2} from a feed of plutonium metal. The PuO{sub 2} will provide feed material for the MOX Fuel Fabrication Facility. After dissolution of the Pu metal in H-Canyon, the solution will be transferred to HB-Line for purification by anion exchange. Subsequent unit operations include Pu(IV) oxalate precipitation, filtration and calcination to form PuO{sub 2}. This report details the results from SRNL anion exchange, precipitation, filtration, calcination, and characterization tests, as requested by HB-Line1 and described in the task plan. This study involved an 80-g batch of Pu and employed testmore » conditions prototypical of HB-Line conditions, wherever feasible. In addition, this study integrated lessons learned from earlier anion exchange and precipitation and calcination studies. H-Area Engineering selected direct strike Pu(IV) oxalate precipitation to produce a more dense PuO{sub 2} product than expected from Pu(III) oxalate precipitation. One benefit of the Pu(IV) approach is that it eliminates the need for reduction by ascorbic acid. The proposed HB-Line precipitation process involves a digestion time of 5 minutes after the time (44 min) required for oxalic acid addition. These were the conditions during HB-line production of neptunium oxide (NpO{sub 2}). In addition, a series of small Pu(IV) oxalate precipitation tests with different digestion times were conducted to better understand the effect of digestion time on particle size, filtration efficiency and other factors. To test the recommended process conditions, researchers performed two nearly-identical larger-scale precipitation and calcination tests. The calcined batches of PuO{sub 2} were characterized for density, specific surface area (SSA), particle size, moisture content, and impurities. Because the 3013 Standard requires that the calcination (or stabilization) process eliminate organics, characterization of PuO{sub 2} batches monitored the presence of oxalate by thermogravimetric analysis-mass spectrometry (TGA-MS). To use the TGA-MS for carbon or oxalate content, some method development will be required. However, the TGA-MS is already used for moisture measurements. Therefore, SRNL initiated method development for the TGA-MS to allow quantification of oxalate or total carbon. That work continues at this time and is not yet ready for use in this study. However, the collected test data can be reviewed later as those analysis tools are available.« less

Signal enhancement using a switchable magnetic trap

DOEpatents

Beer, Neil Reginald [Pleasanton, CA

2012-05-29

A system for analyzing a sample including providing a microchannel flow channel; associating the sample with magnetic nanoparticles or magnetic polystyrene-coated beads; moving the sample with said magnetic nanoparticles or magnetic polystyrene-coated beads in the microchannel flow channel; holding the sample with the magnetic nanoparticles or magnetic polystyrene-coated beads in a magnetic trap in the microchannel flow channel; and analyzing the sample obtaining an enhanced analysis signal. An apparatus for analysis of a sample includes magnetic particles connected to the sample, a microchip, a flow channel in the microchip, a source of carrier fluid connected to the flow channel for moving the sample in the flow channel, an electromagnet trap connected to the flow line for selectively magnetically trapping the sample and the magnetic particles, and an analyzer for analyzing the sample.

Mass Transfer And Hydraulic Testing Of The V-05 And V-10 Contactors With The Next Generation Solvent

DOE Office of Scientific and Technical Information (OSTI.GOV)

Herman, D. T.; Duignan, M. R.; Williams, M. R.

The Modular Caustic Side Solvent Extraction (CSSX) Unit (MCU) facility is actively pursuing the transition from the current BOBCalixC6 based solvent to the Next Generation Solvent (NGS)-MCU solvent. To support this integration of NGS into the MCU facilities, Savannah River Remediation (SRR) requested that Savannah River National Laboratory (SRNL) perform testing of a blend of the NGS (MaxCalix based solvent) with the current solvent (BOBCalixC6 based solvent) for the removal of cesium (Cs) from the liquid salt waste stream. This testing differs from prior testing by utilizing a blend of BOBCalixC6 based solvent and the NGS with the full (0.05more » M) concentration of the MaxCalix as well as a new suppressor, tris(3,7dimethyloctyl) guanidine. Single stage tests were conducted using the full size V-05 and V-10 centrifugal contactors installed at SRNL. These tests were designed to determine the mass transfer and hydraulic characteristics with the NGS solvent blended with the projected heel of the BOBCalixC6 based solvent that will exist in MCU at time of transition. The test program evaluated the amount of organic carryover and the droplet size of the organic carryover phases using several analytical methods. Stage efficiency and mass distribution ratios were determined by measuring Cs concentration in the aqueous and organic phases during single contactor testing. The nominal cesium distribution ratio, D(Cs) measured for extraction ranged from 37-60. The data showed greater than 96% stage efficiency for extraction. No significant differences were noted for operations at 4, 8 or 12 gpm aqueous salt simulant feed flow rates. The first scrub test (contact with weak caustic solution) yielded average scrub D(Cs) values of 3.3 to 5.2 and the second scrub test produced an average value of 1.8 to 2.3. For stripping behavior, the “first stage” D Cs) values ranged from 0.04 to 0.08. The efficiency of the low flow (0.27 gpm aqueous) was calculated to be 82.7%. The Spreadsheet Algorithm for Stagewise Solvent Extraction (SASSE) predicted equivalent DF for MCU from this testing is greater than 3,500 assuming 95% efficiency during extraction and 80% efficiency during scrub and strip. Hydraulically, the system performed very well in all tests. Target flows were easily obtained and stable throughout testing. Though some issues were encountered with plugging in the coalescer, they were not related to the solvent. No hydraulic upsets due to the solvent were experienced during any of the tests conducted. The first extraction coalescer element used in testing developed high pressure drop that made it difficult to maintain the target flow rates. Analysis showed an accumulation of sodium aluminosilicate solids. The coalescer was replaced with one from the same manufacturer’s lot and pressure drop was no longer an issue. Concentrations of Isopar™ L and Modifier were measured using semi-volatile organic analysis (SVOA) and high performance liquid chromatography (HPLC) to determine the amount of solvent carryover. For low-flow (0.27 gpm aqueous) conditions in stripping, SVOA measured the Isopar™ L post-contactor concentration to be 25 mg/L, HPLC measured 39 mg/L of Modifier. For moderate-flow (0.54 gpm aqueous) conditions, SVOA measured the Isopar™ L postcontactor to be ~69 mg/L, while the HPLC measured 56 mg/L for Modifier. For high-flow (0.8 gpm aqueous) conditions, SVOA measured the Isopar™ L post-contactor to be 39 mg/L. The post-coalescer (pre-decanter) measurements by SVOA for Isopar™ L were all less than the analysis detection limit of 10 mg/L. The HPLC measured 18, 22 and 20 mg/L Modifier for the low, medium, and high-low rates respectively. In extraction, the quantity of pre-coalescer Isopar™ L carryover measured by SVOA was ~280-410 mg/L at low flow (4 gpm aqueous), ~400-450 mg/L at moderate flow (8 gpm aqueous), and ~480 mg/L at high flow (12 gpm aqueous). The amount of post coalescer (pre-decanter) Isopar™ L carryover measured by SVOA was less than 45 mg/L for all flow rates. HPLC results for Modifier were 182, 217 and 222 mg/L for the post-contactor low, medium and high flow rates. The post-coalescer (pre-decanter) samples were measured to contain 12, 10 and 22 mg/L Modifier for the low, medium, and high flow rates. The carryover results and droplet size measurements were used to determine the decanter performance utilizing the decanter model developed by the ARES Corporation. Results show for the targeted salt flow rate of approximately 8 gpm, that over 93% of the solvent carryover from stripping is predicted to be recovered and over 96% solvent carryover from extraction is predicted to be recovered. This translates to a predicted solvent carryover of <3 ppm from stripping and <20 ppm solvent carryover from extraction. This projected performance at MCU is expected to be well within the operating limits and the historical performance for the baseline BOBCalixC6 based solvent. Droplet-size data obtained by MicroTrac™ S3400 analyzer consistently shows that the droplet size post-oalescer is significantly greater than the post-contactor or pre-coalescer samples. Increased flow rates did not show a consistent impact to the droplet size results. For the extraction testing, droplet size analysis showed that the post-contactor and pre-coalescer samples were essentially the same. The mean droplet sizes post-coalescer were less than the mean droplet sizes pre-coalescer with a very slight upward trend in the mean droplet size as the flow rate was increased. This result is probably due to the method of sampling. The larger post-coalescer drops immediately rise to the surface after leaving the coalescer element. The downstream sampling point was horizontally in-line with the element and therefore would only capture those organic droplets well mixed in the flowing aqueous stream.« less

SRNL SHELF LIFE STUDIES - SCC STUDIES AT ROOM TEMPERTURE [stress corrosion cracking

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mickalonis, J.; Duffey, J.

Phase II, Series 2 corrosion testing performed by the Savannah River National Laboratory (SRNL) for the Department of Energy 3013 container has been completed. The corrosion tests are part of an integrated plan conducted jointly by Los Alamos National Laboratory and the Savannah River Site. SRNL was responsible for conducting corrosion studies in small-scale vessels to address the influence of salt composition, water loading, and type of oxide/salt contact on the relative humidity inside a 3013 container and on the resulting corrosion of Type 304L and 316L stainless steel (304L and 316L). This testing was conducted in two phases: Phasemore » I evaluated a broad spectrum of salt compositions and initial water loadings on the salt mixtures exposed to 304L and 316L and the resulting corrosion; Phase II evaluated the corrosion of 304L at specific water loadings and a single salt composition. During Phase I testing at high initial moisture levels (0.35 to 1.24 wt%)a, the roomtemperature corrosion of 304L exposed to a series of plutonium oxide/chloride salt mixtures ranged from superficial staining to pitting and stress corrosion cracking (SCC). 304L teardrop coupons that exhibited SCC were directly exposed to a mixture composed of 98 wt % PuO2, 0.9 wt % NaCl, 0.9 wt % KCl, and 0.2 wt % CaCl2. Cracking was not observed in a 316L teardrop coupon. Pitting was also observed in this environment for both 304L and 316L with depths ranging from 20 to 100 μm. Neither pitting nor SCC was observed in mixtures with a greater chloride salt concentration (5 and 28 wt%). These results demonstrated that for a corrosive solution to form a balance existed between the water loading and the salt chloride concentration. This chloride solution results from the interaction of loaded water with the hydrating CaCl2 salt. In Phase II, Series 1 tests, the SCC results were shown to be reproducible with cracking occurring in as little as 85 days. The approximate 0.5 wt% moisture level was found to result in an initial relative humidity of ~55% within the small-scale vessels. Pits were found to be associated with cracks and appeared to act as initiators for the cracking. In a vapor-space only exposure, the weld oxide, which results from the TIG closure weld used to fabricate the teardrop coupon, was also shown to be more susceptible to pitting corrosion than a surface free from weld oxide. This result has important implications for the closure weld of the 3013 inner can since the weld oxide on the can internal surface cannot be removed. The results from the Phase II, Series 2 tests further demonstrated the significance of forming a solution with a critical chloride concentration for corrosion to proceed. 304L teardrop coupons were found to corrode only by pitting with a similar oxide/salt mixture as used in Series 1 testing but with a lower water loading of 0.2 wt%, which resulted in an initial relative humidity of 35-38%. These tests ran twice as long as those for Series 1 testing. The exposure condition was also found to impact the corrosion with salt-exposed surfaces showing lower corrosion resistance. Additional analyses of the Series 2 coupons are recommended especially for determining if cracks emanate from the bottom of pits. Data generated under the 2009 3013 corrosion test plan, as was presented here, increased the understanding of the corrosion process within a sealed 3013 container. Along with the corrosion data from destructive evaluations of 3013 containers, the inner can closure weld region (ICCWR) has been identified as the most vulnerable area of the inner can where corrosion may lead to corrosive species leaking to the interior surface of the outer container, thereby jeopardizing the integrity of the 3013 container. A new corrosion plan has been designed that will characterize the corrosion at the ICCWR of 3013 DEs as well as parameters affecting this corrosion.« less

Performance evaluation of the Abbott CELL-DYN Emerald for use as a bench-top analyzer in a research setting.

PubMed

Khoo, T-L; Xiros, N; Guan, F; Orellana, D; Holst, J; Joshua, D E; Rasko, J E J

2013-08-01

The CELL-DYN Emerald is a compact bench-top hematology analyzer that can be used for a three-part white cell differential analysis. To determine its utility for analysis of human and mouse samples, we evaluated this machine against the larger CELL-DYN Sapphire and Sysmex XT2000iV hematology analyzers. 120 human (normal and abnormal) and 30 mouse (normal and abnormal) samples were analyzed on both the CELL-DYN Emerald and CELL-DYN Sapphire or Sysmex XT2000iV analyzers. For mouse samples, the CELL-DYN Emerald analyzer required manual recalibration based on the histogram populations. Analysis of the CELL-DYN Emerald showed excellent precision, within accepted ranges (white cell count CV% = 2.09%; hemoglobin CV% = 1.68%; platelets CV% = 4.13%). Linearity was excellent (R² ≥ 0.99), carryover was minimal (<1%), and overall interinstrument agreement was acceptable for both human and mouse samples. Comparison between the CELL-DYN Emerald and Sapphire analyzers for human samples or Sysmex XT2000iV analyzer for mouse samples showed excellent correlation for all parameters. The CELL-DYN Emerald was generally comparable to the larger reference analyzer for both human and mouse samples. It would be suitable for use in satellite research laboratories or as a backup system in larger laboratories. © 2012 John Wiley & Sons Ltd.

Droplet actuator analyzer with cartridge

NASA Technical Reports Server (NTRS)

Sturmer, Ryan A. (Inventor); Paik, Philip Y. (Inventor); Srinivasan, Vijay (Inventor); Brafford, Keith R. (Inventor); West, Richard M. (Inventor); Smith, Gregory F. (Inventor); Pollack, Michael G. (Inventor); Pamula, Vamsee K. (Inventor)

2011-01-01

A droplet actuator with cartridge is provided. According to one embodiment, a sample analyzer is provided and includes an analyzer unit comprising electronic or optical receiving means, a cartridge comprising self-contained droplet handling capabilities, and a wherein the cartridge is coupled to the analyzer unit by a means which aligns electronic and/or optical outputs from the cartridge with electronic or optical receiving means on the analyzer unit. According to another embodiment, a sample analyzer is provided and includes a sample analyzer comprising a cartridge coupled thereto and a means of electrical interface and/or optical interface between the cartridge and the analyzer, whereby electrical signals and/or optical signals may be transmitted from the cartridge to the analyzer.

Fluoride content in table salt distributed in Mexico City, Mexico.

PubMed

Hernández-Guerrero, Juan Carlos; de la Fuente-Hernández, Javier; Jiménez-Farfán, Maria Dolores; Ledesma-Montes, Constantino; Castañeda-Castaneira, Enrique; Molina-Frechero, Nelly; Jacinto-Alemán, Luís Fernando; Juárez-Lopez, Lilia Adriana; Moreno-Altamirano, Alejandra

2008-01-01

The aim of this study was to analyze table salt available in Mexico City's market to identify the fluoride concentrations and to compare these with the Mexican regulations. We analyzed 44 different brands of table salt. All samples were purchased at random in different stores, supermarkets, and groceries from Mexico City's metropolitan area and analyzed in triplicate in three different laboratories (nine determinations per sample) with an Orion 720 A potentiometer and an Orion 9609 BN ion-specific electrode. Fluoride concentration in the samples varied from 0 ppm to 485 ppm. It was found that fluoride concentration varied widely among the analyzed brands. Also, we found that fluoride concentration in 92 percent of the analyzed samples did not match with that printed on the label. Only 6.8 percent of the analyzed samples contained fluoride concentrations that meet Mexican and WHO regulations. The broad variation in the analyzed samples suggests that Mexican Public Health authorities must implement more stringent regulation guidelines and procedures for controlling the distribution of salt and its fluoride concentration for human consumption.

Cholesterol content of broiler breast fillets heated with and without the skin in convection and conventional ovens.

PubMed

Prusa, K J; Lonergan, M M

1987-06-01

Six treatment combinations for the heating of broiler breast fillets were investigated: three skin variables (heated and analyzed with skin, heated with and analyzed without skin, and heated and analyzed without skin) and two heating systems (convection broiling and conventional roasting). Matched broiler breast fillets were analyzed raw or breaded and heated to 82 C. Raw and cooked samples of meat, skin, and meat with skin were analyzed for moisture, fat, and cholesterol contents. In the raw state, samples of meat with skin contained greater moisture and fat contents, but similar cholesterol contents, when compared with samples of meat alone. Fillets heated by convection broiling had greater cooking losses but shorter heating times compared with conventionally roasted samples. Fillets with the skin removed before or after heating contained more moisture, less fat, and less cholesterol than samples cooked and analyzed with the skin present.

Evaluating All-Metal Valves for Use in a Tritium Environment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Houk, L.; Payton, A.

In the tritium gas processing system, it is desired to minimize polymer components due to their degradation from tritium exposure (beta decay). One source of polymers in the tritium process is valve components. A vendor has been identified that manufactures a valve that is marketed as being made from all-metal construction. This manufacturer, Ham-Let Group, manufactures a diaphragm valve (3LE series) that claims to be made entirely of metal. SRNL procured twelve (12) Ham-Let diaphragm valves for characterization and evaluation. The characterization tests include identification of the maximum pressure of these valves by performing pressure and burst tests. Leak testsmore » were performed to ensure the valves do not exceed the acceptable leak rate for tritium service. These valves were then cycled in a nitrogen gas and/or vacuum environment to ensure they would be durable in a process environment. They were subsequently leak tested per ASTM protocol to ensure that the valves maintained their leak tight integrity. A detailed material analysis was also conducted to determine hydrogen and tritium compatibility.« less

488-4D ASH LANDFILL CLOSURE CAP HELP MODELING

DOE Office of Scientific and Technical Information (OSTI.GOV)

Phifer, M.

At the request of Area Completion Projects (ACP) in support of the 488-4D Landfill closure, the Savannah River National Laboratory (SRNL) has performed Hydrologic Evaluation of Landfill Performance (HELP) modeling of the planned 488-4D Ash Landfill closure cap to ensure that the South Carolina Department of Health and Environmental Control (SCDHEC) limit of no more than 12 inches of head on top of the barrier layer (saturated hydraulic conductivity of no more than 1.0E-05 cm/s) in association with a 25-year, 24-hour storm event is not projected to be exceeded. Based upon Weber 1998 a 25-year, 24-hour storm event at themore » Savannah River Site (SRS) is 6.1 inches. The results of the HELP modeling indicate that the greatest peak daily head on top of the barrier layer (i.e. geosynthetic clay liner (GCL) or high density polyethylene (HDPE) geomembrane) for any of the runs made was 0.079 inches associated with a peak daily precipitation of 6.16 inches. This is well below the SCDHEC limit of 12 inches.« less

Status Report - Cane Fiberboard Properties and Degradation Rates for Storage of the 9975 Shipping Package in KAMS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Daugherty, W. L.

Thermal, mechanical and physical properties have been measured on cane fiberboard samples following accelerated aging for up to approximately 7 years. The aging environments have included elevated temperature < 250 ?F (the maximum allowed service temperature for fiberboard in 9975 packages) and elevated humidity. The results from this testing have been analyzed, and aging models fit to the data. Correlations relating several properties (thermal conductivity, energy absorption, weight loss and height decrease) to their rate of change in potential storage environments have been developed. Combined with an estimate of the actual conditions the fiberboard experiences in KAMS, these models allowmore » development of service life predictions. Some of the predicted degradation rates presented in this report are relatively extreme. However, these relate to environments that do not exist within KAMS, or would be postulated only as upset conditions that would not likely persist for an extended period. For a typical package with ~10 watts internal heat load or less, and ambient temperatures below 90 ?F, the fiberboard experiences storage conditions less severe than any of the aging environments. Little or no degradation of the fiberboard is expected for typical storage conditions. It should be noted that the ultimate service life will be determined by the cumulative effect of degradation from all the conditions these packages might encounter. The assumptions and inputs behind the models in this report should be well understood before attempting to identify an actual service life in KAMS. Additional data continue to be collected to permit future refinements to the models and assumptions. For developing service life predictions, the ambient conditions within KAMS can be reasonably identified, and the temperature profiles within the various packages (with a range of heat loads and at varying locations within an array of packages) can be calculated. However, the humidity within the package is not as well characterized. While the outer drum does not provide an air-tight seal, it does greatly restrict the gain or loss of moisture in the fiberboard. Preliminary efforts have identified a relationship between the moisture content of fiberboard samples and the relative humidity of the surrounding air, but further work is needed in this area. Improvement in understanding this relationship might be realized with a change in the way humidity data are collected during field surveillances. It is recommended that the humidity be measured through a caplug hole before the package is removed from its storage location. The package would remain in thermal equilibrium, and anomalous humidity changes could be avoided. Further work should be performed to better define KAMS storage conditions and the environment within the 9975 shipping packages, and to identify appropriate limits for each property. This should be a joint effort by SRNL and NMM personnel. The results and model predictions presented in this report are applicable to 9975 packages with cane fiberboard overpack assemblies. A separate effort is underway to identify whether softwood fiberboard would behave similarly. In addition, the degradation models do not address the effects of non-conforming conditions such as the presence of excess moisture and mold, or beetle infestations.« less

Lab Analyses of Pet Coke Samples

EPA Pesticide Factsheets

April 2014: the EPA Chicago Regional Laboratory analyzed samples taken from petroleum coke (petcoke) storage piles at KCBX facilities in southeast Chicago. The samples were analyzed for metals, radionuclides and PAHs.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cordaro, J.; Shull, D.; Farrar, M.

Radiation monitoring in nuclear facilities is essential to safe operation of the equipment as well as protecting personnel. In specific, typical air monitoring of radioactive gases or particulate involves complex systems of valves, pumps, piping and electronics. The challenge is to measure a representative sample in areas that are radioactively contaminated. Running cables and piping to these locations is very expensive due to the containment requirements. Penetration into and out of an airborne or containment area is complex and costly. The process rooms are built with thick rebar-enforced concrete walls with glove box containment chambers inside. Figure 1 shows highmore » temperature radiation resistance cabling entering the top of a typical glove box. In some case, the entire processing area must be contained in a 'hot cell' where the only access into the chamber is via manipulators. An example is shown in Figure 2. A short range wireless network provides an ideal communication link for transmitting the data from the radiation sensor to a 'clean area', or area absent of any radiation fields or radioactive contamination. Radiation monitoring systems that protect personnel and equipment must meet stringent codes and standards due to the consequences of failure. At first glance a wired system would seem more desirable. Concerns with wireless communication include latency, jamming, spoofing, man in the middle attacks, and hacking. The Department of Energy's Savannah River National Laboratory (SRNL) has developed a prototype wireless radiation air monitoring system that address many of the concerns with wireless and allows quick deployment in radiation and contamination areas. It is stand alone and only requires a standard 120 VAC, 60 Hz power source. It is designed to be mounted or portable. The wireless link uses a National Security Agency (NSA) Suite B compliant wireless network from Fortress Technologies that is considered robust enough to be used for classified data transmission in place of NSA Type 1 devices.« less

Test Plan - Solids Accumulation Scouting Studies

DOE Office of Scientific and Technical Information (OSTI.GOV)

Duignan, M. R.; Steeper, T. J.; Steimke, J. L.

This plan documents the highlights of the Solids Accumulations Scouting Studies test; a project, from Washington River Protection Solutions (WRPS), that began on February 1, 2012. During the last 12 weeks considerable progress has been made to design and plan methods that will be used to estimate the concentration and distribution of heavy fissile solids in accumulated solids in the Hanford double-shell tank (DST) 241-AW-105 (AW-105), which is the primary goal of this task. This DST will be one of the several waste feed delivery staging tanks designated to feed the Pretreatment Facility (PTF) of the Waste Treatment and Immobilizationmore » Plant (WTP). Note that over the length of the waste feed delivery mission AW-105 is currently identified as having the most fill empty cycles of any DST feed tanks, which is the reason for modeling this particular tank. At SRNL an existing test facility, the Mixing Demonstration Tank, which will be modified for the present work, will use stainless steel particles in a simulant that represents Hanford waste to perform mock staging tanks transfers that will allow solids to accumulate in the tank heel. The concentration and location of the mock fissile particles will be measured in these scoping studies to produce information that will be used to better plan larger scaled tests. Included in these studies is a secondary goal of developing measurement methods to accomplish the primary goal. These methods will be evaluated for use in the larger scale experiments. Included in this plan are the several pretest activities that will validate the measurement techniques that are currently in various phases of construction. Aspects of each technique, e.g., particle separations, volume determinations, topographical mapping, and core sampling, have been tested in bench-top trials, as discussed herein, but the actual equipment to be employed during the full test will need evaluation after fabrication and integration into the test facility.« less

Evaluation of Canisterized Foams and Evaluation of Radiation Hardened Foams for D&D Activities

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nicholson, J. C.

The introduction of polyurethane foams has previously been examined elsewhere within the DOE complex with regards to decontamination and decommissioning (D&D) activities, though its use has been prohibited as a result of excessive heat generation and flammability concerns per the safety basis. Should these foams be found compatible with respect to the facility safety basis requirements, D&D work involving large void containing structures such as gloveboxes could be eased through the fixation of residual contamination after decontamination efforts have concluded. To this end, SRNL embarked on a characterization of commercial epoxy foams to identify the characteristics that would be mostmore » important to safety basis requirements. Through SRNL’s efforts, the performance of commercial two-part epoxy foams was evaluated for their foaming characteristics, temperature profiles, loading capability with high-Z (high density) additives, and applicability for shielding gamma emission from isotopes including; Am-241, Cs-137, and Co-60. It was found that these foams are capable of encapsulation of a desired volume, though the ideal and experimental expansion coefficients were found to differ. While heat is generated during the reaction, no samples generated heat above 70 °C. Of the down–selected materials, heating was on the order of 40 °C for the flexible foam and 60 °C for the rigid foam. Both were found to return to room temperature after 20 minutes regardless of the volume of foam cast. It was also found that the direct introduction of high-Z additives were capable of attenuating 98% of Am-241 gamma signal, 16% of Cs-137 signal, and 9.5% of Co-60 signal at 1:1 loading capacities of total liquid constituent weight to additive weight. These efforts are currently being reviewed for the ASTM January 2017 subcommittee discussions to address the lack of test methods and standards regarding these materials with respect to D&D environments.« less

The endothelial sample size analysis in corneal specular microscopy clinical examinations.

PubMed

Abib, Fernando C; Holzchuh, Ricardo; Schaefer, Artur; Schaefer, Tania; Godois, Ronialci

2012-05-01

To evaluate endothelial cell sample size and statistical error in corneal specular microscopy (CSM) examinations. One hundred twenty examinations were conducted with 4 types of corneal specular microscopes: 30 with each BioOptics, CSO, Konan, and Topcon corneal specular microscopes. All endothelial image data were analyzed by respective instrument software and also by the Cells Analyzer software with a method developed in our lab. A reliability degree (RD) of 95% and a relative error (RE) of 0.05 were used as cut-off values to analyze images of the counted endothelial cells called samples. The sample size mean was the number of cells evaluated on the images obtained with each device. Only examinations with RE < 0.05 were considered statistically correct and suitable for comparisons with future examinations. The Cells Analyzer software was used to calculate the RE and customized sample size for all examinations. Bio-Optics: sample size, 97 ± 22 cells; RE, 6.52 ± 0.86; only 10% of the examinations had sufficient endothelial cell quantity (RE < 0.05); customized sample size, 162 ± 34 cells. CSO: sample size, 110 ± 20 cells; RE, 5.98 ± 0.98; only 16.6% of the examinations had sufficient endothelial cell quantity (RE < 0.05); customized sample size, 157 ± 45 cells. Konan: sample size, 80 ± 27 cells; RE, 10.6 ± 3.67; none of the examinations had sufficient endothelial cell quantity (RE > 0.05); customized sample size, 336 ± 131 cells. Topcon: sample size, 87 ± 17 cells; RE, 10.1 ± 2.52; none of the examinations had sufficient endothelial cell quantity (RE > 0.05); customized sample size, 382 ± 159 cells. A very high number of CSM examinations had sample errors based on Cells Analyzer software. The endothelial sample size (examinations) needs to include more cells to be reliable and reproducible. The Cells Analyzer tutorial routine will be useful for CSM examination reliability and reproducibility.

Quality-Assurance Data for Routine Water Analyses by the U.S. Geological Survey Laboratory in Troy, New York - July 2005 through June 2007

USGS Publications Warehouse

Lincoln, Tricia A.; Horan-Ross, Debra A.; McHale, Michael R.; Lawrence, Gregory B.

2009-01-01

The laboratory for analysis of low-ionic-strength water at the U.S. Geological Survey (USGS) Water Science Center in Troy, N.Y., analyzes samples collected by USGS projects throughout the Northeast. The laboratory's quality-assurance program is based on internal and interlaboratory quality-assurance samples and quality-control procedures that were developed to ensure proper sample collection, processing, and analysis. The quality-assurance and quality-control data were stored in the laboratory's Lab Master data-management system, which provides efficient review, compilation, and plotting of data. This report presents and discusses results of quality-assurance and quality control samples analyzed from July 2005 through June 2007. Results for the quality-control samples for 19 analytical procedures were evaluated for bias and precision. Control charts indicate that data for eight of the analytical procedures were occasionally biased for either high-concentration or low-concentration samples but were within control limits; these procedures were: total aluminum, calcium, magnesium, nitrate (colorimetric method), potassium, silicon, sodium, and sulfate. Eight of the analytical procedures were biased throughout the analysis period for the high-concentration sample, but were within control limits; these procedures were: total aluminum, calcium, dissolved organic carbon, chloride, nitrate (ion chromatograph), potassium, silicon, and sulfate. The magnesium and pH procedures were biased throughout the analysis period for the low-concentration sample, but were within control limits. The acid-neutralizing capacity, total monomeric aluminum, nitrite, and specific conductance procedures were biased for the high-concentration and low-concentration samples, but were within control limits. Results from the filter-blank and analytical-blank analyses indicated that the procedures for 16 of 17 analytes were within control limits, although the concentrations for blanks were occasionally outside the control limits. The data-quality objective was not met for dissolved organic carbon. Sampling and analysis precision are evaluated herein in terms of the coefficient of variation obtained for triplicate samples in the procedures for 18 of the 21 analytes. At least 93 percent of the samples met data-quality objectives for all analytes except acid-neutralizing capacity (85 percent of samples met objectives), total monomeric aluminum (83 percent of samples met objectives), total aluminum (85 percent of samples met objectives), and chloride (85 percent of samples met objectives). The ammonium and total dissolved nitrogen did not meet the data-quality objectives. Results of the USGS interlaboratory Standard Reference Sample (SRS) Project met the Troy Laboratory data-quality objectives for 87 percent of the samples analyzed. The P-sample (low-ionic-strength constituents) analysis had two outliers each in two studies. The T-sample (trace constituents) analysis and the N-sample (nutrient constituents) analysis had one outlier each in two studies. Results of Environment Canada's National Water Research Institute (NWRI) program indicated that at least 85 percent of the samples met data-quality objectives for 11 of the 14 analytes; the exceptions were acid-neutralizing capacity, total aluminum and ammonium. Data-quality objectives were not met in 41 percent of samples analyzed for acid-neutralizing capacity, 50 percent of samples analyzed for total aluminum, and 44 percent of samples analyzed for ammonium. Results from blind reference-sample analyses indicated that data-quality objectives were met by at least 86 percent of the samples analyzed for calcium, magnesium, pH, potassium, and sodium. Data-quality objectives were met by 76 percent of the samples analyzed for chloride, 80 percent of the samples analyzed for specific conductance, and 77 percent of the samples analyzed for sulfate.

On-Line Analyzer For Monitoring Trace Amounts Of Oil In Turbid Waters

NASA Astrophysics Data System (ADS)

Niemela, P.; Jaatinen, J.

1986-05-01

This report presents an automated analyzer which continuously monitors oil content of a sample water stream that flows through the analyzer. The measuring principle is based on the absorption of infrared radiation by oil molecules contained in the sample water. The wavelength band that is used in the measurement is at 3.4 μm, where different types of oils show nearly equal absorption. Another wavelength band of 3.6 μm, where oil has no absorption, is used to compensate the effect of turbidity, which is due to solid particles and oil droplets contained in the sample water. Before entering the analyzer the sample water flow is properly homogenized. To compensate the strong absorption by water molecules in these wavelength bands the sample water is compared with reference water. This is done by directing them alternately through the same measuring cell. The reference water is obtained from the sample water by ultrafiltration and it determines the base line for the contaminated sample water. To ensure the stability of the base line, temperature and pressure differences of the two waters are kept within adequate ranges. Areas of application of the analyzer are wide ranging i.a. from ships' discharge waters to waste waters of industrial processes. The first application of the analyzer is on board oil tankers to control the discharge process of bilge and ballast waters. The analyzer is the first that fully corresponds to the stringent regulations for oil content monitors by the International Maritime Organization (IMO). Pilot installations of the analyzer are made on industrial plants.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Plemons, R.E.; Hopwood, W.H. Jr.; Hamilton, J.H.

For a number of years the Oak Ridge Y-12 Plant Laboratory has been analyzing coal predominately for the utilities department of the Y-12 Plant. All laboratory procedures, except a Leco sulfur method which used the Leco Instruction Manual as a reference, were written based on the ASTM coal analyses. Sulfur is analyzed at the present time by two methods, gravimetric and Leco. The laboratory has two major endeavors for monitoring the quality of its coal analyses. (1) A control program by the Plant Statistical Quality Control Department. Quality Control submits one sample for every nine samples submitted by the utilitiesmore » departments and the laboratory analyzes a control sample along with the utilities samples. (2) An exchange program with the DOE Coal Analysis Laboratory in Bruceton, Pennsylvania. The Y-12 Laboratory submits to the DOE Coal Laboratory, on even numbered months, a sample that Y-12 has analyzed. The DOE Coal Laboratory submits, on odd numbered months, one of their analyzed samples to the Y-12 Plant Laboratory to be analyzed. The results of these control and exchange programs are monitored not only by laboratory personnel, but also by Statistical Quality Control personnel who provide statistical evaluations. After analysis and reporting of results, all utilities samples are retained by the laboratory until the coal contracts have been settled. The utilities departments have responsibility for the initiation and preparation of the coal samples. The samples normally received by the laboratory have been ground to 4-mesh, reduced to 0.5-gallon quantities, and sealed in air-tight containers. Sample identification numbers and a Request for Analysis are generated by the utilities departments.« less

40 CFR 86.159-08 - Exhaust emission test procedures for US06 emissions.

Code of Federal Regulations, 2013 CFR

2013-07-01

... gasoline-fueled Otto-cycle vehicles, the composite samples collected in bags are analyzed for THC, CO, CO2, CH4, and NOX. For petroleum-fueled diesel-cycle vehicles, THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel bag samples of dilution air are analyzed for THC, CO, CO2...

40 CFR 86.159-08 - Exhaust emission test procedures for US06 emissions.

Code of Federal Regulations, 2014 CFR

2014-07-01

... gasoline-fueled Otto-cycle vehicles, the composite samples collected in bags are analyzed for THC, CO, CO2, CH4, and NOX. For petroleum-fueled diesel-cycle vehicles, THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel bag samples of dilution air are analyzed for THC, CO, CO2...

40 CFR 86.159-08 - Exhaust emission test procedures for US06 emissions.

Code of Federal Regulations, 2011 CFR

2011-07-01

... gasoline-fueled Otto-cycle vehicles, the composite samples collected in bags are analyzed for THC, CO, CO2, CH4, and NOX. For petroleum-fueled diesel-cycle vehicles, THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel bag samples of dilution air are analyzed for THC, CO, CO2...

40 CFR 86.159-08 - Exhaust emission test procedures for US06 emissions.

Code of Federal Regulations, 2010 CFR

2010-07-01

... gasoline-fueled Otto-cycle vehicles, the composite samples collected in bags are analyzed for THC, CO, CO2, CH4, and NOX. For petroleum-fueled diesel-cycle vehicles, THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel bag samples of dilution air are analyzed for THC, CO, CO2...

40 CFR 86.159-08 - Exhaust emission test procedures for US06 emissions.

Code of Federal Regulations, 2012 CFR

2012-07-01

... gasoline-fueled Otto-cycle vehicles, the composite samples collected in bags are analyzed for THC, CO, CO2, CH4, and NOX. For petroleum-fueled diesel-cycle vehicles, THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel bag samples of dilution air are analyzed for THC, CO, CO2...

Radionuclides, inorganic constituents, organic compounds, and bacteria in water from selected wells and springs from the southern boundary of the Idaho National Engineering Laboratory to the Hagerman Area, Idaho, 1991

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bartholomay, R.C.; Edwards, D.D.; Campbell, L.J.

1993-11-01

The US Geological Survey and the Idaho Department of Water Resources, in response to a request from the US Department of Energy, sampled 18 sites as part of a long-term project to monitor water quality of the Snake River Plain aquifer from the southern boundary of the Idaho National Engineering Laboratory to the Hagerman area. Water samples were collected and analyzed for manmade pollutants and naturally occurring constituents. The samples were collected from six irrigation wells, seven domestic wells, two springs, one stock well, one dairy well, and one observation well. Quality assurance samples also were collected and analyzed. Themore » water samples were analyzed for selected radionuclides, inorganic constituents, organic compounds, and bacteria. None of the samples analyzed for radionuclides, inorganic constituents, or organic compounds exceeded the established maximum contaminant levels for drinking water. Most of the radionuclide and inorganic constituent concentrations exceeded their respective reporting levels. All the samples analyzed for dissolved organic carbon had concentrations that exceeded their reporting level. Concentrations of 1,1,1 -trichloroethane exceeded the reporting level in two water samples. Two samples and a quality assurance replicate contained reportable concentrations of 2, 4-D. One sample contained fecal coliform bacteria counts that exceeded established maximum contaminant levels for drinking water.« less

High heating rate thermal desorption for molecular surface sampling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ovchinnikova, Olga S.; Van Berkel, Gary J.

2016-03-29

A method for analyzing a sample having at least one analyte includes the step of heating the sample at a rate of at least 10.sup.6 K/s to thermally desorb at least one analyte from the sample. The desorbed analyte is collected. The analyte can then be analyzed.

Comparing Cumberland With Other Samples Analyzed by Curiosity

NASA Image and Video Library

2014-12-16

This graphic offers comparisons between the amount of an organic chemical named chlorobenzene detected in the Cumberland rock sample and amounts of it in samples from three other Martian surface targets analyzed by NASA Curiosity Mars rover.

Atmospheric sampling glow discharge ionization source

DOEpatents

McLuckey, Scott A.; Glish, Gary L.

1989-01-01

An atmospheric sampling glow discharge ionization source that can be used in combination with an analytical instrument which operates at high vacuum, such as a mass spectrometer. The atmospheric sampling glow discharge ionization source comprises a chamber with at least one pair of electrodes disposed therein, an inlet for a gaseous sample to be analyzed and an outlet communicating with an analyzer which operates at subatmospheric pressure. The ionization chamber is maintained at a pressure below atmospheric pressure, and a voltage difference is applied across the electrodes to induce a glow discharge between the electrodes, so that molecules passing through the inlet are ionized by the glow discharge and directed into the analyzer. The ionization source accepts the sample under atmospheric pressure conditions and processes it directly into the high vacuum instrument, bridging the pressure gap and drawing off unwanted atmospheric gases. The invention also includes a method for analyzing a gaseous sample using the glow discharge ionization source described above.

Fluidics platform and method for sample preparation and analysis

DOEpatents

Benner, W. Henry; Dzenitis, John M.; Bennet, William J.; Baker, Brian R.

2014-08-19

Herein provided are fluidics platform and method for sample preparation and analysis. The fluidics platform is capable of analyzing DNA from blood samples using amplification assays such as polymerase-chain-reaction assays and loop-mediated-isothermal-amplification assays. The fluidics platform can also be used for other types of assays and analyzes. In some embodiments, a sample in a sealed tube can be inserted directly. The following isolation, detection, and analyzes can be performed without a user's intervention. The disclosed platform may also comprises a sample preparation system with a magnetic actuator, a heater, and an air-drying mechanism, and fluid manipulation processes for extraction, washing, elution, assay assembly, assay detection, and cleaning after reactions and between samples.

BACTERIOLOGICAL ANALYSIS WITH SAMPLING AND SAMPLE PRESERVATION SPECIFICS

EPA Science Inventory

Current federal regulations (40CFR 503) specify that under certain conditions treated municipal biosolids must be analyzed for fecal coliform or salmonellae. The regulations state that representative samples of biosolids must be collected and analyzed using standard methods. Th...

Real-time exhaust gas modular flowmeter and emissions reporting system for mobile apparatus

NASA Technical Reports Server (NTRS)

Breton, Leo Alphonse Gerard (Inventor)

2002-01-01

A real-time emissions reporting system includes an instrument module adapted to be detachably connected to the exhaust pipe of a combustion engine to provide for flow of exhaust gas therethrough. The instrument module includes a differential pressure probe which allows for determination of flow rate of the exhaust gas and a gas sampling tube for continuously feeding a sample of the exhaust gas to a gas analyzer or a mounting location for a non-sampling gas analyzer. In addition to the module, the emissions reporting system also includes an elastomeric boot for detachably connecting the module to the exhaust pipe of the combustion engine, a gas analyzer for receiving and analyzing gases sampled within the module and a computer for calculating pollutant mass flow rates based on concentrations detected by the gas analyzer and the detected flowrate of the exhaust gas. The system may also include a particulate matter detector with a second gas sampling tube feeding same mounted within the instrument module.

Environmental Asbestos Assessment Manual: Superfund Method for the Determination of Asbestos in Ambient Air, Part 1: Method

EPA Science Inventory

This is a sampling and analysis method for the determination of asbestos in air. Samples are analyzed by transmission electron microscopy (TEM). Although a small subset of samples are to be prepared using a direct procedure, the majority of samples analyzed using this method wil...

Ground-water-quality and ground-water-level data, Bernalillo County, central New Mexico, 1990-1993

USGS Publications Warehouse

Kues, G.E.; Garcia, B.M.

1995-01-01

Ground-water-quality and ground-water-level data were collected in four unincorporated areas of Bernalillo County during 1990-93. Twenty wells in the east mountain area of Bernalillo County were sampled approximately monthly between January 1990 and June 1993. The water samples were analyzed for concentrations of chloride and selected nutrient species; many of the samples also were analyzed for concentrations of total organic carbon and dissolved boron and iron. Eleven wells northeast of the city of Albuquerque, 20 wells in the Rio Grande Valley immediately north of Albuquerque, and 30 wells in the Rio Grande Valley immediately south of Albuquerque were sampled once each between December 1992 and September 1993; all water samples were analyzed for chloride and selected nutrient species, and selected samples from wells in the north and south valley areas were also analyzed for major dissolved constituents, iron, manganese, and methylene blue active substances. Samples from 10 of the wells in the north and south valley areas were analyzed for 47 selected pesticides. Field measurements of specific conductance, pH, temperature, and alkalinity were made on most samples at the time of sample collection. Water levels also were measured at the time of sample collection when possible. Results of the monthly water-quality and water-level monitoring in the east mountain area of Bernalillo County are presented in graphical form. Water-quality and water-level data collected from the other areas are presented in tabular form.

Quality-assurance data for routine water quality analyses by the U. S. Geological Survey laboratory in Troy, New York; July 1993 through June 1995

USGS Publications Warehouse

Lincoln, Tricia A.; Horan-Ross, Debra A.; McHale, Michael R.; Lawrence, Gregory B.

2001-01-01

A laboratory for analysis of low-ionic strength water has been developed at the U.S. Geological Survey (USGS) office in Troy, N.Y., to analyze samples collected by USGS projects in the Northeast. The laboratory's quality-assurance program is based on internal and interlaboratory quality-assurance samples and quality-control procedures developed to ensure proper sample collection, processing, and analysis. The quality-assurance/quality-control data are stored in the laboratory's SAS data-management system, which provides efficient review, compilation, and plotting of quality-assurance/quality-control data. This report presents and discusses samples analyzed from July 1993 through June 1995. Quality-control results for 18 analytical procedures were evaluated for bias and precision. Control charts show that data from seven of the analytical procedures were biased throughout the analysis period for either high-concentration or low-concentration samples but were within control limits; these procedures were: acid-neutralizing capacity, dissolved inorganic carbon, dissolved organic carbon (soil expulsions), chloride, magnesium, nitrate (colorimetric method), and pH. Three of the analytical procedures were occasionally biased but were within control limits; they were: calcium (high for high-concentration samples for May 1995), dissolved organic carbon (high for highconcentration samples from January through September 1994), and fluoride (high in samples for April and June 1994). No quality-control sample has been developed for the organic monomeric aluminum procedure. Results from the filter-blank and analytical-blank analyses indicate that all analytical procedures in which blanks were run were within control limits, although values for a few blanks were outside the control limits. Blanks were not analyzed for acid-neutralizing capacity, dissolved inorganic carbon, fluoride, nitrate (colorimetric method), or pH. Sampling and analysis precision are evaluated herein in terms of the coefficient of variation obtained for triplicate samples in 14 of the 18 procedures. Data-quality objectives were met by more than 90 percent of the samples analyzed in all procedures except total monomeric aluminum (85 percent of samples met objectives), total aluminum (70 percent of samples met objectives), and dissolved organic carbon (85 percent of samples met objectives). Triplicate samples were not analyzed for ammonium, fluoride, dissolved inorganic carbon, or nitrate (colorimetric method). Results of the USGS interlaboratory Standard Reference Sample Program indicated high data quality with a median result of 3.6 of a possible 4.0. Environment Canada's LRTAP interlaboratory study results indicated that more than 85 percent of the samples met data-quality objectives in 6 of the 12 analyses; exceptions were calcium, dissolved organic carbon, chloride, pH, potassium, and sodium. Data-quality objectives were not met for calcium samples in one LRTAP study, but 94 percent of samples analyzed were within control limits for the remaining studies. Data-quality objectives were not met by 35 percent of samples analyzed for dissolved organic carbon, but 94 percent of sample values were within 20 percent of the most probable value. Data-quality objectives were not met for 30 percent of samples analyzed for chloride, but 90 percent of sample values were within 20 percent of the most probable value. Measurements of samples with a pH above 6.0 were biased high in 54 percent of the samples, although 85 percent of the samples met data-quality objectives for pH measurements below 6.0. Data-quality objectives for potassium and sodium were not met in one study (only 33 percent of the samples analyzed met the objectives), although 85 percent of the sample values were within control limits for the other studies. Measured sodium values were above the upper control limit in all studies. Results from blind reference-sample analyses indicated that data

Job Performance as Multivariate Dynamic Criteria: Experience Sampling and Multiway Component Analysis.

PubMed

Spain, Seth M; Miner, Andrew G; Kroonenberg, Pieter M; Drasgow, Fritz

2010-08-06

Questions about the dynamic processes that drive behavior at work have been the focus of increasing attention in recent years. Models describing behavior at work and research on momentary behavior indicate that substantial variation exists within individuals. This article examines the rationale behind this body of work and explores a method of analyzing momentary work behavior using experience sampling methods. The article also examines a previously unused set of methods for analyzing data produced by experience sampling. These methods are known collectively as multiway component analysis. Two archetypal techniques of multimode factor analysis, the Parallel factor analysis and the Tucker3 models, are used to analyze data from Miner, Glomb, and Hulin's (2010) experience sampling study of work behavior. The efficacy of these techniques for analyzing experience sampling data is discussed as are the substantive multimode component models obtained.

Avian plasma chemistry analysis using diluted samples.

PubMed

Waldoch, Jennifer; Wack, Raymund; Christopher, Mary

2009-12-01

Clinical chemistry tests are essential for the diagnosis and monitoring of disease in birds. The small volume of blood that can be obtained from many avian species limits the use of routine in-house chemistry analyzers. The aim of this study was to examine the accuracy and precision of avian plasma chemistry values obtained by use of a benchtop analyzer in samples diluted with sterile water, as compared with undiluted samples. Whole blood samples were collected from 13 clinically healthy thick-billed parrots (Rhynchopsitta pachyrhyncha). The samples were placed in lithium heparin tubes and centrifuged and the plasma decanted. One aliquot was analyzed immediately using a VetScan benchtop analyzer with an avian-reptile-specific rotor that included 12 analytes. The remainder of the plasma was divided into two aliquots and stored at -80 degrees C until analysis. One of these aliquots was diluted 1:1, 1:1.5, 1:2, and 1:2.5 with sterile water to give final dilutions of 1:2, 1:2.5, 1:3, and 1:3.5, respectively. The other aliquot was pooled with the 12 other samples to create a plasma pool. The undiluted plasma pool and two final dilutions (1:2 and 1:3) of the pooled plasma were analyzed in replicate (n = 20) to determine intra- and interassay imprecision. Each dilution was analyzed using the avian-reptile rotor and the results multiplied by the appropriate dilution factor to obtain the final result. Significant differences were observed in clinical chemistry results obtained from diluted plasma samples for all analytes except aspartate aminotransferase, creatine kinase, and glucose. Uric acid concentration was not significantly different at dilutions of up to 1:3. Bile acids, globulins, and sodium concentrations were below the limit of detection in all diluted samples and were not statistically analyzed. Based on these results, dilution with sterile water is not recommended for biochemical analysis of avian plasma using the VetScan benchtop analyzer.

Quality-Assurance Data for Routine Water Analyses by the U.S. Geological Survey Laboratory in Troy, New York--July 1999 through June 2001

USGS Publications Warehouse

Lincoln, Tricia A.; Horan-Ross, Debra A.; McHale, Michael R.; Lawrence, Gregory B.

2006-01-01

The laboratory for analysis of low-ionic-strength water at the U.S. Geological Survey (USGS) Water Science Center in Troy, N.Y., analyzes samples collected by USGS projects throughout the Northeast. The laboratory's quality-assurance program is based on internal and interlaboratory quality-assurance samples and quality-control procedures that were developed to ensure proper sample collection, processing, and analysis. The quality-assurance and quality-control data were stored in the laboratory's LabMaster data-management system, which provides efficient review, compilation, and plotting of data. This report presents and discusses results of quality-assurance and quality-control samples analyzed from July 1999 through June 2001. Results for the quality-control samples for 18 analytical procedures were evaluated for bias and precision. Control charts indicate that data for eight of the analytical procedures were occasionally biased for either high-concentration or low-concentration samples but were within control limits; these procedures were: acid-neutralizing capacity, total monomeric aluminum, total aluminum, calcium, chloride and nitrate (ion chromatography and colormetric method) and sulfate. The total aluminum and dissolved organic carbon procedures were biased throughout the analysis period for the high-concentration sample, but were within control limits. The calcium and specific conductance procedures were biased throughout the analysis period for the low-concentration sample, but were within control limits. The magnesium procedure was biased for the high-concentration and low concentration samples, but was within control limits. Results from the filter-blank and analytical-blank analyses indicate that the procedures for 14 of 15 analytes were within control limits, although the concentrations for blanks were occasionally outside the control limits. The data-quality objective was not met for dissolved organic carbon. Sampling and analysis precision are evaluated herein in terms of the coefficient of variation obtained for triplicate samples in the procedures for 17 of the 18 analytes. At least 90 percent of the samples met data-quality objectives for all analytes except ammonium (81 percent of samples met objectives), chloride (75 percent of samples met objectives), and sodium (86 percent of samples met objectives). Results of the USGS interlaboratory Standard Reference Sample (SRS) Project indicated good data quality over the time period, with most ratings for each sample in the good to excellent range. The P-sample (low-ionic-strength constituents) analysis had one satisfactory rating for the specific conductance procedure in one study. The T-sample (trace constituents) analysis had one satisfactory rating for the aluminum procedure in one study and one unsatisfactory rating for the sodium procedure in another. The remainder of the samples had good or excellent ratings for each study. Results of Environment Canada's National Water Research Institute (NWRI) program indicated that at least 89 percent of the samples met data-quality objectives for 10 of the 14 analytes; the exceptions were ammonium, total aluminum, dissolved organic carbon, and sodium. Results indicate a positive bias for the ammonium procedure in all studies. Data-quality objectives were not met in 50 percent of samples analyzed for total aluminum, 38 percent of samples analyzed for dissolved organic carbon, and 27 percent of samples analyzed for sodium. Results from blind reference-sample analyses indicated that data-quality objectives were met by at least 91 percent of the samples analyzed for calcium, chloride, fluoride, magnesium, pH, potassium, and sulfate. Data-quality objectives were met by 75 percent of the samples analyzed for sodium and 58 percent of the samples analyzed for specific conductance.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gardiner, W.W.; Barrows, E.S.; Antrim, L.D

Buttermilk Channel was one of seven waterways that was sampled and evaluated for dredging and sediment disposal. Sediment samples were collected and analyses were conducted on sediment core samples. The evaluation of proposed dredged material from the channel included bulk sediment chemical analyses, chemical analyses of site water and elutriate, water column and benthic acute toxicity tests, and bioaccumulation studies. Individual sediment core samples were analyzed for grain size, moisture content, and total organic carbon. A composite sediment samples, representing the entire area proposed for dredging, was analyzed for bulk density, polynuclear aromatic hydrocarbons, and 1,4-dichlorobenzene. Site water and elutriatemore » were analyzed for metals, pesticides, and PCBs.« less

Evaluation of an in-practice wet-chemistry analyzer using canine and feline serum samples.

PubMed

Irvine, Katherine L; Burt, Kay; Papasouliotis, Kostas

2016-01-01

A wet-chemistry biochemical analyzer was assessed for in-practice veterinary use. Its small size may mean a cost-effective method for low-throughput in-house biochemical analyses for first-opinion practice. The objectives of our study were to determine imprecision, total observed error, and acceptability of the analyzer for measurement of common canine and feline serum analytes, and to compare clinical sample results to those from a commercial reference analyzer. Imprecision was determined by within- and between-run repeatability for canine and feline pooled samples, and manufacturer-supplied quality control material (QCM). Total observed error (TEobs) was determined for pooled samples and QCM. Performance was assessed for canine and feline pooled samples by sigma metric determination. Agreement and errors between the in-practice and reference analyzers were determined for canine and feline clinical samples by Bland-Altman and Deming regression analyses. Within- and between-run precision was high for most analytes, and TEobs(%) was mostly lower than total allowable error. Performance based on sigma metrics was good (σ > 4) for many analytes and marginal (σ > 3) for most of the remainder. Correlation between the analyzers was very high for most canine analytes and high for most feline analytes. Between-analyzer bias was generally attributed to high constant error. The in-practice analyzer showed good overall performance, with only calcium and phosphate analyses identified as significantly problematic. Agreement for most analytes was insufficient for transposition of reference intervals, and we recommend that in-practice-specific reference intervals be established in the laboratory. © 2015 The Author(s).

Occurrence and estimation of pesticide residues in edible minor crops in southeastern Poland in 2013-2014.

PubMed

Podbielska, Magdalena; Szpyrka, Ewa; Matyaszek, Aneta; Słowik-Borowiec, Magdalena; Rupar, Julian; Kurdziel, Anna

2016-07-01

This paper presents the results of official control of pesticide residues in minor crops collected in southeastern Poland in 2013-2014. Compliance of used pesticides with applicable law was also verified, and determined residues were compared to maximum residue levels (MRLs) provided for in Regulation (EC) No. 395/2005. A total of 583 samples of 25 different types of fresh fruit and vegetables were analyzed for pesticide residues. Pesticide residues were detected in 158 samples (27.1 % of the analyzed samples). According to the European Commission Health & Consumer Protection Directorate-General (SANCO) guidelines document, MRL violations were understood as cases where a residue level exceeded the MRL after the uncertainty of the method (50 %) was considered. MRL violations were found in four samples. The usage of unauthorized pesticides was detected in 5.8 % of analyzed samples. Substances banned in Poland were found in two samples. Fungicides were the most frequently detected group of pesticides. Pesticide residues were most commonly found in fruit samples (19.4 % of all analyzed samples), mainly in gooseberry, redcurrant, and huckleberry. The majority of samples were compliant with MRLs, which means that they were suitable for trade.

40 CFR 86.109-94 - Exhaust gas sampling system; Otto-cycle vehicles not requiring particulate emission measurements.

Code of Federal Regulations, 2013 CFR

2013-07-01

... detection for the HPLC analyzer. Sampling systems for all phases shall be identical. (iii) The methanol and... detection for the HPLC analyzer. Sampling systems for all phases shall be identical. (iii) The methanol and...

40 CFR 86.109-94 - Exhaust gas sampling system; Otto-cycle vehicles not requiring particulate emission measurements.

Code of Federal Regulations, 2012 CFR

2012-07-01

... detection for the HPLC analyzer. Sampling systems for all phases shall be identical. (iii) The methanol and... detection for the HPLC analyzer. Sampling systems for all phases shall be identical. (iii) The methanol and...

40 CFR 86.109-94 - Exhaust gas sampling system; Otto-cycle vehicles not requiring particulate emission measurements.

Code of Federal Regulations, 2014 CFR

2014-07-01

... detection for the HPLC analyzer. Sampling systems for all phases shall be identical. (iii) The methanol and... detection for the HPLC analyzer. Sampling systems for all phases shall be identical. (iii) The methanol and...

Methods of analyzing crude oil

DOE Office of Scientific and Technical Information (OSTI.GOV)

Cooks, Robert Graham; Jjunju, Fred Paul Mark; Li, Anyin

The invention generally relates to methods of analyzing crude oil. In certain embodiments, methods of the invention involve obtaining a crude oil sample, and subjecting the crude oil sample to mass spectrometry analysis. In certain embodiments, the method is performed without any sample pre-purification steps.

Methods for making nucleotide probes for sequencing and synthesis

DOEpatents

Church, George M; Zhang, Kun; Chou, Joseph

2014-07-08

Compositions and methods for making a plurality of probes for analyzing a plurality of nucleic acid samples are provided. Compositions and methods for analyzing a plurality of nucleic acid samples to obtain sequence information in each nucleic acid sample are also provided.

Feasibility of processing the experimental breeder reactor-II driver fuel from the Idaho National Laboratory through Savannah River Site's H-Canyon facility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Magoulas, V. E.

Savannah River National Laboratory (SRNL) was requested to evaluate the potential to receive and process the Idaho National Laboratory (INL) uranium (U) recovered from the Experimental Breeder Reactor II (EBR-II) driver fuel through the Savannah River Site’s (SRS) H-Canyon as a way to disposition the material. INL recovers the uranium from the sodium bonded metallic fuel irradiated in the EBR-II reactor using an electrorefining process. There were two compositions of EBR-II driver fuel. The early generation fuel was U-5Fs, which consisted of 95% U metal alloyed with 5% noble metal elements “fissium” (2.5% molybdenum, 2.0% ruthenium, 0.3% rhodium, 0.1% palladium,more » and 0.1% zirconium), while the later generation was U-10Zr which was 90% U metal alloyed with 10% zirconium. A potential concern during the H-Canyon nitric acid dissolution process of the U metal containing zirconium (Zr) is the explosive behavior that has been reported for alloys of these materials. For this reason, this evaluation was focused on the ability to process the lower Zr content materials, the U-5Fs material.« less

Radionuclide field lysimeter experiment (RadFLEx): geochemical and hydrological data for SRS performance assessments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kaplan, D.; Powell, B.; Barber, K.

The SRNL Radiological Field Lysimeter Experiment (RadFLEx) is a one-of-a-kind test bed facility designed to study radionuclide geochemical processes in the Savannah River Site (SRS) vadose zone at a larger spatial scale (from grams to tens of kilograms of sediment) and temporal scale (from months to decade) than is readily afforded through laboratory studies. RadFLEx is a decade-long project that was initiated on July 5, 2012 and is funded by six different sources. The objective of this status report is as follows: 1) to report findings to date that have an impact on SRS performance assessment (PA) calculations, and 2)more » to provide performance metrics of the RadFLEx program. The PA results are focused on measurements of transport parameters, such as distribution coefficients (Kd values), solubility, and unsaturated flow values. As this is an interim report, additional information from subsequent research may influence our interpretation of current results. Research related to basic understanding of radionuclide geochemistry in these vadose zone soils and other source terms are not described here but are referenced for the interested reader.« less

In-situ gamma-ray assay of the west cell line in the 235-F plutonium fuel form facility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Couture, A. H.; Diprete, D.

On August 29th, 2013, scientists from SRNL took a series of in-situ gamma-ray measurements in the maintenance trench beneath Cells 6-9 on the west line of the PuFF facility using an uncollimated, highpurity germanium detector. The detector efficiency was estimated using a combination of MCNP simulations and empirical measurements. Data analysis was performed using three gamma-rays emitted by Pu-238 (99.85 keV, 152.7 keV, and 766.4 keV) providing three independent estimates of the mass of Pu-238 holdup in each of the cells. The weighted mean of these three results was used as the best estimate of Pu-238 holdup in the Westmore » Cell Line of PuFF. The results of the assay measurements are found in the table below along with the results from the scoping assay performed in 2006. All uncertainties in this table (as well as the rest of the report) are given as 1σ. The total holdup in the West Cell Line was 2.4 ± 0.7 grams. This result is 0.6 g higher than the previous estimate, a 0.4σ difference.« less

Evaluation of quartz melt rate furnace with the nitric-glycolic flowsheet

DOE Office of Scientific and Technical Information (OSTI.GOV)

Williams, M. S.; Miller, D. H.

The Savannah River National Laboratory (SRNL) was tasked to support validation of the Defense Waste Processing Facility (DWPF) melter offgas flammability model for the Nitric-Glycolic (NG) flowsheet. The work is supplemental to the Cold Cap Evaluation Furnace (CEF) testing conducted in 20141 and the Slurry-fed Melt Rate Furnace (SMRF) testing conducted in 20162 that supported Deliverable 4 of the DWPF & Saltstone Facility Engineering Technical Task Request (TTR).3 The Quartz Melt Rate Furnace (QMRF) was evaluated as a bench-scale scoping tool to potentially be used in lieu of or simply prior to the use of the larger-scale SMRF or CEF.more » The QMRF platform has been used previously to evaluate melt rate behavior and offgas compositions of DWPF glasses prepared from the Nitric-Formic (NF) flowsheet but not for the NG flowsheet and not with continuous feeding.4 The overall objective of the 2016-2017 testing was to evaluate the efficacy of the QMRF as a lab-scale platform for steady state, continuously fed melter testing with the NG flowsheet as an alternative to more expensive and complex testing with the SMRF or CEF platforms.« less

TESTING OF TMR SAND MANTIS FINAL REPORT

DOE Office of Scientific and Technical Information (OSTI.GOV)

Krementz, D; William Daugherty, W

2007-06-12

Screening tests of Sand Mantis candidate materials selected for erosion resistance have been completed. The results of this testing identified that over a relatively short period of operation (<1 hour), measurable erosion will occur in each of the candidate zoom tube materials given equal operating exposure. Additionally, this testing has shown that erosion of the rubber discharge hose directly downstream of the vehicle could be expected to limit the service life of the discharge hose. On the basis of these test results, SRNL recommends the following; {lg_bullet} redesign of critical system components (e.g., zoom tube, discharge hose) should be conductedmore » to improve system characteristics relative to erosion and capitalize on the results of this testing, {lg_bullet} continued efforts to deploy the Sand Mantis should include testing to better define and optimize operating parameters, and gain an understanding of system dynamics, {lg_bullet} discontinue wear testing with the selected materials pending redesign of critical system components (1st recommendation) and inclusion of other candidate materials. The final selection of additional candidate materials should be made following design changes, but might include a Stellite alloy or zirconia.« less

Ni and Cr addition to alloy waste forms to reduce radionuclide environmental releases

DOE Office of Scientific and Technical Information (OSTI.GOV)

Olson, L.

2016-10-11

Reference alloy waste forms (RAW) were fabricated and underwent hybrid corrosion/immersion testing to parameterize the ANL analytical oxidative-dissolution model to enable the calculation of fractional release rates and to determine the effectiveness of Ni and Cr trim additions in reducing release rates of radionuclide surrogates. Figure 1 shows the prototypical multiphase microstructure of the alloys with each phase type contributing about equally to the exposed surface area. The waste forms tested at SRNL were variations of the RAW-6 formulation that uses HT9 as the main alloy component, and are meant to enable evaluation of the impact of Ni and Crmore » trim additions on the release rates of actinides and Tc-99. The test solutions were deaerated alkaline and acidic brines, ranging in pH 3 to pH 10, representing potential repositories with those conditions. The testing approach consisted of 4 major steps; 1) bare surface corrosion measurements at pH values of 3, 5, 8, and 10, 2) hybrid potentiostatic hold/exposure measurements at pH 3, 3) measurement of radionuclide concentrations and relations to anodic current from potentiostatic holds, and 4) identification of corroding phases using SEM/EDS of electrodes.« less

Letter report on PCT/Monolith glass ceramic corrosion tests

DOE Office of Scientific and Technical Information (OSTI.GOV)

Crawford, Charles L.

2015-09-24

The Savannah River National Laboratory (SRNL) is collaborating with personnel from Pacific Northwest National Laboratory (PNNL) to study advanced waste form glass ceramics for immobilization of waste from Used Nuclear Fuel (UNF) separations processes. The glass ceramic waste forms take advantage of both crystalline and glassy phases where ‘troublesome’ elements (e.g., low solubility in glass or very long-lived) partition to highly durable ceramic phases with the remainder of elements residing in the glassy phase. The ceramic phases are tailored to create certain minerals or unique crystalline structures that can host the radionuclides by binding them in their specific crystalline networkmore » while not adversely impacting the residual glass network (Crum et al., 2011). Glass ceramics have been demonstrated using a scaled melter test performed in a pilot scale (1/4 scale) cold crucible induction melter (CCIM) (Crum et al., 2014; Maio et al., 2015). This report summarizes recent results from both Phase I and Phase II bench scale tests involving crucible fabrication and corrosion testing of glass ceramics using the Product Consistency Test (PCT). Preliminary results from both Phase I and Phase II bench scale tests involving statistically designed matrices have previously been reported (Crawford, 2013; Crawford, 2014).« less

Systems and methods for sample analysis

DOEpatents

Cooks, Robert Graham; Li, Guangtao; Li, Xin; Ouyang, Zheng

2015-01-13

The invention generally relates to systems and methods for sample analysis. In certain embodiments, the invention provides a system for analyzing a sample that includes a probe including a material connected to a high voltage source, a device for generating a heated gas, and a mass analyzer.

Atmospheric sampling glow discharge ionization source

DOEpatents

McLuckey, S.A.; Glish, G.L.

1989-07-18

An atmospheric sampling glow discharge ionization source that can be used in combination with an analytical instrument which operates at high vacuum, such as a mass spectrometer. The atmospheric sampling glow discharge ionization source comprises a chamber with at least one pair of electrodes disposed therein, an inlet for a gaseous sample to be analyzed and an outlet communicating with an analyzer which operates at subatmospheric pressure. The ionization chamber is maintained at a pressure below atmospheric pressure, and a voltage difference is applied across the electrodes to induce a glow discharge between the electrodes, so that molecules passing through the inlet are ionized by the glow discharge and directed into the analyzer. The ionization source accepts the sample under atmospheric pressure conditions and processes it directly into the high vacuum instrument, bridging the pressure gap and drawing off unwanted atmospheric gases. The invention also includes a method for analyzing a gaseous sample using the glow discharge ionization source described above. 3 figs.

Integrated system for gathering, processing, and reporting data relating to site contamination

DOEpatents

Long, D.D.; Goldberg, M.S.; Baker, L.A.

1997-11-11

An integrated screening system comprises an intrusive sampling subsystem, a field mobile laboratory subsystem, a computer assisted design/geographical information subsystem, and a telecommunication linkup subsystem, all integrated to provide synergistically improved data relating to the extent of site soil/groundwater contamination. According to the present invention, data samples related to the soil, groundwater or other contamination of the subsurface material are gathered and analyzed to measure contaminants. Based on the location of origin of the samples in three-dimensional space, the analyzed data are transmitted to a location display. The data from analyzing samples and the data from the locating the origin are managed to project the next probable sample location. The next probable sample location is then forwarded for use as a guide in the placement of ensuing sample location, whereby the number of samples needed to accurately characterize the site is minimized. 10 figs.

Integrated system for gathering, processing, and reporting data relating to site contamination

DOEpatents

Long, Delmar D.; Goldberg, Mitchell S.; Baker, Lorie A.

1997-01-01

An integrated screening system comprises an intrusive sampling subsystem, a field mobile laboratory subsystem, a computer assisted design/geographical information subsystem, and a telecommunication linkup subsystem, all integrated to provide synergistically improved data relating to the extent of site soil/groundwater contamination. According to the present invention, data samples related to the soil, groundwater or other contamination of the subsurface material are gathered and analyzed to measure contaminants. Based on the location of origin of the samples in three-dimensional space, the analyzed data are transmitted to a location display. The data from analyzing samples and the data from the locating the origin are managed to project the next probable sample location. The next probable sample location is then forwarded for use as a guide in the placement of ensuing sample location, whereby the number of samples needed to accurately characterize the site is minimized.

Atomic force microscope with combined FTIR-Raman spectroscopy having a micro thermal analyzer

DOEpatents

Fink, Samuel D [Aiken, SC; Fondeur, Fernando F [North Augusta, SC

2011-10-18

An atomic force microscope is provided that includes a micro thermal analyzer with a tip. The micro thermal analyzer is configured for obtaining topographical data from a sample. A raman spectrometer is included and is configured for use in obtaining chemical data from the sample.

40 CFR 86.135-90 - Dynamometer procedure.

Code of Federal Regulations, 2014 CFR

2014-07-01

... petroleum gas-fueled Otto-cycle vehicles, the composite samples collected in bags are analyzed for THC, CO..., liquefied petroleum gas-fueled and methanol-fueled diesel-cycle vehicles), THC is sampled and analyzed... analyzed for THC, CO, CO2, CH4, and NOX. (3) For natural gas-fueled, liquefied petroleum gas-fueled and...

Compilation of data on the uranium and equivalent uranium content of samples analyzed by U.S. Geological Survey during a program of sampling mine, mill, and smelter products

USGS Publications Warehouse

Hall, Marlene Louise; Butler, Arthur Pierce

1952-01-01

In 1942 the Geological Survey began to collect, in response to a request made by the War Production Board, samples of mine, mill, and smelter products. About 1,400 such samples were collected and analyzed spectrographically for about 20 elements that were of strategic importance, in order to determine whether any of the products analyzed might be possible sources of some of the needed elements. When attention was directed to radioactive elements in 1943, most of the samples were scanned for radioactivity. Part of the work was done on behalf of the Division of Raw Materials of the Atomic Energy Commission. The sources, mine mill, smelter, or prospect, from which these samples were collected, the kind of material sampled, i.e. ores, concentrates, middlings, tailings, flue dusts, and so forth, and the radioactivity of the samples are listed in this report. Samples of the materials collected in the course of the Geological Survey’s investigations for uranium are excluded, but about 500 such samples were analyzed spectrographically for some or all of the same 20 elements sought in the samples that are the subject of this report. Most of the samples were tested only for their radioactivity, but a few were analyzed chemically for uranium. The radioactivity of many of the samples tested in the early screening was determined only qualitatively. Several samples were tested at one time, and if the count obtained did not exceed a predetermined minimum above background, the samples were not tested individually. If the count was more than this minimum, the samples were tested individually to identify the radioactive sample or samples and to obtain a quantitative value for the radioactivity. In general, the rough screening served as a basis for separating samples in which the radioactivity amount to less than 0.003 percent equivalent uranium from those in which it exceeded that amount. Some aspects of various phases of the investigation of radioactivity in these samples have been reported in various other reports, as follows.

Radionuclides, inorganic constitutents, organic compounds, and bacteria in water from selected wells and springs from the southern boundary of the Idaho National Engineering Laboratory to the Hagerman Area, Idaho, 1992

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bartholomay, R.C.; Edwards, D.D.; Campbell, L.J.

1994-11-01

The U.S. Geological Survey and the Idaho Department of Water Resources, in response to a request from the U.S. Department of Energy, sampled 18 sites as part of a long-term project to monitor water quality of the Snake River Plain aquifer from the southern boundary of the Idaho National Engineering Laboratory to the Hagerman area. Water samples were collected and analyzed for selected radionuclides, inorganic constituents, organic compounds, and bacteria. The samples were collected from 13 irrigation wells, 1 domestic well, 1 spring, 2 stock wells, and 1 public supply well. Quality assurance samples also were collected and analyzed. Nonemore » of the samples analyzed for radionuclides, inorganic constituents, or organic compounds exceeded the established maximum contaminant levels for drinking water. Most of the radionuclide and inorganic constituent concentrations exceeded their respective reporting levels. Most of the samples analyzed for surfactants and dissolved organic carbon had concentrations that exceeded their reporting levels. None of the samples contained reportable concentrations of purgeable organic compounds or pesticides. Total coliform bacteria was present in nine samples.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Distler, T. M.; Wong, C. M.

Runoff-water samples for the first, third, and fourth quarters of 1975 were analyzed for pesticide residues at LLL and independently by the LFE Environmental Analysis Laboratories. For the compounds analyzed, upper limits to possible contamination were placed conservatively at the low parts-per-billion level. In addition, soil samples were also analyzed. Future work will continue to include quarterly sampling and will be broadened in scope to include quantitative analysis of a larger number of compounds. A study of recovery efficiency is planned. Because of the high backgrounds on soil samples together with the uncertainties introduced by the cleanup procedures, there ismore » little hope of evaluating the distribution of a complex mixture of pesticides among the aqueous and solid phases in a drainage sample. No further sampling of soil from the streambed is therefore contemplated.« less

SCIX IMPACT ON DWPF CPC

DOE Office of Scientific and Technical Information (OSTI.GOV)

Koopman, D.

2011-07-14

A program was conducted to systematically evaluate potential impacts of the proposed Small Column Ion Exchange (SCIX) process on the Defense Waste Processing Facility (DWPF) Chemical Processing Cell (CPC). The program involved a series of interrelated tasks. Past studies of the impact of crystalline silicotitanate (CST) and monosodium titanate (MST) on DWPF were reviewed. Paper studies and material balance calculations were used to establish reasonable bounding levels of CST and MST in sludge. Following the paper studies, Sludge Batch 10 (SB10) simulant was modified to have both bounding and intermediate levels of MST and ground CST. The SCIX flow sheetmore » includes grinding of the CST which is larger than DWPF frit when not ground. Nominal ground CST was not yet available, therefore a similar CST ground previously in Savannah River National Laboratory (SRNL) was used. It was believed that this CST was over ground and that it would bound the impact of nominal CST on sludge slurry properties. Lab-scale simulations of the DWPF CPC were conducted using SB10 simulants with no, intermediate, and bounding levels of CST and MST. Tests included both the Sludge Receipt and Adjustment Tank (SRAT) and Slurry Mix Evaporator (SME) cycles. Simulations were performed at high and low acid stoichiometry. A demonstration of the extended CPC flowsheet was made that included streams from the site interim salt processing operations. A simulation using irradiated CST and MST was also completed. An extensive set of rheological measurements was made to search for potential adverse consequences of CST and MST and slurry rheology in the CPC. The SCIX CPC impact program was conducted in parallel with a program to evaluate the impact of SCIX on the final DWPF glass waste form and on the DWPF melter throughput. The studies must be considered together when evaluating the full impact of SCIX on DWPF. Due to the fact that the alternant flowsheet for DWPF has not been selected, this study did not consider the impact of proposed future alternative DWPF CPC flowsheets. The impact of the SCIX streams on DWPF processing using the selected flowsheet need to be considered as part of the technical baseline studies for coupled processing with the selected flowsheet. In addition, the downstream impact of aluminum dissolution on waste containing CST and MST has not yet been evaluated. The current baseline would not subject CST to the aluminum dissolution process and technical concerns with performing the dissolution with CST have been expressed. Should this option become feasible, the downstream impact should be considered. The main area of concern for DWPF from aluminum dissolution is an impact on rheology. The SCIX project is planning for SRNL to complete MST, CST, and sludge rheology testing to evaluate any expected changes. The impact of ground CST transport and flush water on the DWPF CPC feed tank (and potential need for decanting) has not been defined or studied.« less

Development of an In-Situ Decommissioning Sensor Network Test Bed for Structural Condition Monitoring - 12156

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zeigler, Kristine E.; Ferguson, Blythe A.

2012-07-01

The Savannah River National Laboratory (SRNL) has established an In Situ Decommissioning (ISD) Sensor Network Test Bed, a unique, small scale, configurable environment, for the assessment of prospective sensors on actual ISD system material, at minimal cost. The Department of Energy (DOE) is presently implementing permanent entombment of contaminated, large nuclear structures via ISD. The ISD end state consists of a grout-filled concrete civil structure within the concrete frame of the original building. Validation of ISD system performance models and verification of actual system conditions can be achieved through the development a system of sensors to monitor the materials andmore » condition of the structure. The ISD Sensor Network Test Bed has been designed and deployed to addresses the DOE-Environmental Management Technology Need to develop a remote monitoring system to determine and verify ISD system performance. Commercial off-the-shelf sensors have been installed on concrete blocks taken from walls of the P Reactor Building at the Savannah River Site. Deployment of this low-cost structural monitoring system provides hands-on experience with sensor networks. The initial sensor system consists of groutable thermistors for temperature and moisture monitoring, strain gauges for crack growth monitoring, tilt-meters for settlement monitoring, and a communication system for data collection. Baseline data and lessons learned from system design and installation and initial field testing will be utilized for future ISD sensor network development and deployment. The Sensor Network Test Bed at SRNL uses COTS sensors on concrete blocks from the outer wall of the P Reactor Building to measure conditions expected to occur in ISD structures. Knowledge and lessons learned gained from installation, testing, and monitoring of the equipment will be applied to sensor installation in a meso-scale test bed at FIU and in future ISD structures. The initial data collected from the sensors installed on the P Reactor Building blocks define the baseline materials condition of the P Reactor ISD external concrete structure. Continued monitoring of the blocks will enable evaluation of the effects of aging on the P Reactor ISD structure. The collected data will support validation of the material degradation model and assessment of the condition of the ISD structure over time. The following are recommendations for continued development of the ISD Sensor Network Test Bed: - Establish a long-term monitoring program using the concrete blocks with existing sensor and/or additional sensors for trending the concrete materials and structural condition; - Continue development of a stand-alone test bed sensor system that is self-powered and provides wireless transmission of data to a user-accessible dashboard; - Develop and implement periodic NDE/DE characterization of the concrete blocks to provide verification and validation for the measurements obtained through the sensor system and concrete degradation model(s). (authors)« less

Major- and trace-element concentrations in rock samples collected in 2004 from the Taylor Mountains 1:250,000-scale quadrangle, Alaska

USGS Publications Warehouse

Klimasauskas, Edward P.; Miller, Marti L.; Bradley, Dwight C.; Karl, Sue M.; Baichtal, James F.; Blodgett, Robert B.

2006-01-01

The Kuskokwim mineral belt of Bundtzen and Miller (1997) forms an important metallogenic region in southwestern Alaska that has yielded more than 3.22 million ounces of gold and 400,000 ounces of silver. Precious-metal and related deposits in this region associated with Late Cretaceous to early Tertiary igneous complexes extend into the Taylor Mountains 1:250,000-scale quadrangle. The U.S. Geological Survey is conducting geologic mapping and a mineral resource assessment of this area that will provide a better understanding of the geologic framework, regional geochemistry, and may provide targets for mineral exploration and development. During the 2004 field season 137 rock samples were collected for a variety of purposes. The 4 digital files accompanying this report reflect the type of analysis performed and its intended purpose and are available for download as an Excel workbook, comma delimited format (*.csv), dBase 4 files (*.dbf) or as point coverages in ArcInfo interchange format (*.e00). Data values are provided in percent, pct (1gram per 100grams), or parts per million, ppm (1gram per 1,000,000grams) per the column heading in the table. All samples were analyzed for a suite of 42 trace-elements (icp42.*) to provide data for use in geochemical exploration as well as some baseline data. Selected samples were analyzed by additional methods; 104 targeted geochemical exploration samples were analyzed for gold, arsenic, and mercury (auashg.*); 21 of these samples were also analyzed to obtain concentrations of 10 loosely bound metals (icp10.*); 33 rock samples were analyzed for major element oxides to support the regional mapping program (reg.*), of which 28 sedimentary rock samples were also analyzed for total carbon, and carbonate carbon.

Discrepant post filter ionized calcium concentrations by common blood gas analyzers in CRRT using regional citrate anticoagulation.

PubMed

Schwarzer, Patrik; Kuhn, Sven-Olaf; Stracke, Sylvia; Gründling, Matthias; Knigge, Stephan; Selleng, Sixten; Helm, Maximilian; Friesecke, Sigrun; Abel, Peter; Kallner, Anders; Nauck, Matthias; Petersmann, Astrid

2015-09-08

Ionized calcium (iCa) concentration is often used in critical care and measured using blood gas analyzers at the point of care. Controlling and adjusting regional citrate anticoagulation (RCA) for continuous renal replacement therapy (CRRT) involves measuring the iCa concentration in two samples: systemic with physiological iCa concentrations and post filter samples with very low iCa concentrations. However, modern blood gas analyzers are optimized for physiological iCa concentrations which might make them less suitable for measuring low iCa in blood with a high concentration of citrate. We present results of iCa measurements from six different blood gas analyzers and the impact on clinical decisions based on the recommendations of the dialysis' device manufacturer. The iCa concentrations of systemic and post filter samples were measured using six distinct, frequently used blood gas analyzers. We obtained iCa results of 74 systemic and 84 post filter samples from patients undergoing RCA for CRRT at the University Medicine of Greifswald. The systemic samples showed concordant results on all analyzers with median iCa concentrations ranging from 1.07 to 1.16 mmol/L. The medians of iCa concentrations for post filter samples ranged from 0.21 to 0.50 mmol/L. Results of >70% of the post filter samples would lead to major differences in decisions regarding citrate flow depending on the instrument used. Measurements of iCa in post filter samples may give misleading information in monitoring the RCA. Recommendations of the dialysis manufacturer need to be revised. Meanwhile, little weight should be given to post filter iCa. Reference methods for low iCa in whole blood containing citrate should be established.

South Carolina Solar Development - Tracking the Effects of Act 236 (2014-2017)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Fox, E.; Edwards, Thomas B.; Drory, Michael D.

Since 2014, the installed solar capacity in South Carolina (SC) has mushroomed from 5.5 megawatts to more than 354 megawatts today. Concurrently, the number of customer-sited, load-centered solar generation was expected to grow from less than 600 statewide to as many over 10,000 today. This growth was the direct result of a landmark state policy initiative, Act 236, passed by the SC General Assembly and signed into law by the Governor in June of 2014. Local policy makers in SC were ill-equipped to handle the onslaught of solar permitting and zoning requests expected by 2021. Similarly, the state’s building inspectors,more » first responders, and tax assessors know little about photovoltaic (PV) technology and best practices. Finally, SC’s workforce and workforce trainers were underprepared to benefit from the tremendous opportunity created by the passage of Act 236. Each of these deficits in knowledge of and preparedness for solar PV translated into higher “soft costs” of installed solar PV in SC. The Savannah River National Laboratory (SRNL), together with almost a dozen electricity stakeholders in the Southeast, has studied the ability of Act 236 to serve as replicable model for solar PV cost reduction. In 2015, this study began with a focus on the effects of Act 236 to offer a unique perspective and understanding of the actual impact of rapidly integrating solar energy into the electric grid. This study would analyze the impact of starting at a solar PV penetration of 0.1% and increasing to over 2%, while expanding access, developing regional specific training and educational materials, and developing datasets to support expanding solar markets. Through targeted tracking and analysis, the team developed a baseline of the current market, identified the major obstacles in soft cost reduction, and cooperatively developed stakeholder-centric strategies. This work has enabled us to directly track and report on the growth and effects of recently enacted solar legislation on the industry. This report marks the final in a series of reports examining the effects of Act 236 on the solar economy in SC since 2014.« less

TRIPLICATE SODIUM IODIDE GAMMA RAY MONITORS FOR THE SMALL COLUMN ION EXCHANGE PROGRAM

DOE Office of Scientific and Technical Information (OSTI.GOV)

Couture, A.

2011-09-20

This technical report contains recommendations from the Analytical Development (AD) organization of the Savannah River National Laboratory (SRNL) for a system of triplicate Sodium Iodide (NaI) detectors to be used to monitor Cesium-137 ({sup 137}Cs) content of the Decontaminated Salt Solution (DSS) output of the Small Column Ion Exchange (SCIX) process. These detectors need to be gain stabilized with respect to temperature shifts since they will be installed on top of Tank 41 at the Savannah River Site (SRS). This will be accomplished using NaI crystals doped with the alpha-emitting isotope, Americium-241({sup 241}Am). Two energy regions of the detector outputmore » will be monitored using single-channel analyzers (SCAs), the {sup 137}Cs full-energy {gamma}-ray peak and the {sup 241}Am alpha peak. The count rate in the gamma peak region will be proportional to the {sup 137}Cs content in the DSS output. The constant rate of alpha decay in the NaI crystal will be monitored and used as feedback to adjust the high voltage supply to the detector in response to temperature variation. An analysis of theoretical {sup 137}Cs breakthrough curves was used to estimate the gamma activity expected in the DSS output during a single iteration of the process. Count rates arising from the DSS and background sources were predicted using Microshield modeling software. The current plan for shielding the detectors within an enclosure with four-inch thick steel walls should allow the detectors to operate with the sensitivity required to perform these measurements. Calibration, testing, and maintenance requirements for the detector system are outlined as well. The purpose of SCIX is to remove and concentrate high-level radioisotopes from SRS salt waste resulting in two waste streams. The concentrated high-level waste containing {sup 137}Cs will be sent to the Defense Waste Processing Facility (DWPF) for vitrification and the low-level DSS will be sent to the Saltstone Production Facility (SPF) to be incorporated into grout.« less

40 CFR 86.135-94 - Dynamometer procedure.

Code of Federal Regulations, 2011 CFR

2011-07-01

... in bags are analyzed for THC, CO, CO2, CH4 and NOX. For petroleum-fueled diesel-cycle vehicles...), THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel samples of the dilution air are similarly analyzed for THC, CO, CO2, CH4 and NOX. For natural gas-fueled...

40 CFR 86.135-94 - Dynamometer procedure.

Code of Federal Regulations, 2010 CFR

2010-07-01

... in bags are analyzed for THC, CO, CO2, CH4 and NOX. For petroleum-fueled diesel-cycle vehicles...), THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel samples of the dilution air are similarly analyzed for THC, CO, CO2, CH4 and NOX. For natural gas-fueled...

40 CFR 86.135-94 - Dynamometer procedure.

Code of Federal Regulations, 2013 CFR

2013-07-01

... in bags are analyzed for THC, CO, CO2, CH4 and NOX. For petroleum-fueled diesel-cycle vehicles...), THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel samples of the dilution air are similarly analyzed for THC, CO, CO2, CH4 and NOX. For natural gas-fueled...

40 CFR 86.135-94 - Dynamometer procedure.

Code of Federal Regulations, 2012 CFR

2012-07-01

... in bags are analyzed for THC, CO, CO2, CH4 and NOX. For petroleum-fueled diesel-cycle vehicles...), THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel samples of the dilution air are similarly analyzed for THC, CO, CO2, CH4 and NOX. For natural gas-fueled...

Atmospheric Carbon Dioxide Record from In Situ Measurements at Baring Head (1970 - 1993)

DOE Data Explorer

Manning, M. R. [National Institute of Water and Atmospheric Research, Ltd., Lower Hutt, New Zealand; Gomez, A. J. [National Institute of Water and Atmospheric Research, Ltd., Lower Hutt, New Zealand; Pohl, K. P. [National Institute of Water and Atmospheric Research, Ltd. Lower Hutt, New Zealand

1994-01-01

Determinations of atmospheric CO2 mixing ratios are made using a Siemens Ultramat-3 nondispersive infrared (NDIR) gas analyzer. The NDIR CO2 analyzer is connected via a gas manifold consisting of stainless steel tubing and computer-controlled solenoid switches to 12 gas cylinders and 2 sample air lines. The NDIR analyzer compares ambient air CO2 mixing ratios relative to known CO2 mixing ratios in tanks of compressed reference gases. The analyzer operates in a differential mode, with a "zero" reference gas of CO2 mixing ratio 20 to 30 parts per million (ppm) below ambient air CO2 levels flowing continuously through one cell of the analyzer at ~10 mL/min. When atmospheric CO2 is measured, a diaphragm pump pulls air through a sampling line at ~5 L/min. A small fraction of this (180 mL/min) is dried cryogenically to a temperature of approximately ¬70° Celsius and passed through the sample cell of the CO2 analyzer. Both the "zero" and sample gas are exhausted into the observatory building.

Interlaboratory comparison of extraction efficiency of pesticides from surface and laboratory water using solid-phase extraction disks.

PubMed

Senseman, Scott A; Mueller, Thomas C; Riley, Melissa B; Wauchope, R Don; Clegg, Chris; Young, Roddy W; Southwick, Lloyd M; Moye, H Anson; Dumas, Jose A; Mersie, Wondi; Mattice, John D; Leidy, Ross B

2003-06-18

A continuation of an earlier interlaboratory comparison was conducted (1) to assess solid-phase extraction (SPE) using Empore disks to extract atrazine, bromacil, metolachlor, and chlorpyrifos from various water sources accompanied by different sample shipping and quantitative techniques and (2) to compare quantitative results of individual laboratories with results of one common laboratory. Three replicates of a composite surface water (SW) sample were fortified with the analytes along with three replicates of deionized water (DW). A nonfortified DW sample and a nonfortified SW sample were also extracted. All samples were extracted using Empore C(18) disks. After extraction, part of the samples were eluted and analyzed in-house. Duplicate samples were evaporated in a 2-mL vial, shipped dry to a central laboratory (SDC), redissolved, and analyzed. Overall, samples analyzed in-house had higher recoveries than SDC samples. Laboratory x analysis type and laboratory x water source interactions were significant for all four compounds. Seven laboratories participated in this interlaboratory comparison program. No differences in atrazine recoveries were observed from in-house samples analyzed by laboratories A, B, D, and G compared with the recovery of SDC samples. In-house atrazine recoveries from laboratories C and F were higher when compared with recovery from SDC samples. However, laboratory E had lower recoveries from in-house samples compared with SDC samples. For each laboratory, lower recoveries were observed for chlorpyrifos from the SDC samples compared with samples analyzed in-house. Bromacil recovery was <65% at two of the seven laboratories in the study. Bromacil recoveries for the remaining laboratories were >75%. Three laboratories showed no differences in metolachlor recovery; two laboratories had higher recoveries for samples analyzed in-house, and two other laboratories showed higher metolachlor recovery for SDC samples. Laboratory G had a higher recovery in SW for all four compounds compared with DW. Other laboratories that had significant differences in pesticide recovery between the two water sources showed higher recovery in DW than in the SW regardless of the compound. In comparison to earlier work, recovery of these compounds using SPE disks as a temporary storage matrix may be more effective than shipping dried samples in a vial. Problems with analytes such as chlorpyrifos are unavoidable, and it should not be assumed that an extraction procedure using SPE disks will be adequate for all compounds and transferrable across all chromatographic conditions.

In-situ continuous water analyzing module

DOEpatents

Thompson, Cyril V.; Wise, Marcus B.

1998-01-01

An in-situ continuous liquid analyzing system for continuously analyzing volatile components contained in a water source comprises: a carrier gas supply, an extraction container and a mass spectrometer. The carrier gas supply continuously supplies the carrier gas to the extraction container and is mixed with a water sample that is continuously drawn into the extraction container. The carrier gas continuously extracts the volatile components out of the water sample. The water sample is returned to the water source after the volatile components are extracted from it. The extracted volatile components and the carrier gas are delivered continuously to the mass spectometer and the volatile components are continuously analyzed by the mass spectrometer.

Dynamic multistation photometer

DOEpatents

Bauer, Martin L.; Johnson, Wayne F.; Lakomy, Dale G.

1977-01-01

A portable fast analyzer is provided that uses a magnetic clutch/brake to rapidly accelerate the analyzer rotor, and employs a microprocessor for automatic analyzer operation. The rotor is held stationary while the drive motor is run up to speed. When it is desired to mix the sample(s) and reagent(s), the brake is deenergized and the clutch is energized wherein the rotor is very rapidly accelerated to the running speed. The parallel path rotor that is used allows the samples and reagents to be mixed the moment they are spun out into the rotor cuvetes and data acquisition begins immediately. The analyzer will thus have special utility for fast reactions.

Elemental analysis using temporal gating of a pulsed neutron generator

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mitra, Sudeep

Technologies related to determining elemental composition of a sample that comprises fissile material are described herein. In a general embodiment, a pulsed neutron generator periodically emits bursts of neutrons, and is synchronized with an analyzer circuit. The bursts of neutrons are used to interrogate the sample, and the sample outputs gamma rays based upon the neutrons impacting the sample. A detector outputs pulses based upon the gamma rays impinging upon the material of the detector, and the analyzer circuit assigns the pulses to temporally-based bins based upon the analyzer circuit being synchronized with the pulsed neutron generator. A computing devicemore » outputs data that is indicative of elemental composition of the sample based upon the binned pulses.« less

Rainfall, Discharge, and Water-Quality Data During Stormwater Monitoring, July 1, 2007, to June 30, 2008; Halawa Stream Drainage Basin and the H-1 Storm Drain, Oahu, Hawaii

USGS Publications Warehouse

Presley, Todd K.; Jamison, Marcael T.J.; Young, Stacie T.M.

2008-01-01

Storm runoff water-quality samples were collected as part of the State of Hawaii Department of Transportation Stormwater Monitoring Program. The program is designed to assess the effects of highway runoff and urban runoff on Halawa Stream and to assess the effects from the H-1 storm drain on Manoa Stream. For this program, rainfall data were collected at three stations, continuous discharge data at four stations, and water-quality data at six stations, which include the four continuous discharge stations. This report summarizes rainfall, discharge, and water-quality data collected between July 1, 2007, and June 30, 2008. A total of 16 environmental samples were collected over two storms during July 1, 2007, to June 30, 2008, within the Halawa Stream drainage area. Samples were analyzed for total suspended solids, total dissolved solids, nutrients, chemical oxygen demand, and selected trace metals (cadmium, chromium, copper, lead, and zinc). Additionally, grab samples were analyzed for oil and grease, total petroleum hydrocarbons, fecal coliform, and biological oxygen demand. Some samples were analyzed for only a partial list of these analytes because an insufficient volume of sample was collected by the automatic samplers. Three additional quality-assurance/quality-control samples were collected concurrently with the storm samples. A total of 16 environmental samples were collected over four storms during July 1, 2007, to June 30, 2008 at the H-1 Storm Drain. All samples at this site were collected using an automatic sampler. Samples generally were analyzed for total suspended solids, nutrients, chemical oxygen demand, oil and grease, total petroleum hydrocarbons, and selected trace metals (cadmium, chromium, copper, lead, nickel, and zinc), although some samples were analyzed for only a partial list of these analytes. During the storm of January 29, 2008, 10 discrete samples were collected. Varying constituent concentrations were detected for the samples collected at different times during this storm event. Two quality-assurance/quality-control samples were collected concurrently with the storm samples. Three additional quality-assurance/quality-control samples were collected during routine sampler maintenance to check the effectiveness of equipment-cleaning procedures.

Evaluation of automated enzyme immunoassays for five anticonvulsants and theophylline adapted to a centrifugal analyzer.

PubMed

Urquhart, N; Godolphin, W; Campbell, D J

1979-05-01

We report a clinical evaluation of the enzyme immunoassay (EMIT) performed with the GEMSAEC centrifugal analyzer as compared to gas-liquid and liquid chromatography for anticonvulsant drugs and theophylline, respectively. A good correlation was obtained for all drugs, although some difficulties were experienced with one lot of reagent for ethosuximide. The analyzer has an economic advantage if many samples are being analyzed for few drugs in each sample.

Chemicals of emerging concern in water and bottom sediment in the Great Lakes Basin, 2012: collection methods, analytical methods, quality assurance, and study data

USGS Publications Warehouse

Lee, Kathy E.; Langer, Susan K.; Menheer, Michael A.; Hansen, Donald S.; Foreman, William T.; Furlong, Edward T.; Jorgenson, Zachary G.; Choy, Steven J.; Moore, Jeremy N.; Banda, JoAnn; Gefell, Daniel J.

2015-01-01

During this study, 53 environmental samples, 4 field duplicate samples, and 8 field spike samples of bottom sediment and laboratory matrix-spike samples were analyzed for a wide variety of CECs at the USGS National Water Quality Laboratory using laboratory schedule 5433 for wastewater indicators; research method 6434 for steroid hormones, sterols, and bisphenol A; and research method 9008 for human-use pharmaceuticals and antidepressants. Forty of the 57 chemicals analyzed using laboratory schedule 5433 had detectable concentrations ranging from 1 to 49,000 micrograms per kilogram. Fourteen of the 20 chemicals analyzed using research method 6434 had detectable concentrations ranging from 0.04 to 24,940 nanograms per gram. Ten of the 20 chemicals analyzed using research method 9008 had detectable concentrations ranging from 0.59 to 197.5 micrograms per kilogram. Five of the 11 chemicals analyzed using research method 9008 had detectable concentrations ranging from 1.16 to 25.0 micrograms per kilogram.

3013/9975 Surveillance Program Interim Summary Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dunn, K.; Hackney, B.; McClard, J.

2011-06-22

The K-Area Materials Storage (KAMS) Documented Safety Analysis (DSA) requires a surveillance program to monitor the safety performance of 3013 containers and 9975 shipping packages stored in KAMS. The SRS surveillance program [Reference 1] outlines activities for field surveillance and laboratory tests that demonstrate the packages meet the functional performance requirements described in the DSA. The SRS program also supports the complexwide Integrated Surveillance Program (ISP) [Reference 2] for 3013 containers. The purpose of this report is to provide a summary of the SRS portion of the surveillance program activities through fiscal year 2010 (FY10) and formally communicate the interpretationmore » of these results by the Surveillance Program Authority (SPA). Surveillance for the initial 3013 container random sampling of the Innocuous bin and the Pressure bin has been completed and there has been no indication of corrosion or significant pressurization. The maximum pressure observed was less than 50 psig, which is well below the design pressure of 699 psig for the 3013 container [Reference 3]. The data collected during surveillance of these bins has been evaluated by the Materials Identification and Surveillance (MIS) Working Group and no additional surveillance is necessary for these bins at least through FY13. A decision will be made whether additional surveillance of these bins is needed during future years of storage and as additional containers are generated. Based on the data collected to date, the SPA concludes that 3013 containers in these bins can continue to be safely stored in KAMS. This year, 13 destructive examinations (DE) were performed on random samples from the Pressure & Corrosion bin. To date, DE has been completed for approximately 30% of the random samples from the Pressure & Corrosion bin. In addition, DE has been performed on 6 engineering judgment (EJ) containers, for a total of 17 to date. This includes one container that exceeded the 3013 Standard moisture limit which was opened at LANL. The container pieces and an oxide sample were sent to SRNL for examination in FY11. No significant pressurization has been observed for the Pressure & Corrosion bin containers. Relatively minor corrosion has been observed on some convenience containers and the inside of two inner containers. While the limited extent of corrosion does not jeopardize the integrity of the outer 3013 containers, it does highlight the importance of continuing to perform DE and the Shelf Life program to assure that the corrosion rate is not accelerating or changing to a different corrosion mechanism (e.g., stress corrosion cracking). Statistical sampling is currently scheduled to be completed in FY17, but there is a proposed reduction of the number of DE's per year for FY11 and beyond which may delay the completion date. Since 3013 containers are stored inside 9975 containers, surveillances of 9975 containers are performed in conjunction with 3013 container surveillances. Results of 9975 container nondestructive examinations (NDEs) and DEs indicate that the containers will provide adequate protection of the 3013 containers in K-Area storage for at least 15 years [Reference 4].« less

QUANTIFICATION OF 2,4-D ON SOLID-PHASE EXPOSURE SAMPLING MEDIA BY LC/MS/MS

EPA Science Inventory

Three types of solid phase chemical exposure sampling media: cellulose, polyurethane foam (PUF) and XAD-2, were analyzed for 2,4-D and the amine salts of 2,4-D. Individual samples were extracted into acidified methanol and the extracts were analyzed via LC/MS/MS using electrospra...

Comparison of three sampling instruments, Cytobrush, Curette and OralCDx, for liquid-based cytology of the oral mucosa.

PubMed

Reboiras-López, M D; Pérez-Sayáns, M; Somoza-Martín, J M; Antúnez-López, J R; Gándara-Vila, P; Gayoso-Diz, P; Gándara-Rey, J M; García-García, A

2012-01-01

Exfoliative cytology of the oral cavity is a simple and noninvasive technique that permits the study of epithelial cells. Liquid-based cytology is an auxiliary diagnostic tool for improving the specificity and sensitivity of conventional cytology. The objective of our study was to compare the quality of normal oral mucosa cytology samples obtained using three different instruments, Cytobrush®, dermatological curette and Oral CDx® for liquid-based cytology. One hundred four cytological samples of oral cavity were analyzed. Samples were obtained from healthy volunteer subjects using all three instruments. The clinical and demographic variables were age, sex and smoking habits. We analyzed cellularity, quality of the preparation and types of cells in the samples. All preparations showed appropriate preparation quality. In all smears analyzed, cells were distributed uniformly and showed no mucus, bleeding, inflammatory exudate or artifacts. We found no correlation between the average number of cells and the type of instrument. The samples generally consisted of two types of cells: superficial and intermediate. No differences were found among the cytological preparations of these three instruments. We did not observe basal cells in any of the samples analyzed.

The External Quality Assessment Scheme (EQAS): Experiences of a medium sized accredited laboratory.

PubMed

Bhat, Vivek; Chavan, Preeti; Naresh, Chital; Poladia, Pratik

2015-06-15

We put forth our experiences of EQAS, analyzed the result discrepancies, reviewed the corrective actions and also put forth strategies for risk identification and prevention of potential errors in a medical laboratory. For hematology, EQAS samples - blood, peripheral and reticulocyte smears - were received quarterly every year. All the blood samples were processed on HMX hematology analyzer by Beckman-Coulter. For clinical chemistry, lyophilized samples were received and were processed on Siemens Dimension Xpand and RXL analyzers. For microbiology, EQAS samples were received quarterly every year as lyophilized strains along with smears and serological samples. In hematology no outliers were noted for reticulocyte and peripheral smear examination. Only one outlier was noted for CBC. In clinical chemistry outliers (SDI ≥ 2) were noted in 7 samples (23 parameters) out of total 36 samples (756 parameters) processed. Thirteen of these parameters were analyzed as random errors, 3 as transcriptional errors and seven instances of systemic error were noted. In microbiology, one discrepancy was noted in isolate identification and in the grading of smears for AFB by Ziehl Neelsen stain. EQAS along with IQC is a very important tool for maintaining optimal quality of services. Copyright © 2015 Elsevier B.V. All rights reserved.

System and method for assaying a radionuclide

DOEpatents

Cadieux, James R; King, III, George S; Fugate, Glenn A

2014-12-23

A system for assaying a radionuclide includes a liquid scintillation detector, an analyzer connected to the liquid scintillation detector, and a delay circuit connected to the analyzer. A gamma detector and a multi-channel analyzer are connected to the delay circuit and the gamma detector. The multi-channel analyzer produces a signal reflective of the radionuclide in the sample. A method for assaying a radionuclide includes selecting a sample, detecting alpha or beta emissions from the sample with a liquid scintillation detector, producing a first signal reflective of the alpha or beta emissions, and delaying the first signal a predetermined time. The method further includes detecting gamma emissions from the sample, producing a second signal reflective of the gamma emissions, and combining the delayed first signal with the second signal to produce a third signal reflective of the radionuclide.

An Investigation into the Relationship Between Distillate Yield and Stable Isotope Fractionation

NASA Astrophysics Data System (ADS)

Sowers, T.; Wagner, A. J.

2016-12-01

Recent breakthroughs in laser spectrometry have allowed for faster, more efficient analyses of stable isotopic ratios in water samples. Commercially available instruments from Los Gatos Research and Picarro allow users to quickly analyze a wide range of samples, from seawater to groundwater, with accurate isotope ratios of D/H to within ± 0.2 ‰ and 18O/16O to within ± 0.03 ‰. While these instruments have increased the efficiency of stable isotope laboratories, they come with some major limitations, such as not being able to analyze hypersaline waters. The Los Gatos Research Liquid Water Isotope Analyzer (LWIA) can accurately and consistently measure the stable isotope ratios in waters with salinities ranging from 0 to 4 grams per liter (0 to 40 parts per thousand). In order to analyze water samples with salinities greater than 4 grams per liter, however, it was necessary to develop a consistent method through which to reduce salinity while causing as little fractionation as possible. Using a consistent distillation method, predictable fractionation of δ 18O and δ 2 H values was found to occur. This fractionation occurs according to a linear relationship with respect to the percent yield of the water in the sample. Using this method, samples with high salinity can be analyzed using laser spectrometry instruments, thereby enabling laboratories with Los Gatos or Picarro instruments to analyze those samples in house without having to dilute them using labor-intensive in-house standards or expensive premade standards.

Neutron activation analysis for antimetabolites. [in food samples

NASA Technical Reports Server (NTRS)

1973-01-01

Determination of metal ion contaminants in food samples is studied. A weighed quantity of each sample was digested in a concentrated mixture of nitric, hydrochloric and perchloric acids to affect complete solution of the food products. The samples were diluted with water and the pH adjusted according to the specific analysis performed. The samples were analyzed by neutron activation analysis, polarography, and atomic absorption spectrophotometry. The solid food samples were also analyzed by neutron activation analysis for increased sensitivity and lower levels of detectability. The results are presented in tabular form.

Radionuclides, inorganic constituents, organic compounds, and bacteria in water from selected wells and springs from the southern boundary of the Idaho National Engineering Laboratory to the Hagerman Area, Idaho, 1990

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bartholomay, R.C.; Edwards, D.D.; Campbell, L.J.

1992-03-01

The US Geological Survey and the Idaho Department of Water Resources, in response to a request from the US Department of Energy, sampled 19 sites as part of a long-term project to monitor water quality of the Snake River Plain aquifer from the southern boundary of the Idaho National Engineering Laboratory to the Hagerman area. Water samples were collected and analyzed for manmade pollutants and naturally occurring constituents. The samples were collected from seven irrigation wells, five domestic wells, two springs, one stock well, two dairy wells, one observation well, and one commercial well. Two quality assurance samples also weremore » collected and analyzed. The water samples were analyzed for selected radionuclides, inorganic constituents, organic compounds, and bacteria. None of the radionuclides, inorganic constituents, or organic compounds exceeded the established maximum contaminant levels for drinking water. Most of the radionuclide and inorganic constituent concentrations exceeded their respective reporting levels. All samples analyzed for surfactants and dissolved organic carbon had concentrations that exceeded their reporting level. Toluene concentrations exceeded the reporting level in one water sample. Two samples contained fecal coliform bacteria counts that exceeded established maximum contaminant levels for drinking water.« less

Elemental profiling and geographical differentiation of Ethiopian coffee samples through inductively coupled plasma-optical emission spectroscopy (ICP-OES), ICP-mass spectrometry (ICP-MS) and direct mercury analyzer (DMA).

PubMed

Habte, Girum; Hwang, In Min; Kim, Jae Sung; Hong, Joon Ho; Hong, Young Sin; Choi, Ji Yeon; Nho, Eun Yeong; Jamila, Nargis; Khan, Naeem; Kim, Kyong Su

2016-12-01

This study was aimed to establish the elemental profiling and provenance of coffee samples collected from eleven major coffee producing regions of Ethiopia. A total of 129 samples were analyzed for forty-five elements using inductively coupled plasma (ICP)-optical emission spectroscopy (OES), ICP-mass spectrometry (MS) and direct mercury analyzer (DMA). Among the macro elements, K showed the highest levels whereas Fe was found to have the lowest concentration values. In all the samples, Ca, K, Mg, P and S contents were statistically significant (p<0.05). Micro elements showed the concentrations order of: Mn>Cu>Sr>Zn>Rb>Ni>B. Contents of the trace elements were lower than the permissible standard values. Inter-regions differentiation by cluster analysis (CA), linear discriminant analysis (LDA) and principal component analysis (PCA) showed that micro and trace elements are the best chemical descriptors of the analyzed coffee samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

Advantages and challenges in automated apatite fission track counting

NASA Astrophysics Data System (ADS)

Enkelmann, E.; Ehlers, T. A.

2012-04-01

Fission track thermochronometer data are often a core element of modern tectonic and denudation studies. Soon after the development of the fission track methods interest emerged for the developed an automated counting procedure to replace the time consuming labor of counting fission tracks under the microscope. Automated track counting became feasible in recent years with increasing improvements in computer software and hardware. One such example used in this study is the commercial automated fission track counting procedure from Autoscan Systems Pty that has been highlighted through several venues. We conducted experiments that are designed to reliably and consistently test the ability of this fully automated counting system to recognize fission tracks in apatite and a muscovite external detector. Fission tracks were analyzed in samples with a step-wise increase in sample complexity. The first set of experiments used a large (mm-size) slice of Durango apatite cut parallel to the prism plane. Second, samples with 80-200 μm large apatite grains of Fish Canyon Tuff were analyzed. This second sample set is characterized by complexities often found in apatites in different rock types. In addition to the automated counting procedure, the same samples were also analyzed using conventional counting procedures. We found for all samples that the fully automated fission track counting procedure using the Autoscan System yields a larger scatter in the fission track densities measured compared to conventional (manual) track counting. This scatter typically resulted from the false identification of tracks due surface and mineralogical defects, regardless of the image filtering procedure used. Large differences between track densities analyzed with the automated counting persisted between different grains analyzed in one sample as well as between different samples. As a result of these differences a manual correction of the fully automated fission track counts is necessary for each individual surface area and grain counted. This manual correction procedure significantly increases (up to four times) the time required to analyze a sample with the automated counting procedure compared to the conventional approach.

Chemicals of emerging concern in water and bottom sediment in Great Lakes areas of concern, 2010 to 2011-Collection methods, analyses methods, quality assurance, and data

USGS Publications Warehouse

Lee, Kathy E.; Langer, Susan K.; Menheer, Michael A.; Foreman, William T.; Furlong, Edward T.; Smith, Steven G.

2012-01-01

The U.S. Geological Survey (USGS) cooperated with the U.S. Environmental Protection Agency and the U.S. Fish and Wildlife Service on a study to identify the occurrence of chemicals of emerging concern (CECs) in water and bottom-sediment samples collected during 2010–11 at sites in seven areas of concern (AOCs) throughout the Great Lakes. Study sites include tributaries to the Great Lakes in AOCs located near Duluth, Minn.; Green Bay, Wis.; Roches­ter, N.Y.; Detroit, Mich.; Toledo, Ohio; Milwaukee, Wis.; and Ashtabula, Ohio. This report documents the collection meth­ods, analyses methods, quality-assurance data and analyses, and provides the data for this study. Water and bottom-sediment samples were analyzed at the USGS National Water Quality Laboratory in Denver, Colo., for a broad suite of CECs. During this study, 135 environmental and 23 field dupli­cate samples of surface water and wastewater effluent, 10 field blank water samples, and 11 field spike water samples were collected and analyzed. Sixty-one of the 69 wastewater indicator chemicals (laboratory method 4433) analyzed were detected at concentrations ranging from 0.002 to 11.2 micrograms per liter. Twenty-eight of the 48 pharmaceuticals (research method 8244) analyzed were detected at concentrations ranging from 0.0029 to 22.0 micro­grams per liter. Ten of the 20 steroid hormones and sterols analyzed (research method 4434) were detected at concentrations ranging from 0.16 to 10,000 nanograms per liter. During this study, 75 environmental, 13 field duplicate samples, and 9 field spike samples of bottom sediment were collected and analyzed for a wide variety of CECs. Forty-seven of the 57 wastewater indicator chemicals (laboratory method 5433) analyzed were detected at concentrations ranging from 0.921 to 25,800 nanograms per gram. Seventeen of the 20 steroid hormones and sterols (research method 6434) analyzed were detected at concentrations ranging from 0.006 to 8,921 nanograms per gram. Twelve of the 20 pharmaceuticals (research method 8244) analyzed were detected at concentrations ranging from 2.35 to 453.5 nanograms per gram. Six of the 11 antidepressants (research method 9008) analyzed were detected at concentrations ranging from 2.79 to 91.6 nanograms per gram.

Quantitative Method for Analysis of Hydrocodone, Hydromorphone and Norhydrocodone in Human Plasma by Liquid Chromatography-tandem Mass Spectrometry

DTIC Science & Technology

2013-03-01

ratio ranges obtained for the six standards. Twelve samples were analyzed to demonstrate the efficiency of the extraction procedure. Drug and internal...frozen (−70 ◦C). Refrigerated samples were tested after 2 months of storage ; frozen samples were tested for up to 1 year from stor- age date. The...freeze–thaw stability was evaluated by analyzing three subject samples with known drug concentrations and two quality control samples at concentrations

Analysis of counting errors in the phase/Doppler particle analyzer

NASA Technical Reports Server (NTRS)

Oldenburg, John R.

1987-01-01

NASA is investigating the application of the Phase Doppler measurement technique to provide improved drop sizing and liquid water content measurements in icing research. The magnitude of counting errors were analyzed because these errors contribute to inaccurate liquid water content measurements. The Phase Doppler Particle Analyzer counting errors due to data transfer losses and coincidence losses were analyzed for data input rates from 10 samples/sec to 70,000 samples/sec. Coincidence losses were calculated by determining the Poisson probability of having more than one event occurring during the droplet signal time. The magnitude of the coincidence loss can be determined, and for less than a 15 percent loss, corrections can be made. The data transfer losses were estimated for representative data transfer rates. With direct memory access enabled, data transfer losses are less than 5 percent for input rates below 2000 samples/sec. With direct memory access disabled losses exceeded 20 percent at a rate of 50 samples/sec preventing accurate number density or mass flux measurements. The data transfer losses of a new signal processor were analyzed and found to be less than 1 percent for rates under 65,000 samples/sec.

Portable x-ray fluorescence spectrometer for environmental monitoring of inorganic pollutants

NASA Technical Reports Server (NTRS)

Clark, III, Benton C. (Inventor); Thornton, Michael G. (Inventor)

1991-01-01

A portable x-ray fluorescence spectrometer has a portable sensor unit containing a battery, a high voltage power supply, an x-ray tube which produces a beam x-ray radiation directed toward a target sample, and a detector for fluorescent x-rays produced by the sample. If a silicon-lithium detector is used, the sensor unit also contains either a thermoelectric or thermochemical cooler, or a small dewar flask containing liquid nitrogen to cool the detector. A pulse height analyzer (PHA) generates a spectrum of data for each sample consisting of the number of fluorescent x-rays detected as a function of their energy level. The PHA can also store spectrum data for a number of samples in the field. A processing unit can be attached to the pulse height analyzer to upload and analyze the stored spectrum data for each sample. The processing unit provides a graphic display of the spectrum data for each sample, and provides qualitative and/or quantitative analysis of the elemental composition of the sample by comparing the peaks in the sample spectrum against known x-ray energies for various chemical elements. An optional filtration enclosure can be used to filter particles from a sample suspension, either in the form of a natural suspension or a chemically created precipitate. The sensor unit is then temporarily attached to the filtration unit to analyze the particles collected by the filter medium.

Results from laboratory and field testing of nitrate measuring spectrophotometers

USGS Publications Warehouse

Snazelle, Teri T.

2015-01-01

In Phase II, the analyzers were deployed in field conditions at three diferent USGS sites. The measured nitrate concentrations were compared to discrete (reference) samples analyzed by the Direct UV method on a Shimadzu UV1800 bench top spectrophotometer, and by the National Environmental Methods Index (NEMI) method I-2548-11 at the USGS National Water Quality Laboratory. The first deployment at USGS site 0249620 on the East Pearl River in Hancock County, Mississippi, tested the ability of the TriOs ProPs (10-mm path length), Hach NITRATAX (5 mm), Satlantic SUNA (10 mm), and the S::CAN Spectro::lyser (5 mm) to accurately measure low-level (less than 2 mg-N/L) nitrate concentrations while observing the effect turbidity and colored dissolved organic matter (CDOM) would have on the analyzers' measurements. The second deployment at USGS site 01389005 Passaic River below Pompton River at Two Bridges, New Jersey, tested the analyzer's accuracy in mid-level (2-8 mg-N/L) nitrate concentrations. This site provided the means to test the analyzers' performance in two distinct matrices—the Passaic and the Pompton Rivers. In this deployment, three instruments tested in Phase I (TriOS, Hach, and SUNA) were deployed with the S::CAN Spectro::lyser (35 mm) already placed by the New Jersey Water Science Center (WSC). The third deployment at USGS site 05579610 Kickapoo Creek at 2100E Road near Bloomington, Illinois, tested the ability of the analyzers to measure high nitrate concentrations (greater than 8 mg-N/L) in turbid waters. For Kickapoo Creek, the HIF provided the TriOS (10 mm) and S::CAN (5 mm) from Phase I, and a SUNA V2 (5 mm) to be deployed adjacent to the Illinois WSC-owned Hach (2 mm). A total of 40 discrete samples were collected from the three deployment sites and analyzed. The nitrate concentration of the samples ranged from 0.3–22.2 mg-N/L. The average absolute difference between the TriOS measurements and discrete samples was 0.46 mg-N/L. For the combined data from the Hach 5-mm and 2-mm analyzers, the average absolute difference between the Hach samples and the discrete samples was 0.13 mg-N/L. For the SUNA and SUNA V2 combined data, the average absolute difference between the SUNA samples and the discrete samples was 0.66 mg-N/L. The average absolute difference between the S::CAN samples and the discrete samples was 0.63 mg-N/L.

View of Expedition 15 FE Anderson performing the ANITA Experiment in the Node 1

NASA Image and Video Library

2007-10-06

ISS015-E-32200 (6 Oct. 2007) --- Astronaut Clay Anderson, Expedition 15 flight engineer, uses an air sample pump and 2.5 liter gas sample bag to gather and analyze air samples for the Analyzing Interferometer for Ambient Air (ANITA) experiment in the Unity node of the International Space Station.

Lectin-Magnetic Separation (LMS) for isolation of Toxoplasma gondii oocysts from concentrated water samples prior to detection by microscopy or qPCR

USDA-ARS?s Scientific Manuscript database

Although standard methods for analyzing water samples for the protozoan parasites Cryptosporidium spp. and Giardia duodenalis are available and widely used, equivalent methods for analyzing water samples for Toxoplasma oocysts are lacking. This is partly due to the lack of a readily available, relia...

Flask sample measurements for CO2, CH4 and CO using cavity ring-down spectrometry

NASA Astrophysics Data System (ADS)

Wang, J.-L.; Jacobson, G.; Rella, C. W.; Chang, C.-Y.; Liu, I.; Liu, W.-T.; Chew, C.; Ou-Yang, C.-F.; Liao, W.-C.; Chang, C.-C.

2013-08-01

In recent years, cavity ring-down spectrometry (CRDS) has been demonstrated to be a highly sensitive, stable and fast analytical technique for real-time in situ measurements of greenhouse gases. In this study, we propose the technique (which we call flask-CRDS) of analyzing whole air flask samples for CO2, CH4 and CO using a custom gas manifold designed to connect to a CRDS analyzer. Extremely stable measurements of these gases can be achieved over a large pressure range in the flask, from 175 to 760 Torr. The wide pressure range is conducive to flask sample measurement in three ways: (1) flask samples can be collected in low-pressure environments (e.g. high-altitude locations); (2) flask samples can be first analyzed for other trace gases with the remaining low-pressure sample for CRDS analysis of CO2, CH4 and CO; and (3) flask samples can be archived and re-analyzed for validation. The repeatability of this method (1σ of 0.07 ppm for CO2, 0.4 ppb for CH4, and 0.5 ppb for CO) was assessed by analyzing five canisters filled with the same air sample to a pressure of 200 Torr. An inter-comparison of the flask-CRDS data with in-situ CRDS measurements at a high-altitude mountain baseline station revealed excellent agreement, with differences of 0.10 ± 0.09 ppm (1σ) for CO2 and 0.9 ± 1.0 ppb for CH4. This study demonstrated that the flask-CRDS method was not only simple to build and operate but could also perform highly accurate and precise measurements of atmospheric CO2, CH4 and CO in flask samples.

Rail-RNA: scalable analysis of RNA-seq splicing and coverage.

PubMed

Nellore, Abhinav; Collado-Torres, Leonardo; Jaffe, Andrew E; Alquicira-Hernández, José; Wilks, Christopher; Pritt, Jacob; Morton, James; Leek, Jeffrey T; Langmead, Ben

2017-12-15

RNA sequencing (RNA-seq) experiments now span hundreds to thousands of samples. Current spliced alignment software is designed to analyze each sample separately. Consequently, no information is gained from analyzing multiple samples together, and it requires extra work to obtain analysis products that incorporate data from across samples. We describe Rail-RNA, a cloud-enabled spliced aligner that analyzes many samples at once. Rail-RNA eliminates redundant work across samples, making it more efficient as samples are added. For many samples, Rail-RNA is more accurate than annotation-assisted aligners. We use Rail-RNA to align 667 RNA-seq samples from the GEUVADIS project on Amazon Web Services in under 16 h for US$0.91 per sample. Rail-RNA outputs alignments in SAM/BAM format; but it also outputs (i) base-level coverage bigWigs for each sample; (ii) coverage bigWigs encoding normalized mean and median coverages at each base across samples analyzed; and (iii) exon-exon splice junctions and indels (features) in columnar formats that juxtapose coverages in samples in which a given feature is found. Supplementary outputs are ready for use with downstream packages for reproducible statistical analysis. We use Rail-RNA to identify expressed regions in the GEUVADIS samples and show that both annotated and unannotated (novel) expressed regions exhibit consistent patterns of variation across populations and with respect to known confounding variables. Rail-RNA is open-source software available at http://rail.bio. anellore@gmail.com or langmea@cs.jhu.edu. Supplementary data are available at Bioinformatics online. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please e-mail: journals.permissions@oup.com

40 CFR 86.160-00 - Exhaust emission test procedure for SC03 emissions.

Code of Federal Regulations, 2014 CFR

2014-07-01

... collected in bags are analyzed for THC, CO, CO2, CH4, and NOX. For petroleum-fueled diesel-cycle vehicles, THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel bag samples of dilution air are analyzed for THC, CO, CO2, CH4, and NOX. (b) Dynamometer activities. (1) All...

40 CFR 86.160-00 - Exhaust emission test procedure for SC03 emissions.

Code of Federal Regulations, 2012 CFR

2012-07-01

... collected in bags are analyzed for THC, CO, CO2, CH4, and NOX. For petroleum-fueled diesel-cycle vehicles, THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel bag samples of dilution air are analyzed for THC, CO, CO2, CH4, and NOX. (b) Dynamometer activities. (1) All...

40 CFR 86.160-00 - Exhaust emission test procedure for SC03 emissions.

Code of Federal Regulations, 2013 CFR

2013-07-01

... collected in bags are analyzed for THC, CO, CO2, CH4, and NOX. For petroleum-fueled diesel-cycle vehicles, THC is sampled and analyzed continuously according to the provisions of § 86.110. Parallel bag samples of dilution air are analyzed for THC, CO, CO2, CH4, and NOX. (b) Dynamometer activities. (1) All...

Methyl-CpG island-associated genome signature tags

DOEpatents

Dunn, John J

2014-05-20

Disclosed is a method for analyzing the organismic complexity of a sample through analysis of the nucleic acid in the sample. In the disclosed method, through a series of steps, including digestion with a type II restriction enzyme, ligation of capture adapters and linkers and digestion with a type IIS restriction enzyme, genome signature tags are produced. The sequences of a statistically significant number of the signature tags are determined and the sequences are used to identify and quantify the organisms in the sample. Various embodiments of the invention described herein include methods for using single point genome signature tags to analyze the related families present in a sample, methods for analyzing sequences associated with hyper- and hypo-methylated CpG islands, methods for visualizing organismic complexity change in a sampling location over time and methods for generating the genome signature tag profile of a sample of fragmented DNA.

Increased instrument intelligence--can it reduce laboratory error?

PubMed

Jekelis, Albert W

2005-01-01

Recent literature has focused on the reduction of laboratory errors and the potential impact on patient management. This study assessed the intelligent, automated preanalytical process-control abilities in newer generation analyzers as compared with older analyzers and the impact on error reduction. Three generations of immuno-chemistry analyzers were challenged with pooled human serum samples for a 3-week period. One of the three analyzers had an intelligent process of fluidics checks, including bubble detection. Bubbles can cause erroneous results due to incomplete sample aspiration. This variable was chosen because it is the most easily controlled sample defect that can be introduced. Traditionally, lab technicians have had to visually inspect each sample for the presence of bubbles. This is time consuming and introduces the possibility of human error. Instruments with bubble detection may be able to eliminate the human factor and reduce errors associated with the presence of bubbles. Specific samples were vortexed daily to introduce a visible quantity of bubbles, then immediately placed in the daily run. Errors were defined as a reported result greater than three standard deviations below the mean and associated with incomplete sample aspiration of the analyte of the individual analyzer Three standard deviations represented the target limits of proficiency testing. The results of the assays were examined for accuracy and precision. Efficiency, measured as process throughput, was also measured to associate a cost factor and potential impact of the error detection on the overall process. The analyzer performance stratified according to their level of internal process control The older analyzers without bubble detection reported 23 erred results. The newest analyzer with bubble detection reported one specimen incorrectly. The precision and accuracy of the nonvortexed specimens were excellent and acceptable for all three analyzers. No errors were found in the nonvortexed specimens. There were no significant differences in overall process time for any of the analyzers when tests were arranged in an optimal configuration. The analyzer with advanced fluidic intelligence demostrated the greatest ability to appropriately deal with an incomplete aspiration by not processing and reporting a result for the sample. This study suggests that preanalytical process-control capabilities could reduce errors. By association, it implies that similar intelligent process controls could favorably impact the error rate and, in the case of this instrument, do it without negatively impacting process throughput. Other improvements may be realized as a result of having an intelligent error-detection process including further reduction in misreported results, fewer repeats, less operator intervention, and less reagent waste.

High-throughput quantitative analysis by desorption electrospray ionization mass spectrometry.

PubMed

Manicke, Nicholas E; Kistler, Thomas; Ifa, Demian R; Cooks, R Graham; Ouyang, Zheng

2009-02-01

A newly developed high-throughput desorption electrospray ionization (DESI) source was characterized in terms of its performance in quantitative analysis. A 96-sample array, containing pharmaceuticals in various matrices, was analyzed in a single run with a total analysis time of 3 min. These solution-phase samples were examined from a hydrophobic PTFE ink printed on glass. The quantitative accuracy, precision, and limit of detection (LOD) were characterized. Chemical background-free samples of propranolol (PRN) with PRN-d(7) as internal standard (IS) and carbamazepine (CBZ) with CBZ-d(10) as IS were examined. So were two other sample sets consisting of PRN/PRN-d(7) at varying concentration in a biological milieu of 10% urine or porcine brain total lipid extract, total lipid concentration 250 ng/microL. The background-free samples, examined in a total analysis time of 1.5 s/sample, showed good quantitative accuracy and precision, with a relative error (RE) and relative standard deviation (RSD) generally less than 3% and 5%, respectively. The samples in urine and the lipid extract required a longer analysis time (2.5 s/sample) and showed RSD values of around 10% for the samples in urine and 4% for the lipid extract samples and RE values of less than 3% for both sets. The LOD for PRN and CBZ when analyzed without chemical background was 10 and 30 fmol, respectively. The LOD of PRN increased to 400 fmol analyzed in 10% urine, and 200 fmol when analyzed in the brain lipid extract.

Phenolic Compounds Analysis of Root, Stalk, and Leaves of Nettle

PubMed Central

Otles, Semih; Yalcin, Buket

2012-01-01

Types of nettles (Urtica dioica) were collected from different regions to analyze phenolic compounds in this research. Nettles are specially grown in the coastal part. According to this kind of properties, nettle samples were collected from coastal part of (Mediterranean, Aegean, Black sea, and Marmara) Turkey. Phenolic profile, total phenol compounds, and antioxidant activities of nettle samples were analyzed. Nettles were separated to the part of root, stalk, and leaves. Then, these parts of nettle were analyzed to understand the difference of phenolic compounds and amount of them. Nettle (root, stalk and leaves) samples were analyzed by using High-Performance Liquid Chromatography with Diode-Array Detection (HPLC-DAD) to qualitative and quantitative determination of the phenolic compounds. Total phenolic components were measured by using Folin-Ciocalteu method. The antioxidant activity was measured by using DPPH (2,2-diphenyl-1-picrylhydrazyl) which is generally used for herbal samples and based on single electron transfer (SET). PMID:22593694

Phenolic compounds analysis of root, stalk, and leaves of nettle.

PubMed

Otles, Semih; Yalcin, Buket

2012-01-01

Types of nettles (Urtica dioica) were collected from different regions to analyze phenolic compounds in this research. Nettles are specially grown in the coastal part. According to this kind of properties, nettle samples were collected from coastal part of (Mediterranean, Aegean, Black sea, and Marmara) Turkey. Phenolic profile, total phenol compounds, and antioxidant activities of nettle samples were analyzed. Nettles were separated to the part of root, stalk, and leaves. Then, these parts of nettle were analyzed to understand the difference of phenolic compounds and amount of them. Nettle (root, stalk and leaves) samples were analyzed by using High-Performance Liquid Chromatography with Diode-Array Detection (HPLC-DAD) to qualitative and quantitative determination of the phenolic compounds. Total phenolic components were measured by using Folin-Ciocalteu method. The antioxidant activity was measured by using DPPH (2,2-diphenyl-1-picrylhydrazyl) which is generally used for herbal samples and based on single electron transfer (SET).

Innovative application of the moisture analyzer for determination of dry mass content of processed cheese

NASA Astrophysics Data System (ADS)

Kowalska, Małgorzata; Janas, Sławomir; Woźniak, Magdalena

2018-04-01

The aim of this work was the presentation of an alternative method of determination of the total dry mass content in processed cheese. The authors claim that the presented method can be used in industry's quality control laboratories for routine testing and for quick in-process control. For the test purposes both reference method of determination of dry mass in processed cheese and moisture analyzer method were used. The tests were carried out for three different kinds of processed cheese. In accordance with the reference method, the sample was placed on a layer of silica sand and dried at the temperature of 102 °C for about 4 h. The moisture analyzer test required method validation, with regard to drying temperature range and mass of the analyzed sample. Optimum drying temperature of 110 °C was determined experimentally. For Hochland cream processed cheese sample, the total dry mass content, obtained using the reference method, was 38.92%, whereas using the moisture analyzer method, it was 38.74%. An average analysis time in case of the moisture analyzer method was 9 min. For the sample of processed cheese with tomatoes, the reference method result was 40.37%, and the alternative method result was 40.67%. For the sample of cream processed cheese with garlic the reference method gave value of 36.88%, and the alternative method, of 37.02%. An average time of those determinations was 16 min. Obtained results confirmed that use of moisture analyzer is effective. Compliant values of dry mass content were obtained for both of the used methods. According to the authors, the fact that the measurement took incomparably less time for moisture analyzer method, is a key criterion of in-process control and final quality control method selection.

Fixture for supporting and aligning a sample to be analyzed in an x-ray diffraction apparatus

DOEpatents

Green, L.A.; Heck, J.L. Jr.

1985-04-23

A fixture is provided for supporting and aligning small samples of material on a goniometer for x-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the x-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an x-ray diffraction apparatus previously limited to the analysis of much larger samples.

Fixture for supporting and aligning a sample to be analyzed in an X-ray diffraction apparatus

DOEpatents

Green, Lanny A.; Heck, Jr., Joaquim L.

1987-01-01

A fixture is provided for supporting and aligning small samples of material on a goniometer for X-ray diffraction analysis. A sample-containing capillary is accurately positioned for rotation in the X-ray beam by selectively adjusting the fixture to position the capillary relative to the x and y axes thereof to prevent wobble and position the sample along the z axis or the axis of rotation. By employing the subject fixture relatively small samples of materials can be analyzed in an X-ray diffraction apparatus previously limited to the analysis of much larger samples.

Procedures for Obtaining and Analyzing Writing Samples of School-Age Children and Adolescents.

PubMed

Price, Johanna R; Jackson, Sandra C

2015-10-01

Many students' writing skills are below grade-level expectations, and students with oral language difficulties are at particular risk for writing difficulties. Speech-language pathologists' (SLPs') expertise in language applies to both the oral and written modalities, yet evidence suggests that SLPs' confidence regarding writing assessment is low. Writing samples are a clinically useful, criterion-referenced assessment technique that is relevant to helping students satisfy writing-related requirements of the Common Core State Standards (National Governors Association Center for Best Practices and Council of Chief State School Officers, 2010a). This article provides recommendations for obtaining and analyzing students' writing samples. In this tutorial, the authors provide a comprehensive literature review of methods regarding (a) collection of writing samples from narrative, expository (informational/explanatory), and persuasive (argument) genres; (b) variables of writing performance that are useful to assess; and (c) manual and computer-aided techniques for analyzing writing samples. The authors relate their findings to expectations for writing skills expressed in the Common Core State Standards (National Governors Association Center for Best Practices & Council of Chief State School Officers, 2010a). SLPs can readily implement many techniques for obtaining and analyzing writing samples. The information in this article provides SLPs with recommendations for the use of writing samples and may help increase SLPs' confidence regarding written language assessment.

Quality-Assurance Data for Routine Water Analyses by the U.S. Geological Survey Laboratory in Troy, New York-July 1997 through June 1999

USGS Publications Warehouse

Lincoln, Tricia A.; Horan-Ross, Debra A.; McHale, Michael R.; Lawrence, Gregory B.

2006-01-01

The laboratory for analysis of low-ionic-strength water at the U.S. Geological Survey (USGS) Water Science Center in Troy, N.Y., analyzes samples collected by USGS projects throughout the Northeast. The laboratory's quality-assurance program is based on internal and interlaboratory quality-assurance samples and quality-control procedures that were developed to ensure proper sample collection, processing, and analysis. The quality-assurance/quality-control data for the time period addressed in this report were stored in the laboratory's SAS data-management system, which provides efficient review, compilation, and plotting of data. This report presents and discusses results of quality-assurance and quality- control samples analyzed from July 1997 through June 1999. Results for the quality-control samples for 18 analytical procedures were evaluated for bias and precision. Control charts indicate that data for eight of the analytical procedures were occasionally biased for either high-concentration and (or) low-concentration samples but were within control limits; these procedures were: acid-neutralizing capacity, total monomeric aluminum, total aluminum, ammonium, calcium, chloride, specific conductance, and sulfate. The data from the potassium and sodium analytical procedures are insufficient for evaluation. Results from the filter-blank and analytical-blank analyses indicate that the procedures for 11 of 13 analytes were within control limits, although the concentrations for blanks were occasionally outside the control limits. Blank analysis results for chloride showed that 22 percent of blanks did not meet data-quality objectives and results for dissolved organic carbon showed that 31 percent of the blanks did not meet data-quality objectives. Sampling and analysis precision are evaluated herein in terms of the coefficient of variation obtained for triplicate samples in the procedures for 14 of the 18 analytes. At least 90 percent of the samples met data-quality objectives for all analytes except total aluminum (70 percent of samples met objectives) and potassium (83 percent of samples met objectives). Results of the USGS interlaboratory Standard Reference Sample (SRS) Project indicated good data quality for most constituents over the time period. The P-sample (low-ionic-strength constituents) analysis had good ratings in two of these studies and a satisfactory rating in the third. The results of the T-sample (trace constituents) analysis indicated high data quality with good ratings in all three studies. The N-sample (nutrient constituents) studies had one each of excellent, good, and satisfactory ratings. Results of Environment Canada's National Water Research Institute (NWRI) program indicated that at least 80 percent of the samples met data-quality objectives for 9 of the 13 analytes; the exceptions were dissolved organic carbon, ammonium, chloride, and specific conductance. Data-quality objectives were not met for dissolved organic carbon in two NWRI studies, but all of the samples were within control limits for the last study. Data-quality objectives were not met in 41 percent of samples analyzed for ammonium, 25 percent of samples analyzed for chloride, and 30 percent of samples analyzed for specific conductance. Results from blind reference-sample analyses indicated that data-quality objectives were met by at least 84 percent of the samples analyzed for calcium, chloride, magnesium, pH, and potassium. Data-quality objectives were met by 73 percent of those analyzed for sulfate. The data-quality objective was not met for sodium. The data are insufficient for evaluation of the specific conductance results.

77 FR 41720 - Hazardous Waste Management System; Identification and Listing of Hazardous Waste; Proposed Exclusion

Federal Register 2010, 2011, 2012, 2013, 2014

2012-07-16

... delist? B. How does IBM generate the waste? C. How did IBM sample and analyze the petitioned waste? D..., thickened/conditioned, and pressed to generate the F006 waste stream. C. How did IBM sample and analyze the... the volatiles and semi-volatiles samples were non- detect. E. How did EPA evaluate the risk of...

Results of chemical and isotopic analyses of sediment and water from alluvium of the Canadian River near a closed municipal landfill, Norman, Oklahoma

USGS Publications Warehouse

Breit, George N.; Tuttle, Michele L.W.; Cozzarelli, Isabelle M.; Christenson, Scott C.; Jaeschke, Jeanne B.; Fey, David L.; Berry, Cyrus J.

2005-01-01

Results of physical and chemical analyses of sediment and water collected near a closed municipal landfill at Norman, Oklahoma are presented in this report. Sediment analyses are from 40 samples obtained by freeze-shoe coring at 5 sites, and 14 shallow (depth <1.3 m) sediment samples. The sediment was analyzed to determine grain size, the abundance of extractable iron species and the abundances and isotopic compositions of forms of sulfur. Water samples included pore water from the freeze-shoe core, ground water, and surface water. Pore water from 23 intervals of the core was collected and analyzed for major and trace dissolved species. Thirteen ground-water samples obtained from wells within a few meters of the freeze-shoe core sites and one from the landfill were analyzed for major and trace elements as well as the sulfur and oxygen isotope composition of dissolved sulfate. Samples of surface water were collected at 10 sites along the Canadian River from New Mexico to central Oklahoma. These river-water samples were analyzed for major elements, trace elements, and the isotopic composition of dissolved sulfate.

Relation between urbanization and water quality of streams in the Austin area, Texas

USGS Publications Warehouse

Veenhuis, J.E.; Slade, R.M.

1990-01-01

The ratio of the number of samples with detectable concentrations to the total number of samples analyzed for 18 inorganic trace elements and the concentrations of many of these minor constituents increased with increasing development classifications. Twenty-two of the 42 synthetic organic compounds for which samples were analyzed were detected in one or more samples. The compounds were detected more frequently and in larger concentrations at the sites with more urban classifications.

Watershed trend analysis and water-quality assessment using bottom-sediment cores from Cheney Reservoir, south-central Kansas

USGS Publications Warehouse

Pope, Larry M.

1998-01-01

An examination of Cheney Reservoir bottom sediment was conducted in August 1997 to describe long-term trends and document the occurrence of selected constituents at concentrations that may be detrimental to aquatic organisms. Average concentrations of total phosphorus in bottom-sediment cores ranged from 94 to 674 milligrams per kilogram and were statistically related to silt- and (or) clay-size particles. Results from selected sampling sites in Cheney Reservoir indicate an increasing trend in total phosphorus concentrations. This trend is probably of nonpoint-source origin and may be related to an increase in fertilizer sales in the area, which more than doubled between 1965 and 1996, and to livestock production. Few organochlorine compounds were detected in bottom-sediment samples from Cheney Reservoir. DDT, its degradation products DDD and DDE, and dieldrin had detectable concentrations in the seven samples that were analyzed. DDT and DDD were each detected in one sample at concentrations of 1.0 and 0.65 microgram per kilogram, respectively. By far, the most frequently detected organochlorine insecticide was DDE, which was detected in all seven samples, ranging in concentration from 0.31 to 1.3 micrograms per kilogram. A decreasing trend in DDE concentrations was evident in sediment-core data from one sampling site. Dieldrin was detected in one sample from each of two sampling sites at concentrations of 0.21 and 0.22 micrograms per kilogram. Polychlorinated biphenyls were not detected in any bottom-sediment sample analyzed. Selected organophosphate, chlorophenoxy-acid, triazine, and acetanilide pesticides were analyzed in 18 bottom-sediment samples. Of the 23 pesticides analyzed, only the acetanilide herbicide metolachlor was detected (in 22 percent of the samples). Seven bottom-sediment samples were analyzed for major metals and trace elements. The median and maximum concentrations of arsenic and chromium, the maximum concentration of copper, and all concentrations of nickel in the seven samples were in the range where adverse effects to aquatic organisms occasionally occur. No time trends in trace elements were discernable in the August 1997 data.

Water- and air-quality and surficial bed-sediment monitoring of the Sweetwater Reservoir watershed, San Diego County, California, 2003-09

USGS Publications Warehouse

Mendez, Gregory O.; Majewski, Michael S.; Foreman, William T.; Morita, Andrew Y.

2015-01-01

Sampling results show concentrations of the gasoline oxygenate methyl tert-butyl ether in water and air samples declined after it was phased out by the State of California in January 2004. The largest concentrations of gasoline hydrocarbons benzene and toluene in water were detected at or near the surface of the SWR. Isophorone and phenol were the two most frequently detected BNA compounds in water. Diuron, prometon, and simazine were the most frequently detected pesticide compounds in water. Concentrations of benzene and toluene in air samples were highest during the cooler months and had a consistent seasonal pattern over time. Ten PAH compounds were detected frequently in air samples. Twelve pesticide compounds were also detected in air samples. Surficial bed-sediment samples were analyzed for 53 PAHs; 22 of the compounds had one or more detections. Surficial bed-sediment samples were analyzed for 22 organic compounds; only 6 compounds had one or more detections. Surficial bed-sediment samples were analyzed for 37 metals.

Referred Air Method 25E: Determination of a Vapor Phase Organic Concentration in Waste Samples

EPA Pesticide Factsheets

This method is applicable for determining the vapor pressure of waste. The headspace vapor of the sample is analyzed for carbon content by a headspace analyzer, which uses a flame ionization detector (FID).

Rainfall, discharge, and water-quality data during stormwater monitoring, H-1 storm drain, Oahu, Hawaii, July 1, 2009, to June 30, 2010

USGS Publications Warehouse

Presley, Todd K.; Jamison, Marcael T.J.

2010-01-01

Storm runoff water-quality samples were collected as part of the State of Hawaii Department of Transportation Stormwater Monitoring Program. The program is designed to assess the effects of highway runoff and urban runoff collected by the H-1 storm drain on the Manoa-Palolo Drainage Canal. This report summarizes rainfall, discharge, and water-quality data collected between July 1, 2009, and June 30, 2010. As part of this program, rainfall and continuous discharge data were collected at the H-1 storm drain. During the year, sampling strategy and sample processing methods were modified to improve the characterization of the effects of discharge from the storm drain on the Manoa-Palolo Drainage Canal. During July 1, 2009, to February 1, 2010, samples were collected from only the H-1 storm drain. Beginning February 2, 2010, samples were collected simultaneously from the H-1 storm drain and the Manoa-Palolo Drainage Canal at a location about 50 feet upstream of the discharge point of the H-1 storm drain. Three storms were sampled during July 1, 2009, to June 30, 2010. All samples were collected using automatic samplers. For the storm of August 12, 2009, grab samples (for oil and grease, and total petroleum hydrocarbons) and a composite sample were collected. The composite sample was analyzed for total suspended solids, nutrients, and selected dissolved and total (filtered and unfiltered) trace metals (cadmium, chromium, nickel, copper, lead, and zinc). Two storms were sampled in March 2010 at the H-1 storm drain and from the Manoa-Palolo Drainage Canal. Two samples were collected during the storm of March 4, 2010, and six samples were collected during the storm of March 8, 2010. These two storms were sampled using the modified strategy, in which discrete samples from the automatic sampler were processed and analyzed individually, rather than as a composite sample, using the simultaneously collected samples from the H-1 storm drain and from the Manoa-Palolo Drainage Canal. The discrete samples were analyzed for some or all of the following constituents: total suspended solids, nutrients, oil and grease, and selected dissolved (filtered) trace metals (cadmium, chromium, nickel, copper, lead, and zinc). Five quality-assurance/quality-control samples were analyzed during the year. These samples included one laboratory-duplicate, one field-duplicate, and one matrix-spike sample prepared and analyzed with the storm samples. In addition, two inorganic blank-water samples, one sample at the H-1 storm drain and one sample at the Manoa-Palolo Drainage Canal, were collected by running the blank water (water purified of all inorganic constituents) through the sampling and processing systems after cleaning automatic sampler lines to verify that the sampling lines were not contaminated.

A sample-to-result system for blood coagulation tests on a microfluidic disk analyzer

PubMed Central

Lin, Chia-Hui; Liu, Cheng-Yuan; Shih, Chih-Hsin; Lu, Chien-Hsing

2014-01-01

In this report, we describe in detail a microfluidic analyzer, which is able to conduct blood coagulation tests using whole blood samples. Sample preparation steps, such as whole blood aliquoting and metering, plasma separation, decanting, and mixing with reagents were performed in sequence through microfluidic functions integrated on a disk. Both prothrombin time (PT) and activated partial thromboplastin time (aPTT) were carried out on the same platform and the test results can be reported in 5 min. Fifty clinical samples were tested for both PT and aPTT utilizing the microfluidic disk analyzer and the instrument used in hospitals. The test results showed good correlation and agreement between the two instruments. PMID:25332733

Stormwater-runoff data, Madison, Wisconsin, 1993-94

USGS Publications Warehouse

Waschbusch, R.J.

1996-01-01

As required by Section 402(P) of the Water Quality Control Act of 1987, stormwater-runoff samples collected during storms that met three criteria (rainfall depths 50 to 150 percent of average depth range, rainfall durations 50 to 150 percent of average duration, and antecedent dry-weather period of at least 72 hours) were analyzed for semivolatile organic chemicals, total metals, pesticides, polychlorinated biphenyls, inorganic constituents, bacteria, oil and grease, pH, and water temperature. Two of the seven sites also had samples analyzed for volatile organic chemicals. In addition to the required sampling, additional runoff samples that did not necessarily meet the three rainfall criteria, were analyzed for total metals and inorganic constituents. Storm loads of selected constituents were computed.

Rio Blanco, Colorado, Long-Term Hydrologic Monitoring Program Sampling and Analysis Results for 2009

DOE Office of Scientific and Technical Information (OSTI.GOV)

None

2009-12-21

The U.S. Department of Energy (DOE) Office of Legacy Management conducted annual sampling at the Rio Blanco, Colorado, Site, for the Long-Term Hydrologic Monitoring Program (LTHMP) on May 13 and 14, 2009. Samples were analyzed by the U.S. Environmental Protection Agency (EPA) Radiation&Indoor Environments National Laboratory in Las Vegas, Nevada. Samples were analyzed for gamma-emitting radionuclides by high-resolution gamma spectroscopy and tritium using the conventional and enriched methods.

Hydrocarbon group type determination in jet fuels by high performance liquid chromatography

NASA Technical Reports Server (NTRS)

Antoine, A. C.

1977-01-01

Thirty-two jet and diesel fuel samples of varying chemical composition and physical properties were prepared from oil shale and coal syncrudes. Hydrocarbon types in these samples were determined by a fluorescent indicator adsorption analysis, and the results from three laboratories are presented and compared. Two methods of rapid high performance liquid chromatography were used to analyze some of the samples, and these results are also presented and compared. Two samples of petroleum-based Jet A fuel are similarly analyzed.

Assessment of the Cast Stone Low-Temperature Waste Form Technology Coupled with Technetium Removal - 14379

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brown, Christopher F.; Rapko, Brian M.; Serne, R. Jeffrey

2014-03-03

The U.S. Department of Energy Office of Environmental Management (EM) is engaging the national laboratories to provide the scientific and technological rigor to support EM program and project planning, technology development and deployment, project execution, and assessment of program outcomes. As an early demonstration of this new responsibility, Pacific Northwest National Laboratory (PNNL) and Savannah River National Laboratory (SRNL) were chartered to implement a science and technology program addressing low-temperature waste forms for immobilization of DOE aqueous waste streams, including technetium removal as an implementing technology. As a first step, the laboratories examined the technical risks and uncertainties associated withmore » the Cast Stone waste immobilization and technetium removal projects at Hanford. Science and technology gaps were identified for work associated with 1) conducting performance assessments and risk assessments of waste form and disposal system performance, and 2) technetium chemistry in tank wastes and separation of technetium from waste processing streams. Technical approaches to address the science and technology gaps were identified and an initial sequencing priority was suggested. A subset of research was initiated in 2013 to begin addressing the most significant science and technology gaps. The purpose of this paper is to report progress made towards closing these gaps and provide notable highlights of results achieved to date.« less

Impact of axial velocity and transmembrane pressure (TMP) on ARP filter performance

DOE Office of Scientific and Technical Information (OSTI.GOV)

Poirier, M.; Burket, P.

2016-02-29

The Savannah River Site (SRS) is currently treating radioactive liquid waste with the Actinide Removal Process (ARP) and the Modular Caustic Side Solvent Extraction Unit (MCU). Recently, the low filter flux through the ARP of approximately 5 gallons per minute has limited the rate at which radioactive liquid waste can be treated. Salt Batch 6 had a lower processing rate and required frequent filter cleaning. Savannah River Remediation (SRR) has a desire to understand the causes of the low filter flux and to increase ARP/MCU throughput. One potential method for increasing filter flux is to adjust the axial velocity andmore » transmembrane pressure (TMP). SRR requested SRNL to conduct bench-scale filter tests to evaluate the effects of axial velocity and transmembrane pressure on crossflow filter flux. The objective of the testing was to determine whether increasing the axial velocity at the ARP could produce a significant increase in filter flux. The authors conducted the tests by preparing slurries containing 6.6 M sodium Salt Batch 6 supernate and 2.5 g MST/L, processing the slurry through a bench-scale crossflow filter unit at varying axial velocity and TMP, and measuring filter flux as a function of time.« less

TANK 18-F AND 19-F TANK FILL GROUT SCALE UP TEST SUMMARY

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stefanko, D.; Langton, C.

2012-01-03

High-level waste (HLW) tanks 18-F and 19-F have been isolated from FTF facilities. To complete operational closure the tanks will be filled with grout for the purpose of: (1) physically stabilizing the tanks, (2) limiting/eliminating vertical pathways to residual waste, (3) entombing waste removal equipment, (4) discouraging future intrusion, and (5) providing an alkaline, chemical reducing environment within the closure boundary to control speciation and solubility of select radionuclides. This report documents the results of a four cubic yard bulk fill scale up test on the grout formulation recommended for filling Tanks 18-F and 19-F. Details of the scale upmore » test are provided in a Test Plan. The work was authorized under a Technical Task Request (TTR), HLE-TTR-2011-008, and was performed according to Task Technical and Quality Assurance Plan (TTQAP), SRNL-RP-2011-00587. The bulk fill scale up test described in this report was intended to demonstrate proportioning, mixing, and transportation, of material produced in a full scale ready mix concrete batch plant. In addition, the material produced for the scale up test was characterized with respect to fresh properties, thermal properties, and compressive strength as a function of curing time.« less

Parking Lot Runoff Quality and Treatment Efficiency of a Stormwater-Filtration Device, Madison, Wisconsin, 2005-07

USGS Publications Warehouse

Horwatich, Judy A.; Bannerman, Roger T.

2010-01-01

To evaluate the treatment efficiency of a stormwater-filtration device (SFD) for potential use at Wisconsin Department of Transportation (WisDOT) park-and-ride facilities, a SFD was installed at an employee parking lot in downtown Madison, Wisconsin. This type of parking lot was chosen for the test site because the constituent concentrations and particle-size distributions (PSDs) were expected to be similar to those of a typical park-and-ride lot operated by WisDOT. The objective of this particular installation was to reduce loads of total suspended solids (TSS) in stormwater runoff to Lake Monona. This study also was designed to provide a range of treatment efficiencies expected for a SFD. Samples from the inlet and outlet were analyzed for 33 organic and inorganic constituents, including 18 polycyclic aromatic hydrocarbons (PAHs). Samples were also analyzed for physical properties, including PSD. Water-quality samples were collected for 51 runoff events from November 2005 to August 2007. Samples from all runoff events were analyzed for concentrations of suspended sediment (SS). Samples from 31 runoff events were analyzed for 15 constituents, samples from 15 runoff events were analyzed for PAHs, and samples from 36 events were analyzed for PSD. The treatment efficiency of the SFD was calculated using the summation of loads (SOL) and the efficiency ratio methods. Constituents for which the concentrations and (or) loads were decreased by the SFD include TSS, SS, volatile suspended solids, total phosphorous (TP), total copper, total zinc, and PAHs. The efficiency ratios for these constituents are 45, 37, 38, 55, 22, 5, and 46 percent, respectively. The SOLs for these constituents are 32, 37, 28, 36, 23, 8, and 48 percent, respectively. The SOL for chloride was -21 and the efficiency ratio was -18. Six chemical constituents or properties-dissolved phosphorus, chemical oxygen demand, dissolved zinc, total dissolved solids, dissolved chemical oxygen demand, and dissolved copper-were not included in the efficiency or SOL, because the difference between concentrations in samples from the inlet and outlet were not significant. Concentrations of TP and TSS were inexplicably high in samples at the inlet for one event.

No transmission of hepatitis E virus in pigs fed diets containing commercial spray-dried porcine plasma: a retrospective study of samples from several swine trials.

PubMed

Pujols, Joan; Rodríguez, Carmen; Navarro, Nuria; Pina-Pedrero, Sonia; Campbell, Joy M; Crenshaw, Joe; Polo, Javier

2014-12-24

Hepatitis E virus (HEV) has been reported in the human population and pigs are a recognized reservoir for HEV and a possible source of HEV transmission to humans. Spray-dried porcine plasma (SDPP) is an ingredient commonly used in feed for pigs around the world. Even though processing conditions used to produce SDPP should be adequate to inactivate HEV, it was of interest to analyze commercial SDPP samples for presence of genome and antibodies (AB) against HEV and to retrospectively analyze serum samples collected from pigs used in past experiments that had been fed diets containing either 0% or 8% SDPP to detect potential transmission of HEV as determined by seroconversion. Eighty-five commercial SDPP samples were analyzed by ELISA and 100% of them contained AB against HEV, while 22.4% (11 of 49 samples analyzed) were positive for HEV RNA. Frozen sera samples (n = 140) collected from 70 pigs used in past experiments that had been fed diets containing either 0% or 8% commercial SDPP was analyzed by ELISA for AB against HEV. Age of pigs at sera sampling ranged from 3 to 15 weeks and feeding duration of diets ranged from approximately 4 to 9 weeks. One lot of SDPP used in one experiment was analyzed and confirmed to contain HEV RNA. Regardless of the diet fed, some sera samples collected at the beginning of an experiment contained AB titer against HEV. These sera samples were collected from weaned pigs prior to feeding of the experimental diets and the HEV titer was probably from maternal origin. However, by the end of the experiments, HEV titer was not detected or had declined by more than 50% of the initial titer concentration. To our knowledge, this is the first study reporting presence of HEV AB titer and RNA in SDPP. Retrospective analysis of serum collected from pigs fed diets with SDPP revealed no indication of seroconversion to HEV. The results indicate that feeding SDPP in diets for pigs does not represent a risk of transmitting HEV, even though HEV genome may be detected in SDPP.

UNCERTAINTY IN SCALING NUTRIENT EXPORT COEFFICIENTS

EPA Science Inventory

The Innov-X XT400 portable XRF analyzer features a miniature, rugged x-ray tube excitation source for analyzing a wide variety of elements and sample materials, including alloys, environmental solids, and other analytical samples. The x-ray tube source and Light Element Analysis...

OpenMSI Arrayed Analysis Toolkit: Analyzing Spatially Defined Samples Using Mass Spectrometry Imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

de Raad, Markus; de Rond, Tristan; Rübel, Oliver

Mass spectrometry imaging (MSI) has primarily been applied in localizing biomolecules within biological matrices. Although well-suited, the application of MSI for comparing thousands of spatially defined spotted samples has been limited. One reason for this is a lack of suitable and accessible data processing tools for the analysis of large arrayed MSI sample sets. In this paper, the OpenMSI Arrayed Analysis Toolkit (OMAAT) is a software package that addresses the challenges of analyzing spatially defined samples in MSI data sets. OMAAT is written in Python and is integrated with OpenMSI (http://openmsi.nersc.gov), a platform for storing, sharing, and analyzing MSI data.more » By using a web-based python notebook (Jupyter), OMAAT is accessible to anyone without programming experience yet allows experienced users to leverage all features. OMAAT was evaluated by analyzing an MSI data set of a high-throughput glycoside hydrolase activity screen comprising 384 samples arrayed onto a NIMS surface at a 450 μm spacing, decreasing analysis time >100-fold while maintaining robust spot-finding. The utility of OMAAT was demonstrated for screening metabolic activities of different sized soil particles, including hydrolysis of sugars, revealing a pattern of size dependent activities. Finally, these results introduce OMAAT as an effective toolkit for analyzing spatially defined samples in MSI. OMAAT runs on all major operating systems, and the source code can be obtained from the following GitHub repository: https://github.com/biorack/omaat.« less

Instrumental and statistical methods for the comparison of class evidence

NASA Astrophysics Data System (ADS)

Liszewski, Elisa Anne

Trace evidence is a major field within forensic science. Association of trace evidence samples can be problematic due to sample heterogeneity and a lack of quantitative criteria for comparing spectra or chromatograms. The aim of this study is to evaluate different types of instrumentation for their ability to discriminate among samples of various types of trace evidence. Chemometric analysis, including techniques such as Agglomerative Hierarchical Clustering, Principal Components Analysis, and Discriminant Analysis, was employed to evaluate instrumental data. First, automotive clear coats were analyzed by using microspectrophotometry to collect UV absorption data. In total, 71 samples were analyzed with classification accuracy of 91.61%. An external validation was performed, resulting in a prediction accuracy of 81.11%. Next, fiber dyes were analyzed using UV-Visible microspectrophotometry. While several physical characteristics of cotton fiber can be identified and compared, fiber color is considered to be an excellent source of variation, and thus was examined in this study. Twelve dyes were employed, some being visually indistinguishable. Several different analyses and comparisons were done, including an inter-laboratory comparison and external validations. Lastly, common plastic samples and other polymers were analyzed using pyrolysis-gas chromatography/mass spectrometry, and their pyrolysis products were then analyzed using multivariate statistics. The classification accuracy varied dependent upon the number of classes chosen, but the plastics were grouped based on composition. The polymers were used as an external validation and misclassifications occurred with chlorinated samples all being placed into the category containing PVC.

Concentration data for anthropogenic organic compounds in ground water, surface water, and finished water of selected community water systems in the United States, 2002-05

USGS Publications Warehouse

Carter, Janet M.; Delzer, Gregory C.; Kingsbury, James A.; Hopple, Jessica A.

2007-01-01

The National Water-Quality Assessment Program of the U.S. Geological Survey began implementing Source Water-Quality Assessments (SWQAs) in 2001 that focus on characterizing the quality of source water and finished water of aquifers and major rivers used by some of the larger community water systems (CWSs) in the United States. As used for SWQA studies, source water is the raw (ambient) water collected at the supply well prior to water treatment (for ground water) or the raw (ambient) water collected from the river near the intake (for surface water), and finished water is the water that is treated and ready to be delivered to consumers. Finished water is collected before entering the distribution system. SWQA studies are conducted in two phases, and the objectives of SWQA studies are twofold: (1) to determine the occurrence and, for rivers, seasonal changes in concentrations of a broad list of anthropogenic organic compounds (AOCs) in aquifers and rivers that have some of the largest withdrawals for drinking-water supply (phase 1), and (2) for those AOCs found to occur most frequently in source water, characterize the extent to which these compounds are present in finished water (phase 2). These objectives were met for SWQA studies by collecting ground-water and surface-water (source) samples and analyzing these samples for 258 AOCs during phase 1. Samples from a subset of wells and surface-water sites located in areas with substantial agricultural production in the watershed were analyzed for 19 additional AOCs, for a total of 277 compounds analyzed for SWQA studies. The 277 compounds were classified according to the following 13 primary use or source groups: (1) disinfection by-products; (2) fumigant-related compounds; (3) fungicides; (4) gasoline hydrocarbons, oxygenates, and oxygenate degradates; (5) herbicides and herbicide degradates; (6) insecticides and insecticide degradates; (7) manufacturing additives; (8) organic synthesis compounds; (9) pavement- and combustion-derived compounds; (10) personal care and domestic use products; (11) plant- or animal-derived biochemicals; (12) refrigerants and propellants; and (13) solvents. Source and finished water samples were collected during phase 2 and analyzed for constituents that were detected frequently during phase 1. This report presents concentration data for AOCs in ground water, surface water, and finished water of CWSs sampled for SWQA studies during 2002-05. Specifically, this report presents the analytical results of samples collected during phase 1 including (1) samples from 221 wells that were analyzed for 258 AOCs; (2) monthly samples from 9 surface-water sites that were analyzed for 258 AOCs during phase 1; and (3) samples from a subset of the wells and surface-water sites located in areas with substantial agricultural production that were analyzed for 3 additional pesticides and 16 pesticide degradates. Samples collected during phase 2 were analyzed for selected AOCs that were detected most frequently in source water during phase 1 sampling; analytical results for phase 2 are presented for (1) samples of source water and finished water from 94 wells; and (2) samples of source water and finished water samples that were collected monthly and during selected flow conditions at 8 surface-water sites. Results of quality-assurance/quality-control samples collected for SWQA studies during 2002-05 also are presented.

Groundwater quality of the Gulf Coast aquifer system, Houston, Texas, 2010

USGS Publications Warehouse

Oden, Jeannette H.; Brown, Dexter W.; Oden, Timothy D.

2011-01-01

Gross alpha-particle activities and beta-particle activities for all 47 samples were analyzed at 72 hours after sample collection and again at 30 days after sample collection, allowing for the measurement of the activity of short-lived isotopes. Gross alpha-particle activities reported in this report were not adjusted for activity contributions by radon or uranium and, therefore, are conservatively high estimates if compared to the U.S. Environmental Protection Agency National Primary Drinking Water Regulation for adjusted gross alpha-particle activity. The gross alpha-particle activities at 30 days in the samples ranged from R0.60 to 25.5 picocuries per liter and at 72 hours ranged from 2.58 to 39.7 picocuries per liter, and the "R" preceding the value of 0.60 picocuries per liter refers to a nondetected result less than the sample-specific critical level. Gross beta-particle activities measured at 30 days ranged from 1.17 to 14.4 picocuries per liter and at 72 hours ranged from 1.97 to 4.4 picocuries per liter. Filtered uranium was detected in quantifiable amounts in all of the 47 wells sampled. The uranium concentrations ranged from 0.03 to 42.7 micrograms per liter. One sample was analyzed for carbon-14, and the amount of modern atmospheric carbon was reported as 0.2 percent. Six source-water samples collected from municipal supply wells were analyzed for radium-226, and all of the concentrations were considered detectable concentrations (greater than their associated sample-specific critical level). Three source-water samples collected were analyzed for radon-222, and all of the concentrations were substantially greater than the associated sample-specific critical level.

Lunar sample studies. [breccias basalts, and anorthosites

NASA Technical Reports Server (NTRS)

1977-01-01

Lunar samples discussed and the nature of their analyses are: (1) an Apollo 15 breccia which is thoroughly analyzed as to the nature of the mature regolith from which it derived and the time and nature of the lithification process, (2) two Apollo 11 and one Apollo 12 basalts analyzed in terms of chemistry, Cross-Iddings-Pirsson-Washington norms, mineralogy, and petrography, (3) eight Apollo 17 mare basalts, also analyzed in terms of chemistry, Cross-Iddings-Pirsson-Washington norms, mineralogy, and petrography. The first seven are shown to be chemically similar although of two main textural groups; the eighth is seen to be distinct in both chemistry and mineralogy, (4) a troctolitic clast from a Fra Mauro breccia, analyzed and contrasted with other high-temperature lunar mineral assemblages. Two basaltic clasts from the same breccia are shown to have affinities with rock 14053, and (5) the uranium-thorium-lead systematics of three Apollo 16 samples are determined; serious terrestrial-lead contamination of the first two samples is attributed to bandsaw cutting in the lunar curatorial facility.

Automated blood-sample handling in the clinical laboratory.

PubMed

Godolphin, W; Bodtker, K; Uyeno, D; Goh, L O

1990-09-01

The only significant advances in blood-taking in 25 years have been the disposable needle and evacuated blood-drawing tube. With the exception of a few isolated barcode experiments, most sample-tracking is performed through handwritten or computer-printed labels. Attempts to reduce the hazards of centrifugation have resulted in air-tight lids or chambers, the use of which is time-consuming and cumbersome. Most commonly used clinical analyzers require serum or plasma, distributed into specialized containers, unique to that analyzer. Aliquots for different tests are prepared by handpouring or pipetting. Moderate to large clinical laboratories perform so many different tests that even multi-analyzers performing multiple analyses on a single sample may account for only a portion of all tests ordered for a patient. Thus several aliquots of each specimen are usually required. We have developed a proprietary serial centrifuge and blood-collection tube suitable for incorporation into an automated or robotic sample-handling system. The system we propose is (a) safe--avoids or prevents biological danger to the many "handlers" of blood; (b) small--minimizes the amount of sample taken and space required to adapt to the needs of satellite and mobile testing, and direct interfacing with analyzers; (c) serial--permits each sample to be treated according to its own "merits," optimizes throughput, and facilitates flexible automation; and (d) smart--ensures quality results through monitoring and intelligent control of patient identification, sample characteristics, and separation process.

Evaluating the efficiency of environmental monitoring programs

USGS Publications Warehouse

Levine, Carrie R.; Yanai, Ruth D.; Lampman, Gregory G.; Burns, Douglas A.; Driscoll, Charles T.; Lawrence, Gregory B.; Lynch, Jason; Schoch, Nina

2014-01-01

Statistical uncertainty analyses can be used to improve the efficiency of environmental monitoring, allowing sampling designs to maximize information gained relative to resources required for data collection and analysis. In this paper, we illustrate four methods of data analysis appropriate to four types of environmental monitoring designs. To analyze a long-term record from a single site, we applied a general linear model to weekly stream chemistry data at Biscuit Brook, NY, to simulate the effects of reducing sampling effort and to evaluate statistical confidence in the detection of change over time. To illustrate a detectable difference analysis, we analyzed a one-time survey of mercury concentrations in loon tissues in lakes in the Adirondack Park, NY, demonstrating the effects of sampling intensity on statistical power and the selection of a resampling interval. To illustrate a bootstrapping method, we analyzed the plot-level sampling intensity of forest inventory at the Hubbard Brook Experimental Forest, NH, to quantify the sampling regime needed to achieve a desired confidence interval. Finally, to analyze time-series data from multiple sites, we assessed the number of lakes and the number of samples per year needed to monitor change over time in Adirondack lake chemistry using a repeated-measures mixed-effects model. Evaluations of time series and synoptic long-term monitoring data can help determine whether sampling should be re-allocated in space or time to optimize the use of financial and human resources.

Inter-laboratory comparison study on measuring semi-volatile organic chemicals in standards and air samples.

PubMed

Su, Yushan; Hung, Hayley

2010-11-01

Measurements of semi-volatile organic chemicals (SVOCs) were compared among 21 laboratories from 7 countries through the analysis of standards, a blind sample, an air extract, and an atmospheric dust sample. Measurement accuracy strongly depended on analytes, laboratories, and types of standards and samples. Intra-laboratory precision was generally good with relative standard deviations (RSDs) of triplicate injections <10% and with median differences of duplicate samples between 2.1 and 22%. Inter-laboratory variability, measured by RSDs of all measurements, was in the range of 2.8-58% in analyzing standards, and 6.9-190% in analyzing blind sample and air extract. Inter-laboratory precision was poorer when samples were subject to cleanup processes, or when SVOCs were quantified at low concentrations. In general, inter-laboratory differences up to a factor of 2 can be expected to analyze atmospheric SVOCs. When comparing air measurements from different laboratories, caution should be exercised if the data variability is less than the inter-laboratory differences. 2010. Published by Elsevier Ltd. All rights reserved.

Stability of steviol glycosides in several food matrices.

PubMed

Jooken, Etienne; Amery, Ruis; Struyf, Tom; Duquenne, Barbara; Geuns, Jan; Meesschaert, Boudewijn

2012-10-24

As steviol glycosides are now allowed as a food additive in the European market, it is important to assess the stability of these steviol glycosides after they have been added to different food matrices. We analyzed and tested the stability of steviol glycosides in semiskimmed milk, soy drink, fermented milk drink, ice cream, full-fat and skimmed set yogurt, dry biscuits, and jam. The fat was removed by centrifugation from the dairy and soy drink samples. Proteins were precipitated by the addition of acetonitrile and also removed by centrifugation. Samples of jam were extracted with water. Dry biscuits were extracted with ethanol. The resulting samples were concentrated with solid-phase extraction and analyzed by high-performance liquid chromatography on a C18 stationary phase and a gradient of acetonitrile/aqueous 25 mM phosphoric acid. The accuracy was checked using a standard addition on some samples. For assessing the stability of the steviol glycosides, samples were stored in conditions relevant to each food matrix and analyzed periodically. The results indicate that steviol glycosides can be analyzed with good precision and accuracy in these food categories. The recovery was between 96 and 103%. The method was also validated by standard addition, which showed excellent agreement with the external calibration curve. No sign of decomposition of steviol glycosides was found in any of the samples.

Mass spectrometer with electron source for reducing space charge effects in sample beam

DOEpatents

Houk, Robert S.; Praphairaksit, Narong

2003-10-14

A mass spectrometer includes an ion source which generates a beam including positive ions, a sampling interface which extracts a portion of the beam from the ion source to form a sample beam that travels along a path and has an excess of positive ions over at least part of the path, thereby causing space charge effects to occur in the sample beam due to the excess of positive ions in the sample beam, an electron source which adds electrons to the sample beam to reduce space charge repulsion between the positive ions in the sample beam, thereby reducing the space charge effects in the sample beam and producing a sample beam having reduced space charge effects, and a mass analyzer which analyzes the sample beam having reduced space charge effects.

Microcoulometric measurement of water in minerals

USGS Publications Warehouse

Cremer, M.; Elsheimer, H.N.; Escher, E.E.

1972-01-01

A DuPont Moisture Analyzer is used in a microcoulometric method for determining water in minerals. Certain modifications, which include the heating of the sample outside the instrument, protect the system from acid gases and insure the conversion of all hydrogen to water vapor. Moisture analyzer data are compared to concurrent data obtained by a modified Penfield method. In general, there is a positive bias of from 0.1 to 0.2% in the moisture analyzer results and a similarity of bias in minerals of the same kind. Inhomogeneity, sample size, and moisture pick-up are invoked to explain deviations. The method is particularly applicable to small samples. ?? 1972.

Analysis of volatile organic compounds. [trace amounts of organic volatiles in gas samples

NASA Technical Reports Server (NTRS)

Zlatkis, A. (Inventor)

1977-01-01

An apparatus and method are described for reproducibly analyzing trace amounts of a large number of organic volatiles existing in a gas sample. Direct injection of the trapped volatiles into a cryogenic percolum provides a sharply defined plug. Applications of the method include: (1) analyzing the headspace gas of body fluids and comparing a profile of the organic volatiles with standard profiles for the detection and monitoring of disease; (2) analyzing the headspace gas of foods and beverages and comparing the profile with standard profiles to monitor and control flavor and aroma; and (3) analyses for determining the organic pollutants in air or water samples.

Chemical Characterization of an Envelope B/D Sample from Hanford Tank 241-AZ-102

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hay, M.S.

2000-08-23

A sample from Hanford waste tank 241-AZ-102 was received at the Savannah River Technology Center (SRTC) and chemically characterized. The sample containing supernate and a small amount of sludge solids was analyzed as-received. The filtered supernatant liquid, the total dried solids of the sample, and the washed insoluble solids obtained from filtration of the sample were analyzed. A mass balance calculation of the three fractions of the sample analyzed indicate the analytical results appear relatively self-consistent for major components of the sample. However, some inconsistency was observed between results were more than one method of determination was employed and formore » species present in low concentrations. The actinides isotopes, plutonium, americium, and curium, present analytical challenges due to the low concentration of these species and the potential for introduction of small amounts of contamination during sampling handling resulting in large uncertainties. A direct comparison to previous analyses of material from tank 241-AZ-102 showed good agreement with the filtered supernatant liquid. However, the comparison of solids data showed poor agreement. The poor agreement shown between the current results for the solids samples and previous analyses most likely results from the uncertainties associated with obtaining small solids samples from a large non-homogenized waste tank.« less

Capillary Electrophoresis Analysis of Organic Amines and Amino Acids in Saline and Acidic Samples Using the Mars Organic Analyzer

NASA Astrophysics Data System (ADS)

Stockton, Amanda M.; Chiesl, Thomas N.; Lowenstein, Tim K.; Amashukeli, Xenia; Grunthaner, Frank; Mathies, Richard A.

2009-11-01

The Mars Organic Analyzer (MOA) has enabled the sensitive detection of amino acid and amine biomarkers in laboratory standards and in a variety of field sample tests. However, the MOA is challenged when samples are extremely acidic and saline or contain polyvalent cations. Here, we have optimized the MOA analysis, sample labeling, and sample dilution buffers to handle such challenging samples more robustly. Higher ionic strength buffer systems with pKa values near pH 9 were developed to provide better buffering capacity and salt tolerance. The addition of ethylaminediaminetetraacetic acid (EDTA) ameliorates the negative effects of multivalent cations. The optimized protocol utilizes a 75 mM borate buffer (pH 9.5) for Pacific Blue labeling of amines and amino acids. After labeling, 50 mM (final concentration) EDTA is added to samples containing divalent cations to ameliorate their effects. This optimized protocol was used to successfully analyze amino acids in a saturated brine sample from Saline Valley, California, and a subcritical water extract of a highly acidic sample from the Río Tinto, Spain. This work expands the analytical capabilities of the MOA and increases its sensitivity and robustness for samples from extraterrestrial environments that may exhibit pH and salt extremes as well as metal ions.

Capillary electrophoresis analysis of organic amines and amino acids in saline and acidic samples using the Mars organic analyzer.

PubMed

Stockton, Amanda M; Chiesl, Thomas N; Lowenstein, Tim K; Amashukeli, Xenia; Grunthaner, Frank; Mathies, Richard A

2009-11-01

The Mars Organic Analyzer (MOA) has enabled the sensitive detection of amino acid and amine biomarkers in laboratory standards and in a variety of field sample tests. However, the MOA is challenged when samples are extremely acidic and saline or contain polyvalent cations. Here, we have optimized the MOA analysis, sample labeling, and sample dilution buffers to handle such challenging samples more robustly. Higher ionic strength buffer systems with pK(a) values near pH 9 were developed to provide better buffering capacity and salt tolerance. The addition of ethylaminediaminetetraacetic acid (EDTA) ameliorates the negative effects of multivalent cations. The optimized protocol utilizes a 75 mM borate buffer (pH 9.5) for Pacific Blue labeling of amines and amino acids. After labeling, 50 mM (final concentration) EDTA is added to samples containing divalent cations to ameliorate their effects. This optimized protocol was used to successfully analyze amino acids in a saturated brine sample from Saline Valley, California, and a subcritical water extract of a highly acidic sample from the Río Tinto, Spain. This work expands the analytical capabilities of the MOA and increases its sensitivity and robustness for samples from extraterrestrial environments that may exhibit pH and salt extremes as well as metal ions.

Determination of trace metals in drinking water in Irbid City-Northern Jordan.

PubMed

Alomary, Ahmed

2013-02-01

Drinking water samples from Irbid, the second populated city in Jordan were analyzed for trace metals (As, Ba, Cd, Pb, Cr, Cu, Fe, Zn, Mn, Ni, and Se) content. The study was undertaken to determine if the metal concentrations were within the national and international guidelines. A total of 90 drinking water samples were collected from Al-Yarmouk University area. The samples were collected from three different water types: tap water (TW), home-purified water (HPW), and plant-purified water (PPW). All the samples were analyzed for trace metals using an inductively coupled plasma-optical emission spectrometry. All the samples analyzed were within the United States Environmental Protection Agency admissible pH limit (6.5-8.5). The results showed that concentrations of the trace metals vary significantly between the three drinking water types. The results showed that HPW samples have the lowest level of trace metals and the concentrations of some essential trace metals in these samples are less than the recommended amounts. Slight differences in the metal contents were found between HPW samples, little differences between PPW samples; however, significant differences were found between TW samples. Although some TW samples showed high levels of trace metals, however, the mean level of most elements determined in the samples were well within the Jordanian standards as well as the World Health Organization standards for drinking water.

An on-line database for human milk composition in China.

PubMed

Yin, Shi-An; Yang, Zhen-Yu

2016-12-01

Understanding human milk composition is critical for setting nutrient recommended intakes (RNIs) for both infants and lactating women. However, nationwide human milk composition remains unavailable in China. Through cross-sectional study, human milk samples from 11 provinces in China were collected and their compositions were analyzed. Nutritional and health status of the lactating women and their infants were evaluated through questionnaire, physical examination and biochemical indicators. A total of 6,481 breast milk samples including colostrum (1,859), transitional milk (1,235) and mature milk (3,387) were collected. Contents of protein, fat, lactose, total solid and energy of more than 4,500 samples were analyzed using a human milk analyzer. About 2,000 samples were randomly selected for 24 mineral analyses. Free B-vitamins including thiamin, riboflavin, pyridoxal, pyridomine, pyridoxamine, nicotinamide, nicotinic acid, flavin adenine dinucleotide (FAD), biotin and pantothenic acid were analyzed in 1,800 samples. Amino acids (~800) and proteins (alpha-lactoalbumin, beta-casein, and lactoferrin) were analyzed. In addition, serum retinol and carotenoids, 25(OH)D, vitamin B-12, folic acid, ferritin and biochemical indicators (n=1,200 to 2,000) were analysed in the lactating women who provided the breast milk. Ongoing work: Fatty acids (C4-C24), fatsoluble vitamins and carotenoids, are on-going analysis. A regional breast milk compositional database is at an advanced stage of development in China with the intention that it be available on-line.

Sample analysis at Mars

NASA Astrophysics Data System (ADS)

Coll, P.; Cabane, M.; Mahaffy, P. R.; Brinckerhoff, W. B.; Sam Team

The next landed missions to Mars, such as the planned Mars Science Laboratory and ExoMars, will require sample analysis capabilities refined well beyond what has been flown to date. A key science objective driving this requirement is the determination of the carbon inventory of Mars, and particularly the detection of organic compounds. The Sample Analysis at Mars (SAM) suite consists of a group of tightly-integrated experiments that would analyze samples delivered directly from a coring drill or by a facility sample processing and delivery (SPAD) mechanism. SAM consists of an advanced GC/MS system and a laser desorption mass spectrometer (LDMS). The combined capabilities of these techniques can address Mars science objectives with much improved sensitivity, resolution, and analytical breadth over what has been previously possible in situ. The GC/MS system analyzes the bulk composition (both molecular and isotopic) of solid-phase and atmospheric samples. Solid samples are introduced with a highly flexible chemical derivatization/pyrolysis subsystem (Pyr/GC/MS) that is significantly more capable than the mass spectrometers on Viking. The LDMS analyzes local elemental and molecular composition in solid samples vaporized and ionized with a pulsed laser. We will describe how each of these capabilities has particular strengths that can achieve key measurement objectives at Mars. In addition, the close codevelopment of the GC/MS and LDMS along with a sample manipulation system enables the the sharing of resources, the correlation of results, and the utilization of certain approaches that would not be possible with separate instruments. For instance, the same samples could be analyzed with more than one technique, increasing efficiency and providing cross-checks for quantification. There is also the possibility of combining methods, such as by permitting TOF-MS analyses of evolved gas (Pyr/EI-TOF-MS) or GC/MS analyses of laser evaporated gas (LD-GC/MS).

AFM fluid delivery/liquid extraction surface sampling/electrostatic spray cantilever probe

DOEpatents

Van Berkel, Gary J.

2015-06-23

An electrospray system comprises a liquid extraction surface sampling probe. The probe comprises a probe body having a liquid inlet and a liquid outlet, and having a liquid extraction tip. A solvent delivery conduit is provided for receiving solvent liquid from the liquid inlet and delivering the solvent liquid to the liquid extraction tip. An open liquid extraction channel extends across an exterior surface of the probe body from the liquid extraction tip to the liquid outlet. An electrospray emitter tip is in liquid communication with the liquid outlet of the liquid extraction surface sampling probe. A system for analyzing samples, a liquid junction surface sampling system, and a method of analyzing samples are also disclosed.

Trace elements by instrumental neutron activation analysis for pollution monitoring

NASA Technical Reports Server (NTRS)

Sheibley, D. W.

1975-01-01

Methods and technology were developed to analyze 1000 samples/yr of coal and other pollution-related samples. The complete trace element analysis of 20-24 samples/wk averaged 3-3.5 man-hours/sample. The computerized data reduction scheme could identify and report data on as many as 56 elements. In addition to coal, samples of fly ash, bottom ash, crude oil, fuel oil, residual oil, gasoline, jet fuel, kerosene, filtered air particulates, ore, stack scrubber water, clam tissue, crab shells, river sediment and water, and corn were analyzed. Precision of the method was plus or minus 25% based on all elements reported in coal and other sample matrices. Overall accuracy was estimated at 50%.

"Adultspan" Publication Patterns: Author and Article Characteristics from 1999 to 2009

ERIC Educational Resources Information Center

Erford, Bradley T.; Clark, Kelly H.; Erford, Breann M.

2011-01-01

Publication patterns of articles in "Adultspan" from 1999 to 2009 were reviewed. Author characteristics and article content were analyzed to determine trends over time. Research articles were analyzed specifically for type of research design, classification, sampling method, types of participants, sample size, types of statistics used, and…

NOAA PMEL Station Chemistry Data

DOE Data Explorer

Quinn, Patricia

2008-04-04

Submicron and supermicron samples are analyzed by ion chromatography for Cl-, NO3-, SO4-2, Na+, NH4+, K+, Mg2+, and Ca+2. The analysis of MSA-, Br-, and oxalate has been added to some stations. Samples also are analyzed for total mass by gravimetric analysis at 55 +/- 5% RH.

9 CFR 590.580 - Laboratory tests and analyses.

Code of Federal Regulations, 2011 CFR

2011-01-01

... dried egg whites shall be sampled and analyzed for the presence of Salmonellae in accordance with such...) of this section, are analyzed for the presence of Salmonella, the plant shall immediately advise the inspector of any such samples which are determined to be Salmonella positive. (d) USDA will draw...

9 CFR 590.580 - Laboratory tests and analyses.

Code of Federal Regulations, 2010 CFR

2010-01-01

... dried egg whites shall be sampled and analyzed for the presence of Salmonellae in accordance with such...) of this section, are analyzed for the presence of Salmonella, the plant shall immediately advise the inspector of any such samples which are determined to be Salmonella positive. (d) USDA will draw...

40 CFR 86.317-79 - Hydrocarbon analyzer specifications.

Code of Federal Regulations, 2012 CFR

2012-07-01

... flame ionization detector (HFID) analyzer. (b) Option. A non-heated flame ionization detector (FID) that... temperature oven housing the detector and sample-handling components. It shall maintain temperature with 2 °C of the set point. The detector, oven, and sample-handling components within the oven shall be...

40 CFR 86.317-79 - Hydrocarbon analyzer specifications.

Code of Federal Regulations, 2010 CFR

2010-07-01

... flame ionization detector (HFID) analyzer. (b) Option. A non-heated flame ionization detector (FID) that... temperature oven housing the detector and sample-handling components. It shall maintain temperature with 2 °C of the set point. The detector, oven, and sample-handling components within the oven shall be...

40 CFR 86.317-79 - Hydrocarbon analyzer specifications.

Code of Federal Regulations, 2011 CFR

2011-07-01

... flame ionization detector (HFID) analyzer. (b) Option. A non-heated flame ionization detector (FID) that... temperature oven housing the detector and sample-handling components. It shall maintain temperature with 2 °C of the set point. The detector, oven, and sample-handling components within the oven shall be...

40 CFR 86.317-79 - Hydrocarbon analyzer specifications.

Code of Federal Regulations, 2013 CFR

2013-07-01

... flame ionization detector (HFID) analyzer. (b) Option. A non-heated flame ionization detector (FID) that... temperature oven housing the detector and sample-handling components. It shall maintain temperature with 2 °C of the set point. The detector, oven, and sample-handling components within the oven shall be...

Injection molding of iPP samples in controlled conditions and resulting morphology

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sessa, Nino, E-mail: ninosessa.ns@gmail.com; De Santis, Felice, E-mail: fedesantis@unisa.it; Pantani, Roberto, E-mail: rpantani@unisa.it

2015-12-17

Injection molded parts are driven down in size and weight especially for electronic applications. In this work, an investigation was carried out on the process of injection molding of thin iPP samples and on the morphology of these parts. Melt flow in the mold cavity was analyzed and described with a mathematical model. Influence of mold temperature and injection pressure was analyzed. Samples orientation was studied using optical microscopy.

Short communication: Analytical method and amount of preservative added to milk samples may alter milk urea nitrogen measurements.

PubMed

Weeks, Holley L; Hristov, Alexander N

2017-02-01

Milk urea N (MUN) is used by dairy nutritionists and producers to monitor dietary protein intake and is indicative of N utilization in lactating dairy cows. Two experiments were conducted to explore discrepancies in MUN results provided by 3 milk processing laboratories using different methods. An additional experiment was conducted to evaluate the effect of 2-bromo-2-nitropropane-1, 3-diol (bronopol) on MUN analysis. In experiment 1, 10 replicates of bulk tank milk samples, collected from the Pennsylvania State University's Dairy Center over 5 consecutive days, were sent to 3 milk processing laboratories in Pennsylvania. Average MUN differed between laboratory A (14.9 ± 0.40 mg/dL; analyzed on MilkoScan 4000; Foss, Hillerød, Denmark), laboratory B (6.5 ± 0.17 mg/dL; MilkoScan FT + 6000), and laboratory C (7.4 ± 0.36 mg/dL; MilkoScan 6000). In experiment 2, milk samples were spiked with urea at 0 (7.3 to 15.0 mg/dL, depending on the laboratory analyzing the samples), 17.2, 34.2, and 51.5 mg/dL of milk. Two 35-mL samples from each urea level were sent to the 3 laboratories used in experiment 1. Average analyzed MUN was greater than predicted (calculated for each laboratory based on the control; 0 mg of added urea): for laboratory A (23.2 vs. 21.0 mg/dL), laboratory B (18.0 vs. 13.3 mg/dL), and laboratory C (20.6 vs. 15.2 mg/dL). In experiment 3, replicated milk samples were preserved with 0 to 1.35 mg of bronopol/mL of milk and submitted to one milk processing laboratory that analyzed MUN using 2 different methods. Milk samples with increasing amounts of bronopol ranged in MUN concentration from 7.7 to 11.9 mg/dL and from 9.0 to 9.3 mg/dL when analyzed on MilkoScan 4000 or CL 10 (EuroChem, Moscow, Russia), respectively. In conclusion, measured MUN concentrations varied due to analytical procedure used by milk processing laboratories and were affected by the amount of bronopol used to preserve milk sample, when milk was analyzed using a mid-infrared analyzer. Thus, it is important to maintain consistency in milk sample preservation and analysis to ensure precision of MUN results. Copyright © 2017 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

COST-EFFECTIVE SAMPLING FOR SPATIALLY DISTRIBUTED PHENOMENA

EPA Science Inventory

Various measures of sampling plan cost and loss are developed and analyzed as they relate to a variety of multidisciplinary sampling techniques. The sampling choices examined include methods from design-based sampling, model-based sampling, and geostatistics. Graphs and tables ar...

Economic and workflow analysis of a blood bank automated system.

PubMed

Shin, Kyung-Hwa; Kim, Hyung Hoi; Chang, Chulhun L; Lee, Eun Yup

2013-07-01

This study compared the estimated costs and times required for ABO/Rh(D) typing and unexpected antibody screening using an automated system and manual methods. The total cost included direct and labor costs. Labor costs were calculated on the basis of the average operator salaries and unit values (minutes), which was the hands-on time required to test one sample. To estimate unit values, workflows were recorded on video, and the time required for each process was analyzed separately. The unit values of ABO/Rh(D) typing using the manual method were 5.65 and 8.1 min during regular and unsocial working hours, respectively. The unit value was less than 3.5 min when several samples were tested simultaneously. The unit value for unexpected antibody screening was 2.6 min. The unit values using the automated method for ABO/Rh(D) typing, unexpected antibody screening, and both simultaneously were all 1.5 min. The total cost of ABO/Rh(D) typing of only one sample using the automated analyzer was lower than that of testing only one sample using the manual technique but higher than that of testing several samples simultaneously. The total cost of unexpected antibody screening using an automated analyzer was less than that using the manual method. ABO/Rh(D) typing using an automated analyzer incurs a lower unit value and cost than that using the manual technique when only one sample is tested at a time. Unexpected antibody screening using an automated analyzer always incurs a lower unit value and cost than that using the manual technique.

DEVELOPMENT OF AN INSOLUBLE SALT SIMULANT TO SUPPORT ENHANCED CHEMICAL CLEANING TESTS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eibling, R

The closure process for high level waste tanks at the Savannah River Site will require dissolution of the crystallized salts that are currently stored in many of the tanks. The insoluble residue from salt dissolution is planned to be removed by an Enhanced Chemical Cleaning (ECC) process. Development of a chemical cleaning process requires an insoluble salt simulant to support evaluation tests of different cleaning methods. The Process Science and Engineering section of SRNL has been asked to develop an insoluble salt simulant for use in testing potential ECC processes (HLE-TTR-2007-017). An insoluble salt simulant has been developed based uponmore » the residues from salt dissolution of saltcake core samples from Tank 28F. The simulant was developed for use in testing SRS waste tank chemical cleaning methods. Based on the results of the simulant development process, the following observations were developed: (1) A composition based on the presence of 10.35 grams oxalate and 4.68 grams carbonate per 100 grams solids produces a sufficiently insoluble solids simulant. (2) Aluminum observed in the solids remaining from actual waste salt dissolution tests is probably precipitated from sodium aluminate due to the low hydroxide content of the saltcake. (3) In-situ generation of aluminum hydroxide (by use of aluminate as the Al source) appears to trap additional salts in the simulant in a manner similar to that expected for actual waste samples. (4) Alternative compositions are possible with higher oxalate levels and lower carbonate levels. (5) The maximum oxalate level is limited by the required Na content of the insoluble solids. (6) Periodic mixing may help to limit crystal growth in this type of salt simulant. (7) Long term storage of an insoluble salt simulant is likely to produce a material that can not be easily removed from the storage container. Production of a relatively fresh simulant is best if pumping the simulant is necessary for testing purposes. The insoluble salt simulant described in this report represents the initial attempt to represent the material which may be encountered during final waste removal and tank cleaning. The final selected simulant was produced by heating and evaporation of a salt slurry sample to remove excess water and promote formation and precipitation of solids with solubility characteristics which are consistent with actual tank insoluble salt samples. The exact anion composition of the final product solids is not explicitly known since the chemical components in the final product are distributed between the solid and liquid phases. By combining the liquid phase analyses and total solids analysis with mass balance requirements a calculated composition of assumed simple compounds was obtained and is shown in Table 0-1. Additional improvements to and further characterization of the insoluble salt simulant are possible. During the development of these simulants it was recognized that: (1) Additional waste characterization on the residues from salt dissolution tests with actual waste samples to determine the amount of species such as carbonate, oxalate and aluminosilicate would allow fewer assumptions to be made in constructing an insoluble salt simulant. (2) The tank history will impact the amount and type of insoluble solids that exist in the salt dissolution solids. Varying the method of simulant production (elevated temperature processing time, degree of evaporation, amount of mixing (shear) during preparation, etc.) should be tested.« less

Groundwater quality in the Genesee River Basin, New York, 2010

USGS Publications Warehouse

Reddy, James E.

2012-01-01

Water samples collected from eight production wells and eight private residential wells in the Genesee River Basin from September through December 2010 were analyzed to characterize the groundwater quality in the basin. Eight of the wells were completed in sand and gravel aquifers, and eight were finished in bedrock aquifers. Three of the 16 wells were sampled in the first Genesee River Basin study during 2005-2006. Water samples from the 2010 study were analyzed for 147 physiochemical properties and constituents that included major ions, nutrients, trace elements, radionuclides, pesticides, volatile organic compounds (VOCs), and indicator bacteria. Results of the water-quality analyses are presented in tabular form for individual wells, and summary statistics for specific constituents are presented by aquifer type. The results are compared with Federal and New York State drinking-water standards, which typically are identical. The results indicate that groundwater generally is of acceptable quality, although concentrations of the following constituents exceeded current or proposed Federal or New York State drinking-water standards at each of the 16 wells sampled: color (one sample), sodium (three samples), sulfate (three samples), total dissolved solids (four samples), aluminum (one sample), arsenic (two samples), copper (one sample), iron (nine samples), manganese (eight samples), radon-222 (nine samples), and total coliform bacteria (six samples). Existing drinking-water standards for pH, chloride, fluoride, nitrate, nitrite, antimony, barium, beryllium, cadmium, chromium, lead, mercury, selenium, silver, thallium, zinc, gross alpha radioactivity, uranium, fecal coliform, Escherichia coli, and heterotrophic bacteria were not exceeded in any of the samples collected. None of the pesticides and VOCs analyzed exceeded existing drinking-water standards.

Groundwater quality in western New York, 2011

USGS Publications Warehouse

Reddy, James E.

2013-01-01

Water samples collected from 16 production wells and 15 private residential wells in western New York from July through November 2011 were analyzed to characterize the groundwater quality. Fifteen of the wells were finished in sand and gravel aquifers, and 16 were finished in bedrock aquifers. Six of the 31 wells were sampled in a previous western New York study, which was conducted in 2006. Water samples from the 2011 study were analyzed for 147 physiochemical properties and constituents that included major ions, nutrients, trace elements, radionuclides, pesticides, volatile organic compounds (VOCs), and indicator bacteria. Results of the water-quality analyses are presented in tabular form for individual wells, and summary statistics for specific constituents are presented by aquifer type. The results are compared with Federal and New York State drinking-water standards, which typically are identical. The results indicate that groundwater generally is of acceptable quality, although at 30 of the 31 wells sampled, at least one of the following constituents was detected at a concentration that exceeded current or proposed Federal or New York State drinking-water standards: pH (two samples), sodium (eight samples), sulfate (three samples), total dissolved solids (nine samples), aluminum (two samples), arsenic (one sample), iron (ten samples), manganese (twelve samples), radon-222 (sixteen samples), benzene (one sample), and total coliform bacteria (nine samples). Existing drinking-water standards for color, chloride, fluoride, nitrate, nitrite, antimony, barium, beryllium, cadmium, chromium, copper, lead, mercury, selenium, silver, thallium, zinc, gross alpha radioactivity, uranium, fecal coliform, Escherichia coli, and heterotrophic bacteria were not exceeded in any of the samples collected. None of the pesticides analyzed exceeded existing drinking-water standards.

Probabilistic Round Trip Contamination Analysis of a Mars Sample Acquisition and Handling Process Using Markovian Decompositions

NASA Technical Reports Server (NTRS)

Hudson, Nicolas; Lin, Ying; Barengoltz, Jack

2010-01-01

A method for evaluating the probability of a Viable Earth Microorganism (VEM) contaminating a sample during the sample acquisition and handling (SAH) process of a potential future Mars Sample Return mission is developed. A scenario where multiple core samples would be acquired using a rotary percussive coring tool, deployed from an arm on a MER class rover is analyzed. The analysis is conducted in a structured way by decomposing sample acquisition and handling process into a series of discrete time steps, and breaking the physical system into a set of relevant components. At each discrete time step, two key functions are defined: The probability of a VEM being released from each component, and the transport matrix, which represents the probability of VEM transport from one component to another. By defining the expected the number of VEMs on each component at the start of the sampling process, these decompositions allow the expected number of VEMs on each component at each sampling step to be represented as a Markov chain. This formalism provides a rigorous mathematical framework in which to analyze the probability of a VEM entering the sample chain, as well as making the analysis tractable by breaking the process down into small analyzable steps.

Water-quality assessment of the Rio Grande Valley, Colorado, New Mexico and Texas; organic compounds and trace elements in bed sediment and fish tissue, 1992-93

USGS Publications Warehouse

Carter, L.F.; Anderholm, S.K.

1997-01-01

The occurrence and distribution of contaminants in aquatic systems are major components of the National Water-Quality Assessment (NAWQA) Program. Bed-sediment samples were collected at 18 sites in the Rio Grande Valley study unit between September 1992 and March 1993 to characterize the geographic distribution of organic compounds, including chlorinated insecticides, polychlorinated biphenyls (PCB's), and other chlorinated hydrocarbons, and also trace elements. Two-millimeter-size- fraction sediment was analyzed for organic compounds and less than 63-micron-size-fraction sediment was analyzed for trace elements. Concentrations of p,p'-DDE were detected in 33 percent of the bed-sediment samples. With the exception of DDT-related compounds, no other organochlorine insecticides or polychlorinated biphenyls were detected in samples of bed sediment. Whole-body fish samples were collected at 11 of the bed- sediment sites and analyzed for organic compounds. Organic compounds were reported more frequently in samples of fish, and more types of organic compounds were found in whole-body fish samples than in bed-sediment samples. Concentrations of p,p'-DDE were detected in 91 percent of whole-body fish samples. Polychlorinated biphenyls, cis-chlordane, trans-chlordane, trans- nonachlor, and hexachlorobenzene were other organic compounds detected in whole-body samples of fish from at least one site. Because of the extent of mineralized areas in the Rio Grande Basin arsenic, cadmium, copper, lead, mercury, selenium, and zinc concentrations in bed-sediment samples could represent natural conditions at most sites. However, a combination of natural conditions and human activities appears to be associated with elevated trace-element concentrations in the bed-sediment sample from the site Rio Grande near Creede, Colorado, because this sample exceeded the background trace-element concentrations calculated for this study. Fish-liver samples were collected at 12 of the bed-sediment sites and analyzed for trace elements. Certain trace elements were detected at higher concentrations in fish-liver samples than in bed-sediment samples from the same site. Both bed-sediment and fish-tissue samples are necessary for a complete environmental assessment of the occurrence and distribution of trace elements.

Preliminary Results on the Surface of a New Fe-Based Metallic Material after “In Vivo” Maintaining

NASA Astrophysics Data System (ADS)

Săndulache, F.; Stanciu, S.; Cimpoeşu, N.; Stanciu, T.; Cimpoeșu, R.; Enache, A.; Baciu, R.

2017-06-01

Abstract A new Fe-based alloy was obtained using UltraCast melting equipment. The alloy, after mechanical processing, was implanted in five rabbit specimens (with respect for the “in-bone” procedure). After 30 days of implantation the samples were recovered and analyzed by weight and surface state meanings. Scanning electron microscopy technique was used to determine the new compounds morphology from the metallic surface and X-ray dispersive energy spectroscopy for chemical analyze results. A bond between the metallic material and biological material of the bone was observed through increasing of sample weight and by SEM images. After the first set of tests, as the samples were extracted and biologically cleaned, the samples were ultrasonically cleaned and re-analyzed in order to establish the stability of the chemical compounds.

New approach for cystic fibrosis diagnosis based on chloride/potassium ratio analyzed in non-invasively obtained skin-wipe sweat samples by capillary electrophoresis with contactless conductometric detection.

PubMed

Ďurč, Pavol; Foret, František; Pokojová, Eva; Homola, Lukáš; Skřičková, Jana; Herout, Vladimír; Dastych, Milan; Vinohradská, Hana; Kubáň, Petr

2017-05-01

A new approach for sweat analysis used in cystic fibrosis (CF) diagnosis is proposed. It consists of a noninvasive skin-wipe sampling followed by analysis of target ions using capillary electrophoresis with contactless conductometric detection (C4D). The skin-wipe sampling consists of wiping a defined skin area with precleaned cotton swab moistened with 100 μL deionized water. The skin-wipe sample is then extracted for 3 min into 400 μL deionized water, and the extract is analyzed directly. The developed sampling method is cheap, simple, fast, and painless, and can replace the conventional pilocarpine-induced sweat chloride test commonly applied in CF diagnosis. The aqueous extract of the skin-wipe sample content is analyzed simultaneously by capillary electrophoresis with contactless conductometric detection using a double opposite end injection. A 20 mmol/L L-histidine/2-(N-morpholino)ethanesulfonic acid and 2 mmol/L 18-crown-6 at pH 6 electrolyte can separate all the major ions in less than 7 min. Skin-wipe sample extracts from 30 study participants-ten adult patients with CF (25-50 years old), ten pediatric patients with CF (1-15 years old), and ten healthy control individuals (1-18 years old)-were obtained and analyzed. From the analyzed ions in all samples, a significant difference between chloride and potassium concentrations was found in the CF patients and healthy controls. We propose the use of the Cl - /K + ratio rather than the absolute Cl - concentration and a cutoff value of 4 in skin-wipe sample extracts as an alternative to the conventional sweat chloride analysis. The proposed Cl - /K + ion ratio proved to be a more reliable indicator, is independent of the patient's age, and allows better differentiation between non-CF individuals and CF patients having intermediate values on the Cl - sweat test. Figure New approach for cystic fibrosis diagnosis based on skin-wipe sampling of forearm and analysis of ionic content (Cl - /K + ratio) in skin-wipe extracts by capillary electrophoresis with contactless conductometric detection.

Rainfall, Discharge, and Water-Quality Data During Stormwater Monitoring, July 1, 2008, to June 30, 2009 - Halawa Stream Drainage Basin and the H-1 Storm Drain, Oahu, Hawaii

USGS Publications Warehouse

Presley, Todd K.; Jamison, Marcael T.J.

2009-01-01

Storm runoff water-quality samples were collected as part of the State of Hawaii Department of Transportation Stormwater Monitoring Program. The program is designed to assess the effects of highway runoff and urban runoff on Halawa Stream, and to assess the effects from the H-1 storm drain on Manoa Stream. For this program, rainfall data were collected at three stations, continuous discharge data at five stations, and water-quality data at six stations, which include the five continuous discharge stations. This report summarizes rainfall, discharge, and water-quality data collected between July 1, 2008, and June 30, 2009. Within the Halawa Stream drainage area, three storms (October 25 and December 11, 2008, and February 3, 2009) were sampled during July 1, 2008, to June 30, 2009. A total of 43 environmental samples were collected during these three storms. During the storm of October 25, 2009, 31 samples were collected and analyzed individually for metals only. The other 12 samples from the other two storms were analyzed for some or all of the following analytes: total suspended solids, total dissolved solids, nutrients, chemical oxygen demand, and selected trace metals (cadmium, chromium, copper, lead, and zinc). Additionally, grab samples were analyzed for some or all of the following analytes: oil and grease, total petroleum hydrocarbons, fecal coliform, and biological oxygen demand. Some grab and composite samples were analyzed for only a partial list of these analytes, either because samples could not be delivered to the laboratory in a timely manner, or an insufficient volume of sample was collected by the automatic samplers. Two quality-assurance/quality-control samples were collected after cleaning automatic sampler lines to verify that the sampling lines were not contaminated. Four environmental samples were collected at the H-1 Storm Drain during July 1, 2008, to June 30, 2009. An oil and grease sample and a composite sample were collected during the storm on November 15, 2008, and two composite samples were collected during the January 11, 2009, storm. All samples at this site were collected using an automatic sampler. Samples were analyzed for some or all of the following analytes: total suspended solids, nutrients, oil and grease, total petroleum hydrocarbons, and selected trace metals (cadmium, chromium, copper, lead, nickel, and zinc). One qualityassurance/quality-control sample was collected after cleaning automatic sampler lines to verify that the sampling lines were not contaminated. During the storm of January 11, 2009, the two composite samples collected at H-1 Storm Drain were collected about three hours apart. Higher constituent concentrations were detected in the first 2 composite sample relative to the second composite sample, although the average discharge was higher during the period when the second sample was collected.

Assessing errors in the determination of base excess.

PubMed

Mentel, Alexander; Bach, Friedhelm; Schüler, Joerg; Herrmann, Walter; Koster, Andreas; Crystal, George J; Gatzounis, Georgios; Mertzlufft, Fritz

2002-05-01

We compared estimates for base excess of extracellular fluid (BE(ecf); mmol/L) obtained in five clinically used blood gas analyzers: AVL Compact 2 (Roche Diagnostics, Mannheim, Germany), Ciba-Corning 860 (Bayer Diagnostics, Fernwald, Germany), IL 1620 (Instrumentation Laboratories, Lexington, MA), Stat Profile Ultra (Nova Biomedical, Waltham, MA), and ABL 510 (Radiometer, Copenhagen, Denmark). A total of 134 measurements per analyzer were obtained in arterial and venous blood samples from 10 patients undergoing cardiac surgery and 65 measurements per analyzer in venous blood samples from 2 healthy volunteers. The blood samples were equilibrated in a tonometer with gases of known composition (37 degrees C). Additional theoretical studies were performed to evaluate the relationship between pH and calculated BE(ecf) value (with varied PCO(2)) using the formulas of the various analyzers. The standard deviations of repeated measurements were 0.24 mmol/L for ABL 510 and approximately 0.45 mmol/L for the other 4 analyzers. The maximal systematic difference between the average of all measurements of each analyzer was 3.7 mmol/L; this was primarily attributable to differences in measuring pH, and, to a lesser extent, to differences in calculation and determination of PCO(2). Comparison of the results from samples with different oxygen saturation showed that the relative alkalinity of deoxygenated hemoglobin (Haldane effect) can also influence the determinations of BE(ecf). A clinically useful way to quantify nonrespiratory disturbances of the acid-base balance is calculation of the base excess of extracellular fluid by using blood gas analyzers. In this study, we found significant variability in estimates of base excess of extracellular fluid obtained with five analyzers from different manufacturers. This variability is attributable to multiple factors, including lack of correction for deoxygenated hemoglobin (Haldane effect).

Radionuclides, stable isotopes, inorganic constituents, and organic compounds in water from selected wells and springs from the southern boundary of the Idaho National Engineering Laboratory to the Hagerman area, Idaho, 1993

USGS Publications Warehouse

Bartholomay, Roy C.; Edwards, Daniel D.; Campbell, Linford J.

1994-01-01

The U.S. Geological Survey and the Idaho Department of Water Resources, in response to a request from the U.S. Department of Energy, sampled 19 sites as part of a long-term project to monitor water quality of the Snake River Plain aquifer from the southern boundary of the Idaho National Engineering Laboratory to the Hagerman area. Water samples were collected and analyzed for selected radionuclides, stable isotopes, inorganic constituents, and organic compounds. The samples were collected from seven irrigation wells, four domestic wells, two springs, one stock well, three dairy wells, one observation well, and one commercial well. Two quality assurance samples also were collected and analyzed. None of the radionuclides, inorganic constituents, or organic compounds exceeded the established maximum contaminant levels for drinking water. Most of the radionuclide and inorganic constituent concen- trations exceeded their respective laboratory reporting levels. All samples analyzed for surfactants and dissolved organic carbon had concentrations that exceeded their reporting level. Ethylbenzene concentrations exceeded the reporting level in one water sample.

[Effect sizes, statistical power and sample sizes in "the Japanese Journal of Psychology"].

PubMed

Suzukawa, Yumi; Toyoda, Hideki

2012-04-01

This study analyzed the statistical power of research studies published in the "Japanese Journal of Psychology" in 2008 and 2009. Sample effect sizes and sample statistical powers were calculated for each statistical test and analyzed with respect to the analytical methods and the fields of the studies. The results show that in the fields like perception, cognition or learning, the effect sizes were relatively large, although the sample sizes were small. At the same time, because of the small sample sizes, some meaningful effects could not be detected. In the other fields, because of the large sample sizes, meaningless effects could be detected. This implies that researchers who could not get large enough effect sizes would use larger samples to obtain significant results.

7 CFR 94.101 - Definitions.

Code of Federal Regulations, 2011 CFR

2011-01-01

.... Surveillance sample. This is a 100 gram sample for Salmonella analysis that is drawn by the USDA egg product... analyze for Salmonella in egg products. Unofficial sample. These samples of egg products are drawn by...

Direct Liquid Sampling for Corona Discharge Ion Mobility Spectrometry.

PubMed

Sabo, Martin; Malásková, Michaela; Harmathová, Olga; Hradski, Jasna; Masár, Marián; Radjenovic, Branislav; Matejčík, Štefan

2015-07-21

We present a new technique suitable for direct liquid sampling and analysis by ion mobility spectrometry (IMS). The technique is based on introduction of a droplet stream to the IMS reaction region. The technique was successfully used to detect explosives dissolved in methanol and oil as well as to analyze amino acids and dipeptides. One of the main advantages of this technique is its ability to analyze liquid samples without the requirement of any special solution.

TANKS 18 AND 19-F EQUIPMENT GROUT FILL MATERIAL EVALUATION AND RECOMMENDATIONS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stefanko, D.; Langton, C.

The United States Department of Energy (US DOE) intends to remove Tanks 18-F and 19-F at the Savannah River Site (SRS) from service. The high-level waste (HLW) tanks have been isolated from the F-area Tank Farm (FTF) facilities and will be filled with cementitious grout for the purpose of: (1) physically stabilizing the empty volumes in the tanks, (2) limiting/eliminating vertical pathways from the surface to residual waste on the bottom of the tanks, (3) providing an intruder barrier, and (4) providing an alkaline, chemical reducing environment within the closure boundary to limit solubility of residual radionuclides. Bulk waste andmore » heel waste removal equipment will remain in Tanks 18-F and 19-F when the tanks are closed. This equipment includes: mixer pumps, transfer pumps, transfer jets, equipment support masts, sampling masts and dip tube assemblies. The current Tank 18-F and 19-F closure strategy is to grout the internal void spaces in this equipment to eliminate fast vertical pathways and slow water infiltration to the residual material on the tank floor. This report documents the results of laboratory testing performed to identify a grout formulation for filling the abandoned equipment in Tanks 18-F and 19-F. The objective of this work was to formulate a flowable grout for filling internal voids of equipment that will remain in Tanks 18-F and 19-F during the final closures. This work was requested by V. A. Chander, Tank Farm Closure Engineering, in HLW-TTR-2011-008. The scope for this task is provided in the Task Technical and Quality Assurance Plan (TTQAP), SRNL-RP-2011-00587. The specific objectives of this task were to: (1) Prepare and evaluate the SRR cooling coil grout identified in WSRC-STI-2008-00298 per the TTR for this work. The cooling coil grout is a mixture of BASF MasterFlow{reg_sign} 816 cable grout (67.67 wt. %), Grade 100 ground granulated blast furnace slag (7.52 wt. %) and water (24.81 wt. %); (2) Identify equipment grout placement and performance properties; (3) Design up to 2 additional grout systems for filling the Tank 18-F and Tank 19-F equipment; (4) Prepare samples of candidate grouts and measure fresh properties, thermal properties and cured properties; (5) Recommend a grout for the Tier 1A equipment fill mock up - ADMP 4 foot high mock up, 1 inch and 2 inch pipes; (6) Support procurement of materials for the Tier 1A equipment fill mock up test; (7) Prepare samples of the recommended grout for hydraulic property measurements which can be used for comparison to values used in the F- Tank Farm Performance Assessment (PA); and (8) Document equipment fill grout data and recommendations in a report.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wolfe, M.; Norman, D.

Birds and mammals exposed to waterborne mercury (Hg) and methylmercury (MeHg) were collected and/or sampled at Clear Lake, California, USA, to field test the predictive wildlife criteria model developed for the Great Lakes Water Quality Initiative (GLWQI). Tissue samples collected from sampled animals were analyzed for Hg and organochlorine residues, and for selected physiologic parameters known to be affected by Hg. All mammalian organ tissues analyzed contained less than 12 ppm total Hg, wet weight. All avian tissue samples analyzed contained less than 3 ppm total Hg, wet weight. No evidence of Hg-associated health effects was found. Tissue Hg residuesmore » were compared with water, sediment, and animal food samples to characterize bioaccumulation of mercury in the Clear Lake food web. Total Hg bioaccumulation factors for the Clear Lake site closest to the Hg source were: TL-2: 11,100; TL-3: 31,200; TL-4, 190,000. The results support the final wildlife criterion and suggest that the GLWQI model, with site-specific modifications, is predictive for other Hg-bearing aquatic systems.« less

Mercury Pollution Exploration in Latvia with High-Sensitivity Zeeman Atomic Absorption Spectrometry

NASA Astrophysics Data System (ADS)

Bogans, Egils; Gavare, Zanda; Svagere, Anda; Poikane, Rita; Skudra, Jānis

2011-01-01

This research presents Hg pollution measurements performed in Latvia with sensitive method using Zeeman AAS analyzer RA-915+ and necessary attachments. Air in Riga city and water samples from a number of rivers and lakes of Latvia were analyzed for presence of low-level Hg concentrations. Ombrotrophic bog peat was analyzed to get insight into long-term trends. Environment in the sites sampled is relatively clean according to the results obtained, but there are local spots of pollution.

Capabilities of Direct Sample Introduction - Comprehensive Two-Dimensional Gas Chromatgraphy-Time-of-Flight Mass Spectrometry to Analyze Organic Chemicals of Interest in Fish Oils

USDA-ARS?s Scientific Manuscript database

Most analytical methods for persistent organic pollutants (POPs) focus on targeted analytes. Therefore, analysis of multiple classes of POPs typically entails several sample preparations, fractionations, and injections, whereas other chemicals of possible interest are neglected. To analyze a wider...

1300930

NASA Image and Video Library

2013-08-15

DR. BINAYAK PANDA LOADS A SAMPLE IN THE IMS-6F SECONDARY ION MASS SPECTROSCOPE’S ULTRA HIGH VACUUM CHAMBER. IT IS CAPABLE OF ANALYZING VERY LIGHT ELEMENTS SUCH AS HYDROGEN AND LITHIUM IN ALLOYS. IT CAN ALSO ANALYZE VERY SMALL QUANTITIES OF IMPURITIES IN MATERIALS AT PARTS PER MILLION LEVELS, AND DETERMINE ISOTOPE RATIOS OF ELEMENTS, ALL IN SOLID SAMPLES.

Generating Multiple Imputations for Matrix Sampling Data Analyzed with Item Response Models.

ERIC Educational Resources Information Center

Thomas, Neal; Gan, Nianci

1997-01-01

Describes and assesses missing data methods currently used to analyze data from matrix sampling designs implemented by the National Assessment of Educational Progress. Several improved methods are developed, and these models are evaluated using an EM algorithm to obtain maximum likelihood estimates followed by multiple imputation of complete data…

Method for genetic identification of unknown organisms

DOEpatents

Colston, Jr., Billy W.; Fitch, Joseph P.; Hindson, Benjamin J.; Carter, Chance J.; Beer, Neil Reginald

2016-08-23

A method of rapid, genome and proteome based identification of unknown pathogenic or non-pathogenic organisms in a complex sample. The entire sample is analyzed by creating millions of emulsion encapsulated microdroplets, each containing a single pathogenic or non-pathogenic organism sized particle and appropriate reagents for amplification. Following amplification, the amplified product is analyzed.

Apparatus for measuring resistance change only in a cell analyzer and method for calibrating it

DOEpatents

Hoffman, Robert A.

1980-01-01

The disclosure relates to resistance only monitoring and calibration in an electrical cell analyzer. Sample and sheath fluid flows of different salinities are utilized, the sample flow being diameter modulated to produce a selected pattern which is compared to the resistance measured across the flows.

He, Ne and Ar systematics in single vesicles: Mantle isotopic ratios and origin of the air component in basaltic glasses

NASA Astrophysics Data System (ADS)

Raquin, Aude; Moreira, Manuel Alexis; Guillon, Fabien

2008-09-01

An outstanding problem in understanding the origin of the gaseous phase, particularly the rare gas compositions in magmatic rocks, is the ubiquitous atmospheric component in bulk rock samples, and whether this atmospheric component is a late stage contamination of the sample, or a recycled component though sediments or altered oceanic crust. In the present study we address this problem by analyzing single vesicles from the "popping rock 2∏D43" sample from the Mid-Atlantic Ridge using a UV laser ablation system. We have determined both elemental and isotopic compositions of He, Ne and Ar in single vesicles as well as Kr and Xe abundances. All vesicles analyzed have an isotopic composition identical to the referred degassed mantle value estimated from this same sample, despite analyzing vesicles from a wide size distribution. The atmospheric component, which is always detected in bulk samples by crushing or heating, was not detected in the single vesicles. This implies that the recycling of atmospheric noble gases in the mantle cannot explain the air-like component of this sample. The addition of the atmospheric component must occur either during the eruption, or after sample recovery.

Concentration comparison of selected constituents between groundwater samples collected within the Missouri River alluvial aquifer using purge and pump and grab-sampling methods, near the city of Independence, Missouri, 2013

USGS Publications Warehouse

Krempa, Heather M.

2015-10-29

Relative percent differences between methods were greater than 10 percent for most analyzed trace elements. Barium, cobalt, manganese, and boron had concentrations that were significantly different between sampling methods. Barium, molybdenum, boron, and uranium method concentrations indicate a close association between pump and grab samples based on bivariate plots and simple linear regressions. Grab sample concentrations were generally larger than pump concentrations for these elements and may be because of using a larger pore sized filter for grab samples. Analysis of zinc blank samples suggests zinc contamination in filtered grab samples. Variations of analyzed trace elements between pump and grab samples could reduce the ability to monitor temporal changes and potential groundwater contamination threats. The degree of precision necessary for monitoring potential groundwater threats and application objectives need to be considered when determining acceptable variation amounts.

Improved DESI-MS Performance using Edge Sampling and aRotational Sample Stage

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kertesz, Vilmos; Van Berkel, Gary J

2008-01-01

The position of the surface to be analyzed relative to the sampling orifice or capillary into the mass spectrometer has been known to dramatically affect the observed signal levels in desorption electrospray ionization mass spectrometry (DESIMS). In analyses of sample spots on planar surfaces, DESI-MS signal intensities as much as five times greater were routinely observed when the bottom of the sampling capillary was appropriately positioned beneath the surface plane ( edge sampling") compared to when the capillary just touched the surface. To take advantage of the optimum "edge sampling" geometry and to maximize the number of samples that couldmore » be analyzed in this configuration, a rotational sample stage was integrated into a typical DESI-MS setup. The rapid quantitative determination of caffeine in two diet sport drinks (Diet Turbo Tea, Speed Stack Grape) spiked with an isotopically labeled internal standard demonstrated the utility of this approach.« less

Method and apparatus for automated processing and aliquoting of whole blood samples for analysis in a centrifugal fast analyzer

DOEpatents

Burtis, C.A.; Johnson, W.F.; Walker, W.A.

1985-08-05

A rotor and disc assembly for use in a centrifugal fast analyzer. The assembly is designed to process multiple samples of whole blood followed by aliquoting of the resultant serum into precisely measured samples for subsequent chemical analysis. The assembly requires minimal operator involvement with no mechanical pipetting. The system comprises: (1) a whole blood sample disc; (2) a serum sample disc; (3) a sample preparation rotor; and (4) an analytical rotor. The blood sample disc and serum sample disc are designed with a plurality of precision bore capillary tubes arranged in a spoked array. Samples of blood are loaded into the blood sample disc by capillary action and centrifugally discharged into cavities of the sample preparation rotor where separation of serum and solids is accomplished. The serum is loaded into the capillaries of the serum sample disc by capillary action and subsequently centrifugally expelled into cuvettes of the analyticaly rotor for conventional methods. 5 figs.

Method and apparatus for automated processing and aliquoting of whole blood samples for analysis in a centrifugal fast analyzer

DOEpatents

Burtis, Carl A.; Johnson, Wayne F.; Walker, William A.

1988-01-01

A rotor and disc assembly for use in a centrifugal fast analyzer. The assembly is designed to process multiple samples of whole blood followed by aliquoting of the resultant serum into precisely measured samples for subsequent chemical analysis. The assembly requires minimal operator involvement with no mechanical pipetting. The system comprises (1) a whole blood sample disc, (2) a serum sample disc, (3) a sample preparation rotor, and (4) an analytical rotor. The blood sample disc and serum sample disc are designed with a plurality of precision bore capillary tubes arranged in a spoked array. Samples of blood are loaded into the blood sample disc in capillary tubes filled by capillary action and centrifugally discharged into cavities of the sample preparation rotor where separation of serum and solids is accomplished. The serum is loaded into the capillaries of the serum sample disc by capillary action and subsequently centrifugally expelled into cuvettes of the analytical rotor for analysis by conventional methods.

Laser-induced fluorescence fiber optic probe measurement of oil dilution by fuel

DOEpatents

Parks, II, James E [Knoxville, TN; Partridge, Jr., William P [Oak Ridge, TN

2010-11-23

Apparatus for detecting fuel in oil includes an excitation light source in optical communication with an oil sample for exposing the oil sample to excitation light in order to excite the oil sample from a non-excited state to an excited state and a spectrally selective device in optical communication with the oil sample for detecting light emitted from the oil sample as the oil sample returns from the excited state to a non-excited state to produce spectral indicia that can be analyzed to determine the presence of fuel in the oil sample. A method of detecting fuel in oil includes the steps of exposing a oil sample to excitation light in order to excite the oil sample from a non-excited state to an excited state, as the oil sample returns from the excited state to a non-excited state, detecting light emitted from the oil sample to produce spectral indicia; and analyzing the spectral indicia to determine the presence of fuel in the oil sample.

43 CFR 3430.4-4 - Environmental costs.

Code of Federal Regulations, 2014 CFR

2014-10-01

... and analyzing baseline data on surface water quality and quantity (collecting and analyzing samples...). (2) Groundwater—costs of collecting and analyzing baseline data on groundwater quality and quantity... analyzing baseline air quality data (purchasing rain, air direction, and wind guages and air samplers and...

43 CFR 3430.4-4 - Environmental costs.

Code of Federal Regulations, 2013 CFR

2013-10-01

... and analyzing baseline data on surface water quality and quantity (collecting and analyzing samples...). (2) Groundwater—costs of collecting and analyzing baseline data on groundwater quality and quantity... analyzing baseline air quality data (purchasing rain, air direction, and wind guages and air samplers and...

43 CFR 3430.4-4 - Environmental costs.

Code of Federal Regulations, 2011 CFR

2011-10-01

... and analyzing baseline data on surface water quality and quantity (collecting and analyzing samples...). (2) Groundwater—costs of collecting and analyzing baseline data on groundwater quality and quantity... analyzing baseline air quality data (purchasing rain, air direction, and wind guages and air samplers and...

43 CFR 3430.4-4 - Environmental costs.

Code of Federal Regulations, 2012 CFR

2012-10-01

... and analyzing baseline data on surface water quality and quantity (collecting and analyzing samples...). (2) Groundwater—costs of collecting and analyzing baseline data on groundwater quality and quantity... analyzing baseline air quality data (purchasing rain, air direction, and wind guages and air samplers and...

Method for measuring lead concentrations in blood

DOEpatents

Nogar, Nicholas S.

2001-01-01

Method for measuring lead concentrations in blood. The present invention includes the use of resonant laser ablation to analyze .ltoreq.1 .mu.L (or equivalent mass) samples of blood for lead content. A typical finger prick, for example, yields about 10 .mu.L. Solid samples may also readily be analyzed by resonant laser ablation. The sample is placed on a lead-free, electrically conducting substrate and irradiated with a single, focused laser beam which simultaneously vaporizes, atomizes, and resonantly ionizes an analyte of interest in a sample. The ions are then sorted, collected and detected using a mass spectrometer.