Brooks, Myron H.; Schroder, LeRoy J.; Willoughby, Timothy C.
1987-01-01
Four laboratories involved in the routine analysis of wet-deposition samples participated in an interlaboratory comparison program managed by the U.S. Geological Survey. The four participants were: Illinois State Water Survey central analytical laboratory in Champaign, Illinois; U.S. Geological Survey national water-quality laboratories in Atlanta, Georgia, and Denver, Colorado; and Inland Waters Directorate national water-quality laboratory in Burlington, Ontario, Canada. Analyses of interlaboratory samples performed by the four laboratories from October 1983 through December 1984 were compared.Participating laboratories analyzed three types of interlaboratory samples--natural wet deposition, simulated wet deposition, and deionized water--for pH and specific conductance, and for dissolved calcium, magnesium, sodium, sodium, potassium, chloride, sulfate, nitrate, ammonium, and orthophosphate. Natural wet-deposition samples were aliquots of actual wet-deposition samples. Analyses of these samples by the four laboratories were compared using analysis of variance. Test results indicated that pH, calcium, nitrate, and ammonium results were not directly comparable among the four laboratories. Statistically significant differences between laboratory results probably only were meaningful for analyses of dissolved calcium. Simulated wet-deposition samples with known analyte concentrations were used to test each laboratory for analyte bias. Laboratory analyses of calcium, magnesium, sodium, potassium, chloride, sulfate, and nitrate were not significantly different from the known concentrations of these analytes when tested using analysis of variance. Deionized-water samples were used to test each laboratory for reporting of false positive values. The Illinois State Water Survey Laboratory reported the smallest percentage of false positive values for most analytes. Analyte precision was estimated for each laboratory from results of replicate measurements. In general, the Illinois State Water Survey laboratory achieved the greatest precision, whereas the U.S. Geological Survey laboratories achieved the least precision.
Katz, Brian G.; Krulikas, Richard K.
1979-01-01
Water samples from wells in Nassau and Suffolk Counties were analyzed for chloride and nitrate. Two samples were collected at each well; one was analyzed by the U.S. Geological Survey, the other by a laboratory in the county from which the sample was taken. Results were compared statistically by paired-sample t-test to indicate the degree of uniformity among laboratory results. Chloride analyses from one of the three county laboratories differed significantly (0.95 confidence level) from that of a Geological Survey laboratory. For nitrate analyses, a significant difference (0.95 confidence level) was noted between results from two of the three county laboratories and the Geological Survey laboratory. The lack of uniformity among results reported by the participating laboratories indicates a need for continuing participation in a quality-assurance program and exercise of strong quality control from time of sample collection through analysis so that differences can be evaluated. (Kosco-USGS)
Coplen, T.B.; Qi, H.
2009-01-01
New isotope laboratories can achieve the goal of reporting the same isotopic composition within analytical uncertainty for the same material analysed decades apart by (1) writing their own acceptance testing procedures and putting them into their mass spectrometric or laser-based isotope-ratio equipment procurement contract, (2) requiring a manufacturer to demonstrate acceptable performance using all sample ports provided with the instrumentation, (3) for each medium to be analysed, prepare two local reference materials substantially different in isotopic composition to encompass the range in isotopic composition expected in the laboratory and calibrated them with isotopic reference materials available from the International Atomic Energy Agency (IAEA) or the US National Institute of Standards and Technology (NIST), (4) using the optimum storage containers (for water samples, sealing in glass ampoules that are sterilised after sealing is satisfactory), (5) interspersing among sample unknowns local laboratory isotopic reference materials daily (internationally distributed isotopic reference materials can be ordered at three-year intervals, and can be used for elemental analyser analyses and other analyses that consume less than 1 mg of material) - this process applies to H, C, N, O, and S isotope ratios, (6) calculating isotopic compositions of unknowns by normalising isotopic data to that of local reference materials, which have been calibrated to internationally distributed isotopic reference materials, (7) reporting results on scales normalised to internationally distributed isotopic reference materials (where they are available) and providing to sample submitters the isotopic compositions of internationally distributed isotopic reference materials of the same substance had they been analysed with unknowns, (8) providing an audit trail in the laboratory for analytical results - this trail commonly will be in electronic format and might include a laboratory information management system, (9) making at regular intervals a complete backup of laboratory analytical data (both of samples logged into the laboratory and of mass spectrometric analyses), being sure to store one copy of this backup offsite, and (10) participating in interlaboratory comparison exercises sponsored by the IAEA and other agencies at regular intervals. ?? Taylor & Francis.
Screening of ground water samples for volatile organic compounds using a portable gas chromatograph
Buchmiller, R.C.
1989-01-01
A portable gas chromatograph was used to screen 32 ground water samples for volatile organic compounds. Seven screened samples were positive; four of the seven samples had volatile organic substances identified by second-column confirmation. Four of the seven positive, screened samples also tested positive in laboratory analyses of duplicate samples. No volatile organic compounds were detected in laboratory analyses of samples that headspace screening indicated to be negative. Samples that contained volatile organic compounds, as identified by laboratory analysis, and that contained a volatile organic compound present in a standard of selected compounds were correctly identified by using the portable gas chromatography. Comparisons of screened-sample data with laboratory data indicate the ability to detect selected volatile organic compounds at concentrations of about 1 microgram per liter in the headspace of water samples by use of a portable gas chromatography. -Author
Tank 30 and 37 Supernatant Sample Cross-Check and Evaporator Feed Qualification Analysis-2012
DOE Office of Scientific and Technical Information (OSTI.GOV)
Oji, L. N.
2013-03-07
This report summarizes the analytical data reported by the F/H and Savannah River National Laboratories for the 2012 cross-check analysis for high level waste supernatant liquid samples from SRS Tanks 30 and 37. The intent of this Tank 30 and 37 sample analyses was to perform cross-checks against routine F/H Laboratory analyses (corrosion and evaporator feed qualification programs) using samples collected at the same time from both tanks as well as split samples from the tanks.
McHale, Michael R.; McChesney, Dennis
2007-01-01
In 2003, a study was conducted to evaluate the accuracy and precision of 10 laboratories that analyze water-quality samples for phosphorus concentrations in the Catskill Mountain region of New York State. Many environmental studies in this region rely on data from these different laboratories for water-quality analyses, and the data may be used in watershed modeling and management decisions. Therefore, it is important to determine whether the data reported by these laboratories are of comparable accuracy and precision. Each laboratory was sent 12 samples for triplicate analysis for total phosphorus, total dissolved phosphorus, and soluble reactive phosphorus. Eight of these laboratories reported results that met comparability criteria for all samples; the remaining two laboratories met comparability criteria for only about half of the analyses. Neither the analytical method used nor the sample concentration ranges appeared to affect the comparability of results. The laboratories whose results were comparable gave consistently comparable results throughout the concentration range analyzed, and the differences among methods did not diminish comparability. All laboratories had high data precision as indicated by sample triplicate results. In addition, the laboratories consistently reported total phosphorus values greater than total dissolved phosphorus values, and total dissolved phosphorus values greater than soluble reactive phosphorus values, as would be expected. The results of this study emphasize the importance of regular laboratory participation in sample-exchange programs.
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
Hydrogen Safety Project: Chemical analysis support task. Window ``E`` analyses
DOE Office of Scientific and Technical Information (OSTI.GOV)
Jones, T E; Campbell, J A; Hoppe, E W
1992-09-01
Core samples taken from tank 101-SY at Hanford during ``window E`` were analyzed for organic and radiochemical constituents by staff of the Analytical Chemistry Laboratory at Pacific Northwest Laboratory. Westinghouse Hanford company submitted these samples to the laboratory.
Galea, Karen S; Searl, Alison; Sánchez-Jiménez, Araceli; Woldbæk, Torill; Halgard, Kristin; Thorud, Syvert; Steinsvåg, Kjersti; Krüger, Kirsti; Maccalman, Laura; Cherrie, John W; van Tongeren, Martie
2012-01-01
There are no recognized analytical methods for measuring oil mist and vapours arising from drilling fluids used in offshore petroleum drilling industry. To inform the future development of improved methods of analysis for oil mist and vapours this study assessed the inter- and intra-laboratory variability in oil mist and vapour analysis. In addition, sample losses during transportation and storage were assessed. Replicate samples for oil mist and vapour were collected using the 37-mm Millipore closed cassette and charcoal tube assembly. Sampling was conducted in a simulated shale shaker room, similar to that found offshore for processing drilling fluids. Samples were analysed at two different laboratories, one in Norway and one in the UK. Oil mist samples were analysed using Fourier transform infrared spectroscopy (FTIR), while oil vapour samples were analysed by gas chromatography (GC). The comparison of replicate samples showed substantial within- and between-laboratory variability in reported oil mist concentrations. The variability in oil vapour results was considerably reduced compared to oil mist, provided that a common method of calibration and quantification was adopted. The study also showed that losses can occur during transportation and storage of samples. There is a need to develop a harmonized method for the quantification of oil mist on filter and oil vapour on charcoal supported by a suitable proficiency testing scheme for laboratories involved in the analysis of occupational hygiene samples for the petroleum industry. The uncertainties in oil mist and vapour measurement have substantial implications in relation to compliance with occupational exposure limits and also in the reliability of any exposure-response information reported in epidemiological studies.
Field and laboratory analyses of water from the Columbia aquifer in Eastern Maryland
Bachman, L.J.
1984-01-01
Field and laboratory analyses of pH, alkalinity, and specific conductance from water samples collected from the Columbia aquifer on the Delmarva Peninsula in eastern Maryland were compared to determine if laboratory analyses could be used for making regional water-quality interpretations. Kruskal-Wallis tests of field and laboratory data indicate that the difference between field and laboratory values is usually not enough to affect the outcome of the statistical tests. Thus, laboratory measurements of these constituents may be adequate for making certain regional water-quality interpretations, although they may result in errors if used for geochemical interpretations.
Tilling, Robert I.; Bornhorst, Theodore J.; Taggart, Joseph E.; Rose, William I.; McGee, James J.
1987-01-01
An inter-laboratory comparison has been made of X-ray fluorescence analyses of 10 samples of lava and pumices from El Chichón Volcano, Chiapas, Mexico. Some determinations of major-element constituents agree within analytical uncertainty, whereas others exchibit significant bias. Analyses carried out at the Michigan Technological University (MTU) laboratory are systematically lower in MgO (26–48%), Fetotal(5–18%), CaO (4–15%) and higher in K2O (0–15%) than analyses made at the U.S. Geological Survey (USGS) Denver laboratory. These differences are ascribed in part to a complex combination of calibration assumptionsand mineralogical and particle-size effects inherent in the use of pressed rock-powder pellets in the analytical procedure of the MTU laboratory. Other, but as yet unknown, differences in sample preparation and/or analytical technique may also be important; effects related to natural sample inhomogeneityare believed to be insignificant. The inter-laboratory differences in the analytical data complicated accurate assessment of whether El Chichón magmas have changed composition during the past 300 000 a. Knowledge of such change is needed for understanding petrogenetic history and for such related studies as evaluation of volcanic hazards.
7 CFR 94.3 - Analyses performed and locations of laboratories.
Code of Federal Regulations, 2011 CFR
2011-01-01
... applicable plant on the official certificate. (b) Mandatory egg product samples for Salmonella are required... recognized laboratories for analyzing routine egg product samples for Salmonella. (c) Mandatory egg product...
DOE Office of Scientific and Technical Information (OSTI.GOV)
Miller, G.L.
This data package satisfies the requirement for a format IV, final report. It is a follow-up to the 45-day safety screen report for tank AP-104. Evaporator candidate feed from tank 241-AP-104 (hereafter referred to as AP-104) was characterized for physical, inorganic, organic and radiochemical parameters by the Westinghouse Hanford Company, 222-S Laboratory, and by the Battelle Pacific Northwest National Laboratory (PNNL), Analytical Chemistry Laboratory (ACL) as directed by the Tank Sample and Analysis Plan (TSAP), References 1 through 4. Preliminary data in the form of summary analytical tables were provided to the project in advance of this final report tomore » enable early estimation of evaporator operational parameters, using the Predict modeling program. Laboratory analyses at ACL Laboratory was performed according to the TSAP. Analyses were performed at the 222-S Laboratory as defined and specified in the TSAP and the Laboratory`s Quality Assurance Plan, References 5 and 6. Any deviations from the instructions documented in the TSAP are discussed in this narrative and are supported with additional documentation. SAMPLING The TSAP, section 2, provided sampling information for waste samples collected from tank AP-104. The bottle-on-a-string method was used to collect liquid grab samples from the tank. Each glass sample bottle was amber, precleaned, and contained approximately 100 milliliters. Each bottle was closed with a teflon seal cap (or teflon septum for volatile organic analysis samples). Field blank samples were prepared by placing deionized water into sampling bottles, lowering the unclosed bottles into the riser for a period of time, retrieving them from the riser, and then closing the bottles with the same types of caps used for the tank samples. None of the samples were preserved by acidification. Upon receipt, the sample bottles destined for organic analyses were placed in a refrigerator. No attempt was made during sampling to assure the complete filling of the bottles so as to exclude all headspace. These actions were consistent with safety procedures, which attempt to limit personnel exposure to hazardous ionizing radiation.« less
Interpretation of standard leaching test BS EN 12457-2: is your sample hazardous or inert?
Zandi, Mohammad; Russell, Nigel V; Edyvean, Robert G J; Hand, Russell J; Ward, Philip
2007-12-01
A slag sample from a lead refiner has been obtained and given to two analytical laboratories to determine the release of trace elements from the sample according to BS EN 12457-2. Samples analysed by one laboratory passed waste acceptance criteria, leading it to be classified as an inert material; samples of the same material analysed by the other laboratory failed waste acceptance criteria and were classified as hazardous. It was found that the sample preparation procedure is the critical step in the leaching analysis and that the effects of particle size on leachability should be taken into account when using this standard. The purpose of this paper is to open a debate on designing a better defined standard leaching test and making current waste acceptance criteria more flexible.
10 CFR 74.45 - Measurements and measurement control.
Code of Federal Regulations, 2013 CFR
2013-01-01
... measurements, obtaining samples, and performing laboratory analyses for element concentration and isotope... of random error behavior. On a predetermined schedule, the program shall include, as appropriate: (i) Replicate analyses of individual samples; (ii) Analysis of replicate process samples; (iii) Replicate volume...
10 CFR 74.45 - Measurements and measurement control.
Code of Federal Regulations, 2014 CFR
2014-01-01
... measurements, obtaining samples, and performing laboratory analyses for element concentration and isotope... of random error behavior. On a predetermined schedule, the program shall include, as appropriate: (i) Replicate analyses of individual samples; (ii) Analysis of replicate process samples; (iii) Replicate volume...
10 CFR 74.45 - Measurements and measurement control.
Code of Federal Regulations, 2012 CFR
2012-01-01
... measurements, obtaining samples, and performing laboratory analyses for element concentration and isotope... of random error behavior. On a predetermined schedule, the program shall include, as appropriate: (i) Replicate analyses of individual samples; (ii) Analysis of replicate process samples; (iii) Replicate volume...
78 FR 59621 - Extension of the Current Fees for the Accredited Laboratory Program
Federal Register 2010, 2011, 2012, 2013, 2014
2013-09-27
... regulatory samples of raw or processed meat and poultry products, and through which a check sample program... Laboratory Program. Such accreditation allows laboratories to conduct analyses of official meat and poultry... employer. List of Subjects in 9 CFR Part 391 Fees and charges, Government employees, Meat inspection...
NASA Technical Reports Server (NTRS)
McAdam, A. C.; Mahaffy, P. R.; Blake, D. F.; Ming, D. W.; Franz, H. B.; Eigenbrode, J. L.; Steele, A.
2010-01-01
The 2009 Arctic Mars Analog Svalbard Expedition (AMASE) investigated several geologic settings using methodologies and techniques being developed or considered for future Mars missions, such as the Mars Science Laboratory (MSL), ExoMars, and Mars Sample Return (MSR). AMASE-related research comprises both analyses conducted during the expedition and further analyses of collected samples using laboratory facilities at a variety of institutions. The Sample Analysis at Mars (SAM) instrument suite, which will be part of the Analytical Laboratory on MSL, consists of a quadrupole mass spectrometer (QMS), a gas chromatograph (GC), and a tunable laser spectrometer (TLS). An Evolved Gas Analysis Mass Spectrometer (EGA-MS) was used during AMASE to represent part of the capabilities of SAM. The other instrument included in the MSL Analytical Laboratory is CheMin, which uses X-Ray Diffraction (XRD) and X-Ray Fluorescence (XRF) to perform quantitative mineralogical characterization of samples. Field-portable versions of CheMin were used during the AMASE 2009. Here, we discuss the preliminary interpretation of EGA and XRD analyses of selected AMASE carbonate samples and implications for mineralogical interpretations from MSL. Though CheMin will be the primary mineralogical tool on MSL, SAM EGA could be used to support XRD identifications or indicate the presence of volatile-bearing minerals which may be near or below XRD detection limits. Data collected with instruments in the field and in comparable laboratory setups (e.g., the SAM breadboard) will be discussed.
Contents of microscopic fungi in dusts coming from cereal analysis laboratories.
Szwajkowska-Michalek, Lidia; Stuper, Kinga; Lakomy, Piotr; Matysiak, Anna; Perkowski, Juliusz
2010-01-01
Microscopic fungi - components of bioaerosol found in the workplace environment of individuals employed in the agricultural sector - constitute a considerable hazard for their health. This study includes quantitative and qualitative analyses of mycobionta contained in 20 samples of dusts collected from laboratories conducting analyses of cereals. A total of 27 species of viable microscopic fungi were isolated. The most frequently isolated genera Penicillium and Aspergillus, accounting for 27 percent and 26 percent of analyzed isolates. The content of fungal biomass was determined quantitatively using a fungal marker, ergosterol (ERG). Concentrations of this metabolite for all samples ranged from 0.48 mg/kg-212.36 mg/kg. Based on the analyses, it may be stated that the concentration of microfungi in settled dust from laboratories conducting analyses of cereals was varied, and in several cases markedly exceeded admissible concentration levels.
Intercomparison of CO 2 measurements
NASA Astrophysics Data System (ADS)
Poisson, A.; Culkin, F.; Ridout, P.
1990-10-01
Seawater samples, of four different salinities, were analysed for total alkalinity, total CO 2, pH and pCO 2 by up to 12 laboratories. The results showthat although most laboratories are capable of high precision in these determinations, there is an unacceptably high disagreement between their analyses of the same samples. For global programmes involving studies of the CO 2 system in seawater, it is strongly recommended that standard reference materials be made widely available.
Long, H. Keith; Daddow, Richard L.; Farrar, Jerry W.
1998-01-01
Since 1962, the U.S. Geological Survey (USGS) has operated the Standard Reference Sample Project to evaluate the performance of USGS, cooperator, and contractor analytical laboratories that analyze chemical constituents of environmental samples. The laboratories are evaluated by using performance evaluation samples, called Standard Reference Samples (SRSs). SRSs are submitted to laboratories semi-annually for round-robin laboratory performance comparison purposes. Currently, approximately 100 laboratories are evaluated for their analytical performance on six SRSs for inorganic and nutrient constituents. As part of the SRS Project, a surplus of homogeneous, stable SRSs is maintained for purchase by USGS offices and participating laboratories for use in continuing quality-assurance and quality-control activities. Statistical evaluation of the laboratories results provides information to compare the analytical performance of the laboratories and to determine possible analytical deficiences and problems. SRS results also provide information on the bias and variability of different analytical methods used in the SRS analyses.
NASA Astrophysics Data System (ADS)
Chiari, M.; Yubero, E.; Calzolai, G.; Lucarelli, F.; Crespo, J.; Galindo, N.; Nicolás, J. F.; Giannoni, M.; Nava, S.
2018-02-01
Within the framework of research projects focusing on the sampling and analysis of airborne particulate matter, Particle Induced X-ray Emission (PIXE) and Energy Dispersive X-ray Fluorescence (ED-XRF) techniques are routinely used in many laboratories throughout the world to determine the elemental concentration of the particulate matter samples. In this work an inter-laboratory comparison of the results obtained from analysing several samples (collected on both Teflon and quartz fibre filters) using both techniques is presented. The samples were analysed by PIXE (in Florence, at the 3 MV Tandetron accelerator of INFN-LABEC laboratory) and by XRF (in Elche, using the ARL Quant'X EDXRF spectrometer with specific conditions optimized for specific groups of elements). The results from the two sets of measurements are in good agreement for all the analysed samples, thus validating the use of the ARL Quant'X EDXRF spectrometer and the selected measurement protocol for the analysis of aerosol samples. Moreover, thanks to the comparison of PIXE and XRF results on Teflon and quartz fibre filters, possible self-absorption effects due to the penetration of the aerosol particles inside the quartz fibre-filters were quantified.
7 CFR 94.5 - Charges for laboratory service.
Code of Federal Regulations, 2013 CFR
2013-01-01
..., Inspections, Marketing Practices), DEPARTMENT OF AGRICULTURE (CONTINUED) COMMODITY LABORATORY TESTING PROGRAMS... costs for analysis of mandatory egg product samples at Science and Technology Division laboratories... program. The costs for any other mandatory laboratory analyses and testing of an egg product's identity...
7 CFR 94.5 - Charges for laboratory service.
Code of Federal Regulations, 2011 CFR
2011-01-01
..., Inspections, Marketing Practices), DEPARTMENT OF AGRICULTURE (CONTINUED) COMMODITY LABORATORY TESTING PROGRAMS... costs for analysis of mandatory egg product samples at Science and Technology Division laboratories... program. The costs for any other mandatory laboratory analyses and testing of an egg product's identity...
7 CFR 94.5 - Charges for laboratory service.
Code of Federal Regulations, 2012 CFR
2012-01-01
..., Inspections, Marketing Practices), DEPARTMENT OF AGRICULTURE (CONTINUED) COMMODITY LABORATORY TESTING PROGRAMS... costs for analysis of mandatory egg product samples at Science and Technology Division laboratories... program. The costs for any other mandatory laboratory analyses and testing of an egg product's identity...
7 CFR 94.5 - Charges for laboratory service.
Code of Federal Regulations, 2014 CFR
2014-01-01
..., Inspections, Marketing Practices), DEPARTMENT OF AGRICULTURE (CONTINUED) COMMODITY LABORATORY TESTING PROGRAMS... costs for analysis of mandatory egg product samples at Science and Technology Division laboratories... program. The costs for any other mandatory laboratory analyses and testing of an egg product's identity...
40 CFR 141.24 - Organic chemicals, sampling and analytical requirements.
Code of Federal Regulations, 2014 CFR
2014-07-01
... available from U.S. Environmental Protection Agency, National Exposure Research Laboratory (NERL)-Cincinnati... for which the laboratory desires certification. (B) Achieve the quantitative acceptance limits under... contaminants included in the PE sample. (C) Achieve quantitative results on the analyses performed under...
40 CFR 141.24 - Organic chemicals, sampling and analytical requirements.
Code of Federal Regulations, 2011 CFR
2011-07-01
... available from U.S. Environmental Protection Agency, National Exposure Research Laboratory (NERL)-Cincinnati... for which the laboratory desires certification. (B) Achieve the quantitative acceptance limits under... contaminants included in the PE sample. (C) Achieve quantitative results on the analyses performed under...
40 CFR 141.24 - Organic chemicals, sampling and analytical requirements.
Code of Federal Regulations, 2013 CFR
2013-07-01
... available from U.S. Environmental Protection Agency, National Exposure Research Laboratory (NERL)-Cincinnati... for which the laboratory desires certification. (B) Achieve the quantitative acceptance limits under... contaminants included in the PE sample. (C) Achieve quantitative results on the analyses performed under...
40 CFR 141.24 - Organic chemicals, sampling and analytical requirements.
Code of Federal Regulations, 2012 CFR
2012-07-01
... available from U.S. Environmental Protection Agency, National Exposure Research Laboratory (NERL)-Cincinnati... for which the laboratory desires certification. (B) Achieve the quantitative acceptance limits under... contaminants included in the PE sample. (C) Achieve quantitative results on the analyses performed under...
40 CFR 141.24 - Organic chemicals, sampling and analytical requirements.
Code of Federal Regulations, 2010 CFR
2010-07-01
... available from U.S. Environmental Protection Agency, National Exposure Research Laboratory (NERL)-Cincinnati... for which the laboratory desires certification. (B) Achieve the quantitative acceptance limits under... contaminants included in the PE sample. (C) Achieve quantitative results on the analyses performed under...
SOIL AND FILL LABORATORY SUPPORT - 1992 RADIOLOGICAL ANALYSES - FLORIDA RADON RESEARCH PROGRAM
The report gives results of soil analysis laboratory work by the University of Florida in support of the Florida Radon Research Program (FRRP). Analyses were performed on soil and fill samples collected during 1992 by the FRRP Research House Program and the New House Evaluation P...
Chemical analyses in the World Coal Quality Inventory
Tewalt, Susan J.; Belkin, Harvey E.; SanFilipo, John R.; Merrill, Matthew D.; Palmer, Curtis A.; Warwick, Peter D.; Karlsen, Alexander W.; Finkelman, Robert B.; Park, Andy J.
2010-01-01
The main objective of the World Coal Quality Inventory (WoCQI) was to collect and analyze a global set of samples of mined coal during a time period from about 1995 to 2006 (Finkelman and Lovern, 2001). Coal samples were collected by foreign collaborators and submitted to country specialists in the U.S. Geological Survey (USGS) Energy Program. However, samples from certain countries, such as Afghanistan, India, and Kyrgyzstan, were collected collaboratively in the field with USGS personnel. Samples were subsequently analyzed at two laboratories: the USGS Inorganic Geochemistry Laboratory located in Denver, CO and a commercial laboratory (Geochemical Testing, Inc.) located in Somerset, PA. Thus the dataset, which is in Excel (2003) format and includes 1,580 samples from 57 countries, does not have the inter-laboratory variability that is present in many compilations. Major-, minor-, and trace-element analyses from the USGS laboratory, calculated to a consistent analytical basis (dry, whole-coal) and presented with available sample identification information, are sorted alphabetically by country name. About 70 percent of the samples also have data from the commercial laboratory, which are presented on an as-received analytical basis. The USGS initiated a laboratory review of quality assurance in 2008, covering quality control and methodology used in inorganic chemical analyses of coal, coal power plant ash, water, and sediment samples. This quality control review found that data generated by the USGS Inorganic Geochemistry Laboratory from 1996 through 2006 were characterized by quality practices that did not meet USGS requirements commonly in use at the time. The most serious shortcomings were (1) the adjustment of raw sample data to standards when the instrument values for those standards exceeded acceptable limits or (2) the insufficient use of multiple standards to provide adequate quality assurance. In general, adjustment of raw data to account for instrument 'drift' is an acceptable practice within strictly defined limits. During the denoted period, USGS required that the maximum adjustment of instrument values, guided by calibration standards, was not allowed to exceed 10 percent. However, in some cases, the Inorganic Geochemistry Laboratory released data that were adjusted by more than 10 percent and (or) were not constrained by an adequate number of control standards. Original instrument values no longer exist for about 80 percent of the analyses during this period; therefore, the acceptability of drift corrections for most of the samples analyzed cannot be determined. For these reasons, the WoCQI data from the USGS Inorganic Geochemistry Laboratory should be used with care. For more information, individuals may contact laboratory management at EnergyLabs@usgs.gov with specific questions about particular datasets or analytical attributes. Standard USGS sampling methods were provided and recommended to collaborators, but the analyzed samples may or may not be representative of their locale; for some samples, only limited information is available concerning sample provenance. Single samples cannot represent spatial or temporal variability within a coal area. Geochemical datasets of U.S. coals can be found in the COALQUAL database (Bragg and others, 1997) and the National Coal Quality Inventory (Hatch and others, 2006), as only non-U.S. sample data are presented in the WoCQI. Although the WoCQI does not contain worldwide coverage of coal deposits, it is truly a unique and valuable compilation. The information in the WoCQI should prove useful for identifying possible areas for future global coal research.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Not Available
This purpose of this report is to summarize the activities of the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory (ANL) for Fiscal Year 1990. The ACL has four technical groups -- Chemical Analysis, Instrumental Analysis, Organic Analysis, and Environmental Analysis. The Chemical Analysis Group uses wet-chemical and instrumental methods for elemental, compositional, and isotopic analyses of solid, liquid, and gaseous samples and provides specialized analytical services. The Instrumental Analysis Group uses nuclear counting techniques in radiochemical analyses over a wide range of sample types from low-level environmental samples to samples of high radioactivity. The Organic Analysis Group uses amore » number of complementary techniques to separate and to quantitatively and qualitatively analyze complex organic mixtures and compounds at the trace level, including synthetic fuels, toxic substances, fossil-fuel residues and emissions, pollutants, biologically active compounds, pesticides, and drugs. The Environmental Analysis Group performs analyses of inorganic environmental and hazardous waste and coal samples.« less
NASA Astrophysics Data System (ADS)
McAdam, A.; Knudson, C. A.; Sutter, B.; Andrejkovicova, S. C.; Archer, P. D., Jr.; Franz, H. B.; Eigenbrode, J. L.; Morris, R. V.; Ming, D. W.; Sun, V. Z.; Milliken, R.; Wilhelm, M. B.; Mahaffy, P. R.; Navarro-Gonzalez, R.
2016-12-01
The Chemistry and Mineralogy (CheMin) instrument onboard the Mars Science Laboratory (MSL) rover detected Si-rich amorphous or poorly ordered materials in several samples from Murray Formation mudstones and Stimson Formation sandstones. High-SiO2 amorphous materials such as opal-A or rhyolitic glass are candidate phases, but CheMin data cannot be used to distinguish between these possibilities. In the Buckskin (BS) sample from the upper Murray Formation, and the Big Sky (BY) and Greenhorn (GH) samples from the Stimson Formation, evolved gas analyses by the Sample Analysis at Mars (SAM) instrument showed very broad H2O evolutions during sample heating at temperatures >450-500°C, which had not been observed from previous samples. BS also had a significant broad evolution <450-500°C. We have undertaken a laboratory study targeted at understanding if the data from SAM analyses can be used to place constraints on the nature of the amorphous phases. SAM-like evolved gas analyses have been performed on several opal and rhyolitic glass samples. Opal-A samples exhibited wide <500°C H2O evolutions, with lesser H2O evolved above 500°C. H2O evolution traces from rhyolitic glasses varied, having either two broad H2O peaks, <300°C and >500°C, or a broad peak centered around 400°C. For samples that produced two evolutions, the lower temperature peak was more intense than the higher temperature peak, a trend also exhibited by opal-A. This trend is consistent with data from BS, but does not seem consistent with data from BY and GH which evolved most of their H2O >500°C. It may be that dehydration of opal-A and/or rhyolitic glass can result in some preferential loss of lower temperature H2O, to produce traces that more closely resemble BY and GH. This is currently under investigation and results will be reported.
Tank 241-AY-101 Privatization Push Mode Core Sampling and Analysis Plan
DOE Office of Scientific and Technical Information (OSTI.GOV)
TEMPLETON, A.M.
2000-05-19
This sampling and analysis plan (SAP) identifies characterization objectives pertaining to sample collection, laboratory analytical evaluation, and reporting requirements for samples obtained from tank 241-AY-101. The purpose of this sampling event is to obtain information about the characteristics of the contents of 241-AY-101 required to satisfy ''Data Quality Objectives For RPP Privatization Phase I: Confirm Tank T Is An Appropriate Feed Source For High-Level Waste Feed Batch X(HLW DQO)' (Nguyen 1999a), ''Data Quality Objectives For TWRS Privatization Phase I: Confirm Tank T Is An Appropriate Feed Source For Low-Activity Waste Feed Butch X (LAW DQO) (Nguyen 1999b)'', ''Low Activity Wastemore » and High-Level Waste Feed Data Quality Objectives (L&H DQO)'' (Patello et al. 1999), and ''Characterization Data Needs for Development, Design, and Operation of Retrieval Equipment Developed through the Data Quality Objective Process (Equipment DQO)'' (Bloom 1996). Special instructions regarding support to the LAW and HLW DQOs are provided by Baldwin (1999). Push mode core samples will be obtained from risers 15G and 150 to provide sufficient material for the chemical analyses and tests required to satisfy these data quality objectives. The 222-S Laboratory will extrude core samples; composite the liquids and solids; perform chemical analyses on composite and segment samples; archive half-segment samples; and provide sub-samples to the Process Chemistry Laboratory. The Process Chemistry Laboratory will prepare test plans and perform process tests to evaluate the behavior of the 241-AY-101 waste undergoing the retrieval and treatment scenarios defined in the applicable DQOs. Requirements for analyses of samples originating in the process tests will be documented in the corresponding test plans and are not within the scope of this SAP.« less
NASA Astrophysics Data System (ADS)
Hoffmann, V. H.; Kaliwoda, M.; Hochleitner, R.; Mikouchi, T.; Wimmer, K.
2018-04-01
Very sophisticated, high-end techniques are requested for the investigation of pristine particles from a planetary surface, such as Mars, in situ or in our laboratories, in case of martian meteorites or even returned samples from (future) missions.
Application of selected methods of remote sensing for detecting carbonaceous water pollution
NASA Technical Reports Server (NTRS)
Davis, E. M.; Fosbury, W. J.
1973-01-01
A reach of the Houston Ship Channel was investigated during three separate overflights correlated with ground truth sampling on the Channel. Samples were analyzed for such conventional parameters as biochemical oxygen demand, chemical oxygen demand, total organic carbon, total inorganic carbon, turbidity, chlorophyll, pH, temperature, dissolved oxygen, and light penetration. Infrared analyses conducted on each sample included reflectance ATR analysis, carbon tetrachloride extraction of organics and subsequent scanning, and KBr evaporate analysis of CCl4 extract concentrate. Imagery which was correlated with field and laboratory data developed from ground truth sampling included that obtained from aerial KA62 hardware, RC-8 metric camera systems, and the RS-14 infrared scanner. The images were subjected to analysis by three film density gradient interpretation units. Data were then analyzed for correlations between imagery interpretation as derived from the three instruments and laboratory infrared signatures and other pertinent field and laboratory analyses.
Physical deterioration of preservative treated poles and pilings exposed to salt water
Grant T. Kirker; Jessie Glaeser; Stan T. Lebow; Frederick Green III; Carol A. Clausen
2011-01-01
This report details the results of laboratory analyses of wooden pilings sent to the USDA Forest Products Laboratory in March 2011. These samples were removed from coastal wooden posts, poles, piles, and deck boards. A total of 22 samples, consisting of either core borings or surface fiber samples, were removed from four installations along the South Carolina coast....
Auditing of chromatographic data.
Mabie, J T
1998-01-01
During a data audit, it is important to ensure that there is clear documentation and an audit trail. The Quality Assurance Unit should review all areas, including the laboratory, during the conduct of the sample analyses. The analytical methodology that is developed should be documented prior to sample analyses. This is an important document for the auditor, as it is the instrumental piece used by the laboratory personnel to maintain integrity throughout the process. It is expected that this document will give insight into the sample analysis, run controls, run sequencing, instrument parameters, and acceptance criteria for the samples. The sample analysis and all supporting documentation should be audited in conjunction with this written analytical method and any supporting Standard Operating Procedures to ensure the quality and integrity of the data.
Tank 241-AY-101 Privatization Push Mode Core Sampling and Analysis Plan
DOE Office of Scientific and Technical Information (OSTI.GOV)
TEMPLETON, A.M.
2000-01-12
This sampling and analysis plan (SAP) identifies characterization objectives pertaining to sample collection, laboratory analytical evaluation, and reporting requirements for samples obtained from tank 241-AY-101. The purpose of this sampling event is to obtain information about the characteristics of the contents of 241-AY-101 required to satisfy Data Quality Objectives For RPP Privatization Phase I: Confirm Tank T Is An Appropriate Feed Source For High-Level Waste Feed Batch X(HLW DQO) (Nguyen 1999a), Data Quality Objectives For TWRS Privatization Phase I : Confirm Tank T Is An Appropriate Feed Source For Low-Activity Waste Feed Batch X (LAW DQO) (Nguyen 1999b), Low Activitymore » Waste and High-Level Waste Feed Data Quality Objectives (L and H DQO) (Patello et al. 1999), and Characterization Data Needs for Development, Design, and Operation of Retrieval Equipment Developed through the Data Quality Objective Process (Equipment DQO) (Bloom 1996). Special instructions regarding support to the LAW and HLW DQOs are provided by Baldwin (1999). Push mode core samples will be obtained from risers 15G and 150 to provide sufficient material for the chemical analyses and tests required to satisfy these data quality objectives. The 222-S Laboratory will extrude core samples; composite the liquids and solids; perform chemical analyses on composite and segment samples; archive half-segment samples; and provide subsamples to the Process Chemistry Laboratory. The Process Chemistry Laboratory will prepare test plans and perform process tests to evaluate the behavior of the 241-AY-101 waste undergoing the retrieval and treatment scenarios defined in the applicable DQOs. Requirements for analyses of samples originating in the process tests will be documented in the corresponding test plans and are not within the scope of this SAP.« less
USGS Blind Sample Project: monitoring and evaluating laboratory analytical quality
Ludtke, Amy S.; Woodworth, Mark T.
1997-01-01
The U.S. Geological Survey (USGS) collects and disseminates information about the Nation's water resources. Surface- and ground-water samples are collected and sent to USGS laboratories for chemical analyses. The laboratories identify and quantify the constituents in the water samples. Random and systematic errors occur during sample handling, chemical analysis, and data processing. Although all errors cannot be eliminated from measurements, the magnitude of their uncertainty can be estimated and tracked over time. Since 1981, the USGS has operated an independent, external, quality-assurance project called the Blind Sample Project (BSP). The purpose of the BSP is to monitor and evaluate the quality of laboratory analytical results through the use of double-blind quality-control (QC) samples. The information provided by the BSP assists the laboratories in detecting and correcting problems in the analytical procedures. The information also can aid laboratory users in estimating the extent that laboratory errors contribute to the overall errors in their environmental data.
Mirzazadeh, Mehdi; Morovat, Alireza; James, Tim; Smith, Ian; Kirby, Justin; Shine, Brian
2016-03-01
Point-of-care testing allows rapid analysis of samples to facilitate prompt clinical decisions. Electrolyte and calcium abnormalities are common in acutely ill patients and can be associated with life-threatening consequences. There is uncertainty whether clinical decisions can be based on the results obtained from blood gas analysers or if laboratory results should be awaited. To assess the agreement between sodium, potassium and calcium results from blood gas and laboratory mainstream analysers in a tertiary centre, with a network consisting of one referral and two peripheral hospitals, consisting of three networked clinical biochemistry laboratories. Using the laboratory information management system database and over 11 000 paired samples in three hospital sites, the results of sodium, potassium and ionised calcium on blood gas analysers were studied over a 5-year period and compared with the corresponding laboratory results from the same patients booked in the laboratory within 1 h. The Pearson's linear correlation coefficient between laboratory and blood gas results for sodium, potassium and calcium were 0.92, 0.84 and 0.78, respectively. Deming regression analysis showed a slope of 1.04 and an intercept of -5.7 for sodium, slope of 0.93 and an intercept of 0.22 for potassium and a slope of 1.23 with an intercept of -0.55 for calcium. With some strict statistical assumptions, percentages of results lying outside the least significant difference were 9%, 26.7% and 20.8% for sodium, potassium and calcium, respectively. Most clinicians wait for the laboratory confirmation of results generated by blood gas analysers. In a large retrospective study we have shown that there is sufficient agreement between the results obtained from the blood gas and laboratory analysers to enable prompt clinical decisions to be made. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted under a licence) please go to http://www.bmj.com/company/products-services/rights-and-licensing/
Lab Analyses of Pet Coke Samples
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.
Cooperative investigation of precision and accuracy: In chemical analysis of silicate rocks
Schlecht, W.G.
1951-01-01
This is the preliminary report of the first extensive program ever organized to study the analysis of igneous rocks, a study sponsored by the United States Geological Survey, the Massachusetts Institute of Technology, and the Geophysical Laboratory of the Carnegie Institution of Washington. Large samples of two typical igneous rocks, a granite and a diabase, were carefully prepared and divided. Small samples (about 70 grams) of each were sent to 25 rock-analysis laboratories throughout the world; analyses of one or both samples were reported by 34 analysts in these laboratories. The results, which showed rather large discrepancies, are presented in histograms. The great discordance in results reflects the present unsatisfactory state of rock analysis. It is hoped that the ultimate establishment of standard samples and procedures will contribute to the improvement of quality of analyses. The two rock samples have also been thoroughly studied spectrographically and petrographically. Detailed reports of all the studies will be published.
Chemical analyses of surface waters in Oklahoma, September - December, 1944
,
1945-01-01
Red River at Denison Dam, Texas Sport samples were collected at the remainder of the stations. The analyses of the spot samples were made largely in a laboratory provided by the Oklahoma A. & M. College, under the supervision of Dr. O.M. Smith, Head, Department of Chemistry; Dr. S.R. Wood, Associate Professor of Chemistry; and W.W. Hastings, U.S. Geological Survey. The daily samples were analyzed in the water resources laboratory of the Geological Survey at Austin, Texas. These data have been summarized in a report to the Oklahoma Planning and Resources Board prepared by the U.S. Geological Survey, March 1, 1945. The streams of Oklahoma are classified into two major drainage basins: the Arkansas River and the Red River and their tributaries. The attached analyses are arranged in geographical order for their respective drainage basins, with records listed in downstream order for stations on the main stem first, followed by the analyses for the tributaries. When available, the mean daily discharge is given for the analyses.
Mayer, Horst; Brümmer, Jens; Brinkmann, Thomas
2011-01-01
To implement Lean Six Sigma in our central laboratory we conducted a project to measure single pre-analytical steps influencing turnaround time (TAT) of emergency department (ED) serum samples. The traditional approach of extracting data from the Laboratory Information System (LIS) for a retrospective calculation of a mean TAT is not suitable. Therefore, we used radiofrequency identification (RFID) chips for real time tracking of individual samples at any pre-analytical step. 1,200 serum tubes were labelled with RFID chips and were provided to the emergency department. 3 RFID receivers were installed in the laboratory: at the outlet of the pneumatic tube system, at the centrifuge, and in the analyser area. In addition, time stamps of sample entry at the automated sample distributor and communication of results from the analyser were collected from LIS. 1,023 labelled serum tubes arrived at our laboratory. 899 RFID tags were used for TAT calculation. The following transfer times were determined (median 95th percentile in min:sec): pneumatic tube system --> centrifuge (01:25/04:48), centrifuge --> sample distributor (14:06/5:33), sample distributor --> analysis system zone (02:39/15:07), analysis system zone --> result communication (12:42/22:21). Total TAT was calculated at 33:19/57:40 min:sec. Manual processes around centrifugation were identified as a major part of TAT with 44%/60% (median/95th percentile). RFID is a robust, easy to use, and error-free technology and not susceptible to interferences in the laboratory environment. With this study design we were able to measure significant variations in a single manual sample transfer process. We showed that TAT is mainly influenced by manual steps around the centrifugation process and we concluded that centrifugation should be integrated in solutions for total laboratory automation.
7 CFR 94.3 - Analyses performed and locations of laboratories.
Code of Federal Regulations, 2013 CFR
2013-01-01
... by AMS Science and Technology (S&T) personnel for microbiological, chemical, and physical attributes..., microorganism, dextrin, or other substance. (e) The AMS Science and Technology's Eastern Laboratory shall... samples are performed at the following USDA location: USDA, AMS, Science & Technology, Eastern Laboratory...
7 CFR 94.3 - Analyses performed and locations of laboratories.
Code of Federal Regulations, 2012 CFR
2012-01-01
... by AMS Science and Technology (S&T) personnel for microbiological, chemical, and physical attributes..., microorganism, dextrin, or other substance. (e) The AMS Science and Technology's Eastern Laboratory shall... samples are performed at the following USDA location: USDA, AMS, Science & Technology, Eastern Laboratory...
7 CFR 94.3 - Analyses performed and locations of laboratories.
Code of Federal Regulations, 2014 CFR
2014-01-01
... by AMS Science and Technology (S&T) personnel for microbiological, chemical, and physical attributes..., microorganism, dextrin, or other substance. (e) The AMS Science and Technology's Eastern Laboratory shall... samples are performed at the following USDA location: USDA, AMS, Science & Technology, Eastern Laboratory...
NASA Astrophysics Data System (ADS)
Ergenç, Duygu; Freire, David; Fort, Rafael
2016-04-01
The chemical characterization of lime mortars used in Roman period has a great significance and plays a key role in the acquisition of knowledge with respect to construction technology, raw materials and, accordingly, in its conservation works. When it comes to cultural heritage studies, sampling is always complicated since the minimum damage is the primary concern. The use of non-destructive techniques and direct measurements with portable devices reduce the amount of samples and time consumed in analyses, consequently it could be stated that such techniques are extremely useful in conservation and restoration works. In this study, the portable XRF device was used to determine the composition of chemical elements which compose the Roman lime mortars in the archaeological site of Complutum, Alcalá de Henares (Madrid, Spain) which is listed as a World Heritage Site by UNESCO since 1998. Portable XRF devices have some detection limits below the ones of the laboratory equipment that are immovable and require sampling. In order to correlate the results, sampling and grinding were initially done to prepare the powders for the laboratory XRF analysis with the following elements: Si, Al, Fe, Ca, Mg, K, Ti, Nb, Zr, Sr, Rb, Pb, Zn and Cr. The analyses of the powdered samples were conducted with the laboratory equipment PHILIPS Magix Pro (PW-2440) from the Centre of Scientific Instrumentation CIC in the University of Granada, and the results were compared to the results gathered with X Ray Florescence (EDTRX) THERMO NITON model XL3T from the Petrophysics Laboratory Geosciences Institute IGEO (CSIC-UCM). Analyses were performed on the surfaces of the samples -without any previous preparation-, and on the powdered samples to compare the variations between both traditional XRF analyses and the portable XRF. A good correlation was found among the results obtained by the laboratory equipment, the portable device as well as the surface measurements. The results of this study enable to differentiate the types of lime mortars used in the site (Caementicium and Signinum) and in different buildings that form the Roman city. Acknowledgements: Thanks to the project CLIMORTEC (BIA2014-53911-R), to CEI-Moncloa of UCM-UPM-UCM and to Madrid Community for funding the Geomateriales2 (P2013/MIT2914) program
NASA Technical Reports Server (NTRS)
Messenger, S.; Connolly, H. C., Jr.; Lauretta, D. S.; Bottke, W. F.
2014-01-01
The NASA New Frontiers Mission OSRIS-REx will return surface regolith samples from near-Earth asteroid 101955 Bennu in September 2023. This target is classified as a B-type asteroid and is spectrally similar to CI and CM chondrite meteorites [1]. The returned samples are thus expected to contain primitive ancient Solar System materials that formed in planetary, nebular, interstellar, and circumstellar environments. Laboratory studies of primitive astromaterials have yielded detailed constraints on the origins, properties, and evolutionary histories of a wide range of Solar System bodies. Yet, the parent bodies of meteorites and cosmic dust are generally unknown, genetic and evolutionary relationships among asteroids and comets are unsettled, and links between laboratory and remote observations remain tenuous. The OSIRIS-REx mission will offer the opportunity to coordinate detailed laboratory analyses of asteroidal materials with known and well characterized geological context from which the samples originated. A primary goal of the OSIRIS-REx mission will be to provide detailed constraints on the origin and geological and dynamical history of Bennu through coordinated analytical studies of the returned samples. These microanalytical studies will be placed in geological context through an extensive orbital remote sensing campaign that will characterize the global geological features and chemical diversity of Bennu. The first views of the asteroid surface and of the returned samples will undoubtedly bring remarkable surprises. However, a wealth of laboratory studies of meteorites and spacecraft encounters with primitive bodies provides a useful framework to formulate priority scientific questions and effective analytical approaches well before the samples are returned. Here we summarize our approach to unraveling the geological history of Bennu through returned sample analyses.
Lincoln, Tricia A.; Horan-Ross, Debra A.; McHale, Michael R.; Lawrence, Gregory B.
2005-01-01
Results from blind reference-sample analyses indicated that data-quality objectives were met by at least 90 percent of the calcium, pH, potassium, and sodium samples. Data-quality objectives were met by 77 percent of the chloride samples, 83 percent of the magnesium samples, and 80 percent of the sulfate samples. There is insufficient data to evaluate the specific conductance samples.
Intact Capture, Aerogel, SOCCER, Stardust and LIFE
NASA Astrophysics Data System (ADS)
Tsou, P.
2013-11-01
In order to definitively determine many complex exploration curiosities, we must bring samples to terrestrial laboratories for detailed analyses by collaborating laboratories and analysts. We report this endeavor in SOCCER, NEARER, Stardust and LIFE.
Reddy, Michael M.; Gunther, Charmaine D.
2012-01-01
Samples were collected from groundwater wells in and about the city of Las Vegas, Nevada, and were analyzed for selected major, minor and trace constituents. Analyses of blank and reference samples are summarized as mean and standard deviation values for all positive results.
Contracting of Samples for Chemical Analyses. What You Should Know about It
1990-08-01
Laboratory (AFSC) Human Systems Division Brooks Air Force Base , Texas 78235-5501 o O NOTICES When Government drawings, specifications, or other data...Assurance Efforts 3 Analyses Costs 3 Certifications 4 How To Protect Your Base And The Air Force 4 References 6 Appendix A - IG Writeup Of A Laboratory...their agency certifications showing the period of certitication and for what analyses. HOW TO PROTECT YOUR BASE AND THE AIR FORCE What I am wondering on
See, Randolph B.; Schroder, LeRoy J.; Willoughby, Timothy C.
1988-01-01
During 1986, the U.S. Geological Survey operated three programs to provide external quality-assurance monitoring of the National Atmospheric Deposition Program and National Trends Network. An intersite-comparison program was used to assess the accuracy of onsite pH and specific-conductance determinations at quarterly intervals. The blind-audit program was used to assess the effect of routine sample handling on the precision and bias of program and network wet-deposition data. Analytical results from four laboratories, which routinely analyze wet-deposition samples, were examined to determine if differences existed between laboratory analytical results and to provide estimates of the analytical precision of each laboratory. An average of 78 and 89 percent of the site operators participating in the intersite-comparison met the network goals for pH and specific conductance. A comparison of analytical values versus actual values for samples submitted as part of the blind-audit program indicated that analytical values were slightly but significantly (a = 0.01) larger than actual values for pH, magnesium, sodium, and sulfate; analytical values for specific conductance were slightly less than actual values. The decreased precision in the analyses of blind-audit samples when compared to interlaboratory studies indicates that a large amount of uncertainty in network deposition data may be a result of routine field operations. The results of the interlaboratory comparison study indicated that the magnitude of the difference between laboratory analyses was small for all analytes. Analyses of deionized, distilled water blanks by participating laboratories indicated that the laboratories had difficulty measuring analyte concentrations near their reported detection limits. (USGS)
This product is an LC/MS/MS single laboratory validated method for the determination of cylindrospermopsin and anatoxin-a in ambient waters. The product contains step-by-step instructions for sample preparation, analyses, preservation, sample holding time and QC protocols to ensu...
Trace-element analyses of core samples from the 1967-1988 drillings of Kilauea Iki lava lake, Hawaii
Helz, Rosalind Tuthill
2012-01-01
This report presents previously unpublished analyses of trace elements in drill core samples from Kilauea Iki lava lake and from the 1959 eruption that fed the lava lake. The two types of data presented were obtained by instrumental neutron-activation analysis (INAA) and energy-dispersive X-ray fluorescence analysis (EDXRF). The analyses were performed in U.S. Geological Survey (USGS) laboratories from 1989 to 1994. This report contains 93 INAA analyses on 84 samples and 68 EDXRF analyses on 68 samples. The purpose of the study was to document trace-element variation during chemical differentiation, especially during the closed-system differentiation of Kilauea Iki lava lake.
Results and analysis of saltstone cores taken from saltstone disposal unit cell 2A
DOE Office of Scientific and Technical Information (OSTI.GOV)
Reigel, M. M.; Hill, K. A.
2016-03-01
As part of an ongoing Performance Assessment (PA) Maintenance Plan, Savannah River Remediation (SRR) has developed a sampling and analyses strategy to facilitate the comparison of field-emplaced samples (i.e., saltstone placed and cured in a Saltstone Disposal Unit (SDU)) with samples prepared and cured in the laboratory. The primary objectives of the Sampling and Analyses Plan (SAP) are; (1) to demonstrate a correlation between the measured properties of laboratory-prepared, simulant samples (termed Sample Set 3), and the field-emplaced saltstone samples (termed Sample Set 9), and (2) to validate property values assumed for the Saltstone Disposal Facility (SDF) PA modeling. Themore » analysis and property data for Sample Set 9 (i.e. six core samples extracted from SDU Cell 2A (SDU2A)) are documented in this report, and where applicable, the results are compared to the results for Sample Set 3. Relevant properties to demonstrate the aforementioned objectives include bulk density, porosity, saturated hydraulic conductivity (SHC), and radionuclide leaching behavior.« less
Five years' experience of classical swine fever polymerase chain reaction ring trials in France.
Po, F; Le Dimna, M; Le Potier, M F
2011-12-01
Since 2004, the French National Reference Laboratory for classical swine fever (CSF) has conducted an annual proficiency test (PT) to evaluate the ability of local veterinary laboratories to perform real-time polymerase chain reaction (PCR) for CSF virus. The results of five years of testing (2004-2008) are described here. The PT was conducted under blind conditions on 20 samples. The same batch of samples was used for all five years. The number of laboratories that analysed the samples increased from four in 2004 to 13 in 2008. The results of the PT showed the following: cross-contamination between samples and deficiencies in RNA preparation can occur even in experienced laboratories; sample homogeneity should be checked carefully before selection; samples stored at-80 degrees C for several years remain stable; and poor shipment conditions do not damage the samples with regard to detection of CSF virus genome. These results will enable redesign of the panel to improve the overall quality of the PT, which will encourage laboratories to check and improve their PCR procedures and expertise. This is an excellent way to determine laboratory performance.
Park, Douglas L; Coates, Scott; Brewer, Vickery A; Garber, Eric A E; Abouzied, Mohamed; Johnson, Kurt; Ritter, Bruce; McKenzie, Deborah
2005-01-01
Performance Tested Method multiple laboratory validations for the detection of peanut protein in 4 different food matrixes were conducted under the auspices of the AOAC Research Institute. In this blind study, 3 commercially available ELISA test kits were validated: Neogen Veratox for Peanut, R-Biopharm RIDASCREEN FAST Peanut, and Tepnel BioKits for Peanut Assay. The food matrixes used were breakfast cereal, cookies, ice cream, and milk chocolate spiked at 0 and 5 ppm peanut. Analyses of the samples were conducted by laboratories representing industry and international and U.S governmental agencies. All 3 commercial test kits successfully identified spiked and peanut-free samples. The validation study required 60 analyses on test samples at the target level 5 microg peanut/g food and 60 analyses at a peanut-free level, which was designed to ensure that the lower 95% confidence limit for the sensitivity and specificity would not be <90%. The probability that a test sample contains an allergen given a prevalence rate of 5% and a positive test result using a single test kit analysis with 95% sensitivity and 95% specificity, which was demonstrated for these test kits, would be 50%. When 2 test kits are run simultaneously on all samples, the probability becomes 95%. It is therefore recommended that all field samples be analyzed with at least 2 of the validated kits.
Vacata, Vladimir; Jahns-Streubel, Gerlinde; Baldus, Mirjana; Wood, William Graham
2007-01-01
This report was written in response to the article by Wood published recently in this journal. It describes a practical solution to the problems of controlling the pre-analytical phase in the clinical diagnostic laboratory. As an indicator of quality in the pre-analytical phase of sample processing, a target analyte was chosen which is sensitive to delay in centrifugation and/or analysis. The results of analyses of the samples sent by satellite medical practitioners were compared with those from an on-site hospital laboratory with a controllable optimized pre-analytical phase. The aim of the comparison was: (a) to identify those medical practices whose mean/median sample values significantly deviate from those of the control situation in the hospital laboratory due to the possible problems in the pre-analytical phase; (b) to aid these laboratories in the process of rectifying these problems. A Microsoft Excel-based Pre-Analytical Survey tool (PAS tool) has been developed which addresses the above mentioned problems. It has been tested on serum potassium which is known to be sensitive to delay and/or irregularities in sample treatment. The PAS tool has been shown to be one possibility for improving the quality of the analyses by identifying the sources of problems within the pre-analytical phase, thus allowing them to be rectified. Additionally, the PAS tool has an educational value and can also be adopted for use in other decentralized laboratories.
Wassenaar, L I; Terzer-Wassmuth, S; Douence, C; Araguas-Araguas, L; Aggarwal, P K; Coplen, T B
2018-03-15
Water stable isotope ratios (δ 2 H and δ 18 O values) are widely used tracers in environmental studies; hence, accurate and precise assays are required for providing sound scientific information. We tested the analytical performance of 235 international laboratories conducting water isotope analyses using dual-inlet and continuous-flow isotope ratio mass spectrometers and laser spectrometers through a water isotope inter-comparison test. Eight test water samples were distributed by the IAEA to international stable isotope laboratories. These consisted of a core set of five samples spanning the common δ-range of natural waters, and three optional samples (highly depleted, enriched, and saline). The fifth core sample contained unrevealed trace methanol to assess analyst vigilance to the impact of organic contamination on water isotopic measurements made by all instrument technologies. For the core and optional samples ~73 % of laboratories gave acceptable results within 0.2 ‰ and 1.5 ‰ of the reference values for δ 18 O and δ 2 H, respectively; ~27 % produced unacceptable results. Top performance for δ 18 O values was dominated by dual-inlet IRMS laboratories; top performance for δ 2 H values was led by laser spectrometer laboratories. Continuous-flow instruments yielded comparatively intermediate results. Trace methanol contamination of water resulted in extreme outlier δ-values for laser instruments, but also affected reactor-based continuous-flow IRMS systems; however, dual-inlet IRMS δ-values were unaffected. Analysis of the laboratory results and their metadata suggested inaccurate or imprecise performance stemmed mainly from skill- and knowledge-based errors including: calculation mistakes, inappropriate or compromised laboratory calibration standards, poorly performing instrumentation, lack of vigilance to contamination, or inattention to unreasonable isotopic outcomes. To counteract common errors, we recommend that laboratories include 1-2 'known' control standards in all autoruns; laser laboratories should screen each autorun for spectral contamination; and all laboratories should evaluate whether derived d-excess values are realistic when both isotope ratios are measured. Combined, these data evaluation strategies should immediately inform the laboratory about fundamental mistakes or compromised samples. Copyright © 2018 John Wiley & Sons, Ltd.
Wassenaar, L. I.; Terzer-Wassmuth, S.; Douence, C.; Araguas-Araguas, L.; Aggarwal, P. K.; Coplen, Tyler B.
2018-01-01
RationaleWater stable isotope ratios (δ2H and δ18O values) are widely used tracers in environmental studies; hence, accurate and precise assays are required for providing sound scientific information. We tested the analytical performance of 235 international laboratories conducting water isotope analyses using dual-inlet and continuous-flow isotope ratio mass spectrometers and laser spectrometers through a water isotope inter-comparison test.MethodsEight test water samples were distributed by the IAEA to international stable isotope laboratories. These consisted of a core set of five samples spanning the common δ-range of natural waters, and three optional samples (highly depleted, enriched, and saline). The fifth core sample contained unrevealed trace methanol to assess analyst vigilance to the impact of organic contamination on water isotopic measurements made by all instrument technologies.ResultsFor the core and optional samples ~73 % of laboratories gave acceptable results within 0.2 ‰ and 1.5 ‰ of the reference values for δ18O and δ2H, respectively; ~27 % produced unacceptable results. Top performance for δ18O values was dominated by dual-inlet IRMS laboratories; top performance for δ2H values was led by laser spectrometer laboratories. Continuous-flow instruments yielded comparatively intermediate results. Trace methanol contamination of water resulted in extreme outlier δ-values for laser instruments, but also affected reactor-based continuous-flow IRMS systems; however, dual-inlet IRMS δ-values were unaffected.ConclusionsAnalysis of the laboratory results and their metadata suggested inaccurate or imprecise performance stemmed mainly from skill- and knowledge-based errors including: calculation mistakes, inappropriate or compromised laboratory calibration standards, poorly performing instrumentation, lack of vigilance to contamination, or inattention to unreasonable isotopic outcomes. To counteract common errors, we recommend that laboratories include 1–2 'known' control standards in all autoruns; laser laboratories should screen each autorun for spectral contamination; and all laboratories should evaluate whether derived d-excess values are realistic when both isotope ratios are measured. Combined, these data evaluation strategies should immediately inform the laboratory about fundamental mistakes or compromised samples.
Mineral discrimination using a portable ratio-determining radiometer.
Whitney, G.; Abrams, M.J.; Goetz, A.F.H.
1983-01-01
A portable ratio-determining radiometer has been tested in the laboratory to evaluate the use of narrow band filters for separating geologically important minerals. The instrument has 10 bands in the visible and near-infrared portion of the spectrum (0.5-2.4mm), positioned to sample spectral regions having absorption bands characteristic of minerals in this wavelength region. Measurements and statistical analyses were performed on 66 samples, which were characterized by microscopic and X-ray diffraction analyses. Comparison with high-resolution laboratory spectral reflectance curves indicated that the radiometer's raw values faithfully reproduced the shapes of the spectra. -from Authors
Ludtke, Amy S.; Woodworth, Mark T.; Marsh, Philip S.
2000-01-01
The U.S. Geological Survey operates a quality-assurance program based on the analyses of reference samples for two laboratories: the National Water Quality Laboratory and the Quality of Water Service Unit. Reference samples that contain selected inorganic, nutrient, and low-level constituents are prepared and submitted to the laboratory as disguised routine samples. The program goal is to estimate precision and bias for as many analytical methods offered by the participating laboratories as possible. Blind reference samples typically are submitted at a rate of 2 to 5 percent of the annual environmental-sample load for each constituent. The samples are distributed to the laboratories throughout the year. The reference samples are subject to the identical laboratory handling, processing, and analytical procedures as those applied to environmental samples and, therefore, have been used as an independent source to verify bias and precision of laboratory analytical methods and ambient water-quality measurements. The results are stored permanently in the National Water Information System and the Blind Sample Project's data base. During water year 1998, 95 analytical procedures were evaluated at the National Water Quality Laboratory and 63 analytical procedures were evaluated at the Quality of Water Service Unit. An overall evaluation of the inorganic and low-level constituent data for water year 1998 indicated 77 of 78 analytical procedures at the National Water Quality Laboratory met the criteria for precision. Silver (dissolved, inductively coupled plasma-mass spectrometry) was determined to be imprecise. Five of 78 analytical procedures showed bias throughout the range of reference samples: chromium (dissolved, inductively coupled plasma-atomic emission spectrometry), dissolved solids (dissolved, gravimetric), lithium (dissolved, inductively coupled plasma-atomic emission spectrometry), silver (dissolved, inductively coupled plasma-mass spectrometry), and zinc (dissolved, inductively coupled plasma-mass spectrometry). At the National Water Quality Laboratory during water year 1998, lack of precision was indicated for 2 of 17 nutrient procedures: ammonia as nitrogen (dissolved, colorimetric) and orthophosphate as phosphorus (dissolved, colorimetric). Bias was indicated throughout the reference sample range for ammonia as nitrogen (dissolved, colorimetric, low level) and nitrate plus nitrite as nitrogen (dissolved, colorimetric, low level). All analytical procedures tested at the Quality of Water Service Unit during water year 1998 met the criteria for precision. One of the 63 analytical procedures indicated a bias throughout the range of reference samples: aluminum (whole-water recoverable, inductively coupled plasma-atomic emission spectrometry, trace).
Fornaini, Carlo; Passaretti, Francesca; Villa, Elena; Rocca, Jean-Paul; Merigo, Elisabetta; Vescovi, Paolo; Meleti, Marco; Manfredi, Maddalena; Nammour, Samir
2011-07-01
The Nd:YAG laser has been used since 1970 in dental laboratories to weld metals on dental prostheses. Recently in several clinical cases, we have suggested that the Nd:YAG laser device commonly utilized in the dental office could be used to repair broken fixed, removable and orthodontic prostheses and to weld metals directly in the mouth. The aim of this work was to evaluate, using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and dynamic mechanical analysis (DMA), the quality of the weld and its mechanical strength, comparing a device normally used in dental laboratory and a device normally used in the dental office for oral surgery, the same as that described for intraoral welding. Metal plates of a Co-Cr-Mo dental alloy and steel orthodontic wires were subjected to four welding procedures: welding without filler metal using the laboratory laser, welding with filler metal using the laboratory laser, welding without filler metal using the office laser, and welding with filler metal using the office laser. The welded materials were then analysed by SEM, EDS and DMA. SEM analysis did not show significant differences between the samples although the plates welded using the office laser without filler metal showed a greater number of fissures than the other samples. EDS microanalysis of the welding zone showed a homogeneous composition of the metals. Mechanical tests showed similar elastic behaviours of the samples, with minimal differences between the samples welded with the two devices. No wire broke even under the maximum force applied by the analyser. This study seems to demonstrate that the welds produced using the office Nd:YAG laser device and the laboratory Nd:YAG laser device, as analysed by SEM, EDS and DMA, showed minimal and nonsignificant differences, although these findings need to be confirmed using a greater number of samples.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Adams, Wade C.
Oak Ridge Institute for Science and Education (ORISE) personnel visited the United Nuclear Corporation (UNC) Naval Products site on three separate occasions during the months of October and November 2011. The purpose of these visits was to conduct confirmatory surveys of soils associated with the Argyle Street sewer line that was being removed. Soil samples were collected from six different, judgmentally determined locations in the Argyle Street sewer trench. In addition to the six soil samples collected by ORISE, four replicate soil samples were collected by Cabrera Services, Inc. (CSI) for analysis by the ORISE laboratory. Replicate samples S0010 andmore » S0011 were final status survey (FSS) bias samples; S0012 was an FSS systematic sample; and S0015 was a waste characterization sample. Six soil samples were also collected for background determination. Uranium-235 and uranium-238 concentrations were determined via gamma spectroscopy; the spectra were also reviewed for other identifiable photopeaks. Radionuclide concentrations for these soil samples are provided. In addition to the replicate samples and the samples collected by ORISE, CSI submitted three soil samples for inter-laboratory comparison analyses. One sample was from the background reference area, one was from waste characterization efforts (material inside the sewer line), and one was a FSS sample. The inter-laboratory comparison analyses results between ORISE and CSI were in agreement, except for one sample collected in the reference area. Smear results For Argyle Street sewer pipes are tabulated.« less
Tank 241-AZ-102 Privatization Push Mode Core Sampling and Analysis Plan
DOE Office of Scientific and Technical Information (OSTI.GOV)
RASMUSSEN, J.H.
1999-08-02
This sampling and analysis plan (SAP) identifies characterization objectives pertaining to sample collection, laboratory analytical evaluation, and reporting requirements for samples obtained from tank 241-AZ-102. The purpose of this sampling event is to obtain information about the characteristics of the contents of 241-AZ-102 required to satisfy the Data Quality Objectives For TWRS Privatization Phase I: Confirm Tank TIS An Appropriate Feed Source For High-Level Waste Feed Batch X(HLW DQO) (Nguyen 1999a), Data Quality Objectives For TWRS Privatization Phase 1: Confirm Tank TIS An Appropriate Feed Source For Low-Activity Waste Feed Batch X (LAW DQO) (Nguyen 1999b), Low Activity Waste andmore » High Level Waste Feed Data Quality Objectives (L&H DQO) (Patello et al. 1999) and Characterization Data Needs for Development, Design, and Operation of Retrieval Equipment Developed through the Data Quality Objective Process (Equipment DQO) (Bloom 1996). The Tank Characterization Technical Sampling Basis document (Brown et al. 1998) indicates that these issues, except the Equipment DQO apply to tank 241-AZ-102 for this sampling event. The Equipment DQO is applied for shear strength measurements of the solids segments only. Poppiti (1999) requires additional americium-241 analyses of the sludge segments. Brown et al. (1998) also identify safety screening, regulatory issues and provision of samples to the Privatization Contractor(s) as applicable issues for this tank. However, these issues will not be addressed via this sampling event. Reynolds et al. (1999) concluded that information from previous sampling events was sufficient to satisfy the safety screening requirements for tank 241 -AZ-102. Push mode core samples will be obtained from risers 15C and 24A to provide sufficient material for the chemical analyses and tests required to satisfy these data quality objectives. The 222-S Laboratory will extrude core samples, composite the liquids and solids, perform chemical analyses, and provide subsamples to the Process Chemistry Laboratory. The Process Chemistry Laboratory will prepare test plans and perform process tests to evaluate the behavior of the 241-AZ-102 waste undergoing the retrieval and treatment scenarios defined in the applicable DQOs. Requirements for analyses of samples originating in the process tests will be documented in the corresponding test plan.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Longmire, Patrick A.; Goff, Fraser; Counce, D. A.
2004-01-01
Background or baseline water chemistry data and information are required to distingu ish between contaminated and non-contaminated waters for environmental investigations conducted at Los Alamos National Laboratory (referred to as the Laboratory). The term 'background' refers to natural waters discharged by springs or penetrated by wells that have not been contaminated by LANL or other municipal or industrial activities, and that are representative of groundwater discharging from their respective aquifer material. These investigations are conducted as part of the Environmental Restoration (ER) Project, Groundwater Protection Program (GWPP), Laboratory Surveillance Program, the Hydrogeologic Workplan, and the Site-Wide Environmental Impact Statement (SWEIS).more » This poster provides a comprehensive, validated database of inorganic, organic, stable isotope, and radionuclide analyses of up to 136 groundwater samples collected from 15 baseline springs and wells located in and around Los Alamos National Laboratory, New Mexico. The region considered in this investigation extends from the western edge of the Jemez Mountains eastward to the Rio Grande and from Frijoles Canyon northward to Garcia Canyon. Figure 1 shows the fifteen stations sampled for this investigation. The sampling stations and associated aquifer types are summarized in Table 1.« less
Marine anthropogenic radiotracers in the Southern Hemisphere: New sampling and analytical strategies
NASA Astrophysics Data System (ADS)
Levy, I.; Povinec, P. P.; Aoyama, M.; Hirose, K.; Sanchez-Cabeza, J. A.; Comanducci, J.-F.; Gastaud, J.; Eriksson, M.; Hamajima, Y.; Kim, C. S.; Komura, K.; Osvath, I.; Roos, P.; Yim, S. A.
2011-04-01
The Japan Agency for Marine Earth Science and Technology conducted in 2003-2004 the Blue Earth Global Expedition (BEAGLE2003) around the Southern Hemisphere Oceans, which was a rare opportunity to collect many seawater samples for anthropogenic radionuclide studies. We describe here sampling and analytical methodologies based on radiochemical separations of Cs and Pu from seawater, as well as radiometric and mass spectrometry measurements. Several laboratories took part in radionuclide analyses using different techniques. The intercomparison exercises and analyses of certified reference materials showed a reasonable agreement between the participating laboratories. The obtained data on the distribution of 137Cs and plutonium isotopes in seawater represent the most comprehensive results available for the Southern Hemisphere Oceans.
Investigation into stutter ratio variability between different laboratories.
Bright, Jo-Anne; Curran, James M
2014-11-01
The determination of parameters such as stutter ratio is important to inform a laboratory's forensic DNA profile interpretation strategy. As part of a large data analysis project to implement a continuous model of DNA profile interpretation we analysed stutter ratio data from eight different forensic laboratories for the Promega PowerPlex(®) 21 multiplex. This allowed a comparison of inter laboratory variation. The maximum difference for any one laboratory from the average of the best fit determined by the model was 0.31%. These results indicate that stutter ratios calculated from samples analysed using the same profiling kit are not expected to differ between laboratories, even those using different capillary electrophoresis platforms. A common set of laboratory parameters are able to be generated and used for profile interpretation at all laboratories using the same multiplex and cycle number, potentially reducing the need for individual laboratories to determine stutter ratios. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.
Sampling procedure for lake or stream surface water chemistry
Robert Musselman
2012-01-01
Surface waters collected in the field for chemical analyses are easily contaminated. This research note presents a step-by-step detailed description of how to avoid sample contamination when field collecting, processing, and transporting surface water samples for laboratory analysis.
Box, Stephen E.; Bookstrom, Arthur A.; Ikramuddin, Mohammed; Lindsay, James
2001-01-01
(Fe), manganese (Mn), arsenic (As), and cadmium (Cd). In general inter-laboratory correlations are better for samples within the compositional range of the Standard Reference Materials (SRMs) from the National Institute of Standards and Technology (NIST). Analyses by EWU are the most accurate relative to the NIST standards (mean recoveries within 1% for Pb, Fe, Mn, and As, 3% for Zn and 5% for Cd) and are the most precise (within 7% of the mean at the 95% confidence interval). USGS-EDXRF is similarly accurate for Pb and Zn. XRAL and ACZ are relatively accurate for Pb (within 5-8% of certified NIST values), but were considerably less accurate for the other 5 elements of concern (10-25% of NIST values). However, analyses of sample splits by more than one laboratory reveal that, for some elements, XRAL (Pb, Mn, Cd) and ACZ (Pb, Mn, Zn, Fe) analyses were comparable to EWU analyses of the same samples (when values are within the range of NIST SRMs). These results suggest that, for some elements, XRAL and ACZ dissolutions are more effective on the matrix of the CdA samples than on the matrix of the NIST samples (obtained from soils around Butte, Montana). Splits of CdA samples analyzed by CHEMEX were the least accurate, yielding values 10-25% less than those of EWU.
Latysh, N.; Gordon, J.
2004-01-01
A study was undertaken to investigate differences between laboratory and field pH measurements for precipitation samples collected from 135 weekly precipitation-monitoring sites in the National Trends Network from 12/30/1986 to 12/28/1999. Differences in pH between field and laboratory measurements occurred for 96% of samples collected during this time period. Differences between the two measurements were evaluated for precipitation samples collected before and after January 1994, when modifications to sample-handling protocol and elimination of the contaminating bucket o-ring used in sample shipment occurred. Median hydrogen-ion and pH differences between field and laboratory measurements declined from 3.9 ??eq L-1 or 0.10 pH units before the 1994 protocol change to 1.4 ??eq L-1 or 0.04 pH units after the 1994 protocol change. Hydrogen-ion differences between field and laboratory measurements had a high correlation with the sample pH determined in the field. The largest pH differences between the two measurements occurred for high-pH samples (>5.6), typical of precipitation collected in Western United States; however low- pH samples (<5.0) displayed the highest variability in hydrogen-ion differences between field and laboratory analyses. Properly screened field pH measurements are a useful alternative to laboratory pH values for trend analysis, particularly before 1994 when laboratory pH values were influenced by sample-collection equipment.
Doping control analysis at the Rio 2016 Olympic and Paralympic Games.
Pereira, Henrique Marcelo Gualberto; Sardela, Vinicius Figueiredo; Padilha, Monica Costa; Mirotti, Luciana; Casilli, Alessandro; de Oliveira, Fabio Azamor; de Albuquerque Cavalcanti, Gustavo; Rodrigues, Lucas Martins Lisandro; de Araujo, Amanda Lessa Dutra; Levy, Rachel Santos; Teixeira, Pedro Antonio Castelo; de Oliveira, Felipe Alves Gomes; Duarte, Ana Carolina Giordani; Carneiro, Ana Carolina Dudenhoeffer; Evaristo, Joseph Albert Medeiros; Dos Santos, Gustavo Ramalho Cardoso; da Costa, Giovanni Carlo Verissimo; de Lima Castro, Fernando; Nogueira, Fabio Cesar Sousa; Scalco, Fernanda Bertão; Pizzatti, Luciana; de Aquino Neto, Francisco Radler
2017-11-01
This paper summarises the results obtained from the doping control analyses performed during the Summer XXXI Olympic Games (August 3-21, 2016) and the XV Paralympic Games (September 7-18, 2016). The analyses of all doping control samples were performed at the Brazilian Doping Control Laboratory (LBCD), a World Anti-Doping Agency (WADA)-accredited laboratory located in Rio de Janeiro, Brazil. A new facility at Rio de Janeiro Federal University (UFRJ) was built and fully operated by over 700 professionals, including Brazilian and international scientists, administrative staff, and volunteers. For the Olympic Games, 4913 samples were analysed. In 29 specimens, the presence of a prohibited substance was confirmed, resulting in adverse analytical findings (AAFs). For the Paralympic Games, 1687 samples were analysed, 12 of which were reported as AAFs. For both events, 82.8% of the samples were urine, and 17.2% were blood samples. In total, more than 31 000 analytical procedures were conducted. New WADA technical documents were fully implemented; consequently, state-of-the-art analytical toxicology instrumentation and strategies were applied during the Games, including different types of mass spectrometry (MS) analysers, peptide, and protein detection strategies, endogenous steroid profile measurements, and blood analysis. This enormous investment yielded one of the largest Olympic legacies in Brazil and South America. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.
NASA Astrophysics Data System (ADS)
Millan, M.; Szopa, C.; Buch, A.; Coll, P.; Glavin, D. P.; Freissinet, C.; Navarro-Gonzalez, R.; François, P.; Coscia, D.; Bonnet, J. Y.; Teinturier, S.; Cabane, M.; Mahaffy, P. R.
2016-09-01
The Sample Analysis at Mars (SAM) instrument onboard the Curiosity rover, is specifically designed for in situ molecular and isotopic analyses of martian surface materials and atmosphere. It contributes to the Mars Science Laboratory (MSL) missions primary scientific goal to characterize the potential past, present or future habitability of Mars. In all of the analyses of solid samples delivered to SAM so far, chlorinated organic compounds have been detected above instrument background levels and identified by gas chromatography coupled to mass spectrometry (GC-MS) (Freissinet et al., 2015; Glavin et al., 2013). While some of these may originate from reactions between oxychlorines and terrestrial organic carbon present in the instrument background (Glavin et al., 2013), others have been demonstrated to originate from indigenous organic carbon present in samples (Freissinet et al., 2015). We present here laboratory calibrations that focused on the analyses performed with the MXT-CLP GC column (SAM GC-5 channel) used for nearly all of the GC-MS analyses of the martian soil samples carried out with SAM to date. Complementary to the mass spectrometric data, gas chromatography allows us to separate and identify the species analyzable in a nominal SAM-GC run time of about 21 min. To characterize the analytical capabilities of this channel within the SAM Flight Model (FM) operating conditions on Mars, and their implications on the detection of organic matter, it is required to perform laboratory experimental tests and calibrations on spare model components. This work assesses the SAM flight GC-5 column efficiency, confirms the identification of the molecules based on their retention time, and enables a better understanding of the behavior of the SAM injection trap (IT) and its release of organic molecules. This work will enable further optimization of the SAM-GC runs for additional samples to be analyzed during the MSL mission.
NASA Technical Reports Server (NTRS)
Millan, M.; Szopa, C.; Buch, A.; Coll, P.; Glavin, D. P.; Freissinet, C.; Navarro-Gonzalez, R.; Francois, P.; Coscia, D.; Bonnet, J. Y.;
2016-01-01
The Sample Analysis at Mars (SAM) instrument onboard the Curiosity rover, is specifically designed for in situ molecular and isotopic analyses of martian surface materials and atmosphere. It contributes to the Mars Science Laboratory (MSL) missions primary scientific goal to characterize the potential past, present or future habitability of Mars. In all of the analyses of solid samples delivered to SAM so far, chlorinated organic compounds have been detected above instrument background levels and identified by gas chromatography coupled to mass spectrometry (GC-MS) (Freissinet et al., 2015; Glavin et al., 2013). While some of these may originate from reactions between oxychlorines and terrestrial organic carbon present in the instrument background (Glavin et al., 2013), others have been demonstrated to originate from indigenous organic carbon present in samples (Freissinet et al., 2015). We present here laboratory calibrations that focused on the analyses performed with the MXT-CLP GC column (SAM GC-5 channel) used for nearly all of the GC-MS analyses of the martian soil samples carried out with SAM to date. Complementary to the mass spectrometric data, gas chromatography allows us to separate and identify the species analyzable in a nominal SAM-GC run time of about 21 min. To characterize the analytical capabilities of this channel within the SAM Flight Model (FM) operating conditions on Mars, and their implications on the detection of organic matter, it is required to perform laboratory experimental tests and calibrations on spare model components. This work assesses the SAM flight GC-5 column efficiency, confirms the identification of the molecules based on their retention time, and enables a better understanding of the behavior of the SAM injection trap (IT) and its release of organic molecules. This work will enable further optimization of the SAM-GC runs for additional samples to be analyzed during the MSL mission.
NASA Technical Reports Server (NTRS)
McAdam, A. C.; Franz, H. B.; Mahaffy, P. R.; Eigenbrode, J. L.; Stern, J. C.; Brunner, B.; Sutter, B.; Archer, P. D.; Ming , D. W.; Morris, R. V.;
2014-01-01
While in Yellowknife Bay, the Mars Science Laboratory Curiosity rover collected two drilled samples, John Klein (hereafter "JK") and Cumberland ("CB"), from the Sheepbed mudstone, as well as a scooped sample from the Rocknest aeolian bedform ("RN"). These samples were sieved by Curiosity's sample processing system and then several subsamples of these materials were delivered to the Sample Analysis at Mars (SAM) instrument suite and the CheMin X-ray diffraction/X-ray fluorescence instrument. CheMin provided the first in situ X-ray diffraction-based evidence of clay minerals on Mars, which are likely trioctahedral smectites (e.g., Fe-saponite) and comprise 20 wt% of the mudstone samples [1]. SAM's evolved gas analysis (EGA) mass spectrometry analyses of JK and CB subsamples, as well as RN subsamples, detected H2O, CO2, O2, H2, SO2, H2S, HCl, NO, OCS, CS2 and other trace gases evolved during pyrolysis. The identity of evolved gases and temperature( s) of evolution can augment mineral detection by CheMin and place constraints on trace volatile-bearing phases present below the CheMin detection limit or those phases difficult to characterize with XRD (e.g., X-ray amorphous phases). Here we will focus on the SAM H2O data, in the context of CheMin analyses, and comparisons to laboratory SAM-like analyses of several phyllosilicate minerals including smectites.
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
Glaser, Robert; Kurimo, Robert; Shulman, Stanley
2007-08-01
A performance test of NIOSH Method 5524/ASTM Method D-7049-04 for analysis of metalworking fluids (MWF) was conducted. These methods involve determination of the total and extractable weights of MWF samples; extractions are performed using a ternary blend of toluene:dichloromethane:methanol and a binary blend of methanol:water. Six laboratories participated in this study. A preliminary analysis of 20 blank samples was made to familiarize the laboratories with the procedure(s) and to estimate the methods' limits of detection/quantitation (LODs/LOQs). Synthetically generated samples of a semisynthetic MWF aerosol were then collected on tared polytetrafluoroethylene (PTFE) filters and analyzed according to the methods by all participants. Sample masses deposited (approximately 400-500 micro g) corresponded to amounts expected in an 8-hr shift at the NIOSH recommended exposure levels (REL) of 0.4 mg/m(3) (thoracic) and 0.5 mg/m(3) (total particulate). The generator output was monitored with a calibrated laser particle counter. One laboratory significantly underreported the sampled masses relative to the other five labs. A follow-up study compared only gravimetric results of this laboratory with those of two other labs. In the preliminary analysis of blanks; the average LOQs were 0.094 mg for the total weight analysis and 0.136 mg for the extracted weight analyses. For the six-lab study, the average LOQs were 0.064 mg for the total weight analyses and 0.067 mg for the extracted weight analyses. Using ASTM conventions, h and k statistics were computed to determine the degree of consistency of each laboratory with the others. One laboratory experienced problems with precision but not bias. The precision estimates for the remaining five labs were not different statistically (alpha = 0.005) for either the total or extractable weights. For all six labs, the average fraction extracted was > or =0.94 (CV = 0.025). Pooled estimates of the total coefficients of variation of analysis were 0.13 for the total weight samples and 0.13 for the extracted weight samples. An overall method bias of -5% was determined by comparing the overall mean concentration reported by the participants to that determined by the particle counter. In the three-lab follow-up study, the nonconsistent lab reported results that were unbiased but statistically less precise than the others; the average LOQ was 0.133 mg for the total weight analyses. It is concluded that aerosolized MWF sampled at concentrations corresponding to either of the NIOSH RELs can generally be shipped unrefrigerated, stored refrigerated up to 7 days, and then analyzed quantitatively and precisely for MWF using the NIOSH/ASTM procedures.
SOIL AND FILL LABORATORY SUPPORT - 1991
The report gives results of soil analysis laboratory work by the University of Florida in Support of the Florida Radon Research Program (FRRP). Analyses were performed on soil and fill samples collected during 1991 by the FRRP Research House program and the New House Evaluation P...
7 CFR 94.3 - Analyses performed and locations of laboratories.
Code of Federal Regulations, 2010 CFR
2010-01-01
... by AMS Science and Technology (S&T) personnel for microbiological, chemical, and physical attributes... product samples may be analyzed for extraneous material, color, color additive, pesticide, heavy metal, microorganism, dextrin, or other substance. (e) The AMS Science and Technology's Eastern Laboratory shall...
Parkhurst, David L.
1987-01-01
Chemical analyses are presented for 169 water samples from Tar Creek drainage and the Picher lead-zinc mining area of northeast Oklahoma and southeast Kansas. Water samples were taken from November 1983 through February 1986 from the abandoned mines, from points of mine-water discharge, and from surface-water locations upstream and downstream from mine discharge area. The pH, temperature, alkalinity, dissolved oxygen, and specific conductance were measured in the field. Laboratory analyses routinely included the major ions plus aluminum, cadmium, copper, iron, lead, manganese, nickel, and zinc. Non-routine analyses of dissolved gases and tritium are presented. Stable carbon-isotope ratios for 11 mine-water samples and three carbonate-rock samples are reported. Miscellaneous stream-discharge measurements made at the time of sampling or taken from gaging-station records are included in the report.
Process improvement for regulatory analyses of custom-blend fertilizers.
Wegner, Keith A
2014-01-01
Chemical testing of custom-blend fertilizers is essential to ensure that the products meet the formulation requirements. For purposes of proper crop nutrition and consumer protection, regulatory oversight promotes compliance and particular attention to blending and formulation specifications. Analyses of custom-blend fertilizer products must be performed and reported within a very narrow window in order to be effective. The Colorado Department of Agriculture's Biochemistry Laboratory is an ISO 17025 accredited facility and conducts analyses of custom-blend fertilizer products primarily during the spring planting season. Using the Lean Six Sigma (LSS) process, the Biochemistry Laboratory has reduced turnaround times from as much as 45 days to as little as 3 days. The LSS methodology focuses on waste reduction through identifying: non-value-added steps, unneeded process reviews, optimization of screening and confirmatory analyses, equipment utilization, nonessential reporting requirements, and inefficient personnel deployment. Eliminating these non-value-added activities helped the laboratory significantly shorten turnaround time and reduce costs. Key improvement elements discovered during the LSS process included: focused sample tracking, equipment redundancy, strategic supply stocking, batch size optimization, critical sample paths, elimination of nonessential QC reviews, and more efficient personnel deployment.
[Errors in laboratory daily practice].
Larrose, C; Le Carrer, D
2007-01-01
Legislation set by GBEA (Guide de bonne exécution des analyses) requires that, before performing analysis, the laboratory directors have to check both the nature of the samples and the patients identity. The data processing of requisition forms, which identifies key errors, was established in 2000 and in 2002 by the specialized biochemistry laboratory, also with the contribution of the reception centre for biological samples. The laboratories follow a strict criteria of defining acceptability as a starting point for the reception to then check requisition forms and biological samples. All errors are logged into the laboratory database and analysis report are sent to the care unit specifying the problems and the consequences they have on the analysis. The data is then assessed by the laboratory directors to produce monthly or annual statistical reports. This indicates the number of errors, which are then indexed to patient files to reveal the specific problem areas, therefore allowing the laboratory directors to teach the nurses and enable corrective action.
NASA Technical Reports Server (NTRS)
Stern, Jennifer C.; Navarro-Gonzalez, Rafael; Freissinet, Caroline; McKay, Christopher P.; Archer, P. Douglas, Jr.; Buch, Arnaud; Coll, Patrice; Eigenbrode, Jennifer L.; Franz, Heather B.; Glavin, Daniel P.;
2014-01-01
The Sampl;e Analysis at Mars (sam) instrument suite on the Mars Science Laboratory (MSL) Curiosity Rover detected both reduced and oxidized nitrogen bearing compounds during the pyrolysis of surface materials from the three sites at Gale Crater. Preliminary detections of nitrogen species include No, HCN, ClCN, and TFMA ((trifluoro-N-methyl-acetamide), Confirmation of indigenous Martian nitrogen-bearing compounds requires quantifying N contribution from the terrestrial derivatization reagents carried for SAM's wet chemistry experiment that contribute to the SAM background. Nitrogen species detected in the SAM solid sample analyses can also be produced during laboratory pyrolysis experiments where these reagents are heated in the presence of perchlorate a compound that has also been identified by SAM in Mars solid samples.
Martin, J; Schuster, T; Moessmer, G; Kochs, E F; Wagner, K J
2012-10-01
Thromboelastometry as point-of-care (POC) testing enables the analysis of the clotting process at the bedside, providing rapid results to guide haemostatic therapy. However, POC testing utilizes medical staff who are managing critically ill patients, as non-laboratory personnel may not be sufficiently trained to run the devices. To resolve these problems, thromboelastometry can be performed in the central laboratory and rapid transport of samples can be accomplished via a pneumatic tube system (PTS). This study compares thromboelastometry parameters of blood samples analysed immediately with those analysed after PTS transport. In patients with normal haemostasis, two arterial blood samples were collected from each patient (n=92) in citrated plastic tubes to investigate the assays INTEM (n=35), EXTEM (n=27), and FIBTEM (n=30). One blood sample was analysed immediately, the other sample after PTS transport. Thromboelastometry was performed using a single ROTEM(®) device. The mean clot firmness values were significantly lower for PTS samples in both the INTEM (-0.7 mm cf. -1.1 mm) and EXTEM (-1.4 cf. -1.7 mm) assays. INTEM coagulation time (CT) was significantly lower in PTS samples with a mean difference of -13 s. EXTEM CT was significantly higher in PTS samples with a mean difference of +3.9 s. Thromboelastometry parameters of blood samples analysed after PTS transport are significantly altered compared with those analysed immediately. However, in patients with normal haemostasis, the alterations were small and without clinical consequence, implying that analysis after PTS transport is an acceptable alternative to prompt analysis at the bedside. Further studies should focus on patients with impaired haemostasis.
D.S. Ross; S.W. Bailey; R.D. Briggs; J. Curry; I.J. Fernandez; G. Fredriksen; C.L. Goodale; P.W. Hazlett; P.R. Heine; C.E. Johnson; J.T. Larson; G.B. Lawrence; R.K. Kolka; R. Ouimet; D. Pare; D. deB Richter; C.D. Schirmer; R.A. Warby
2015-01-01
Long-term forest soil monitoring and research often requires a comparison of laboratory data generated at different times and in different laboratories. Quantifying the uncertainty associated with these analyses is necessary to assess temporal changes in soil properties. Forest soil chemical properties, and methods to measure these properties, often differ from...
Colucci, G; Giabbani, E; Barizzi, G; Urwyler, N; Alberio, L
2011-08-01
ROTEM(®) is considered a helpful point-of-care device to monitor blood coagulation. Centrally performed analysis is desirable but rapid transport of blood samples and real-time transmission of graphic results are an important prerequisite. The effect of sample transport through a pneumatic tube system on ROTEM(®) results is unknown. The aims of the present work were (i) to determine the influence of blood sample transport through a pneumatic tube system on ROTEM(®) parameters compared to manual transportation, and (ii) to verify whether graphic results can be transmitted on line via virtual network computing using local area network to the physician in charge of the patient. Single centre study with 30 normal volunteers. Two whole blood samples were transferred to the central haematology laboratory by either normal transport or pneumatic delivery. EXTEM, INTEM, FIBTEM and APTEM were analysed in parallel with two ROTEM(®) devices and compared. Connection between central laboratory, emergency and operating rooms was established using local area network. All collected ROTEM(®) parameters were within normal limits. No statistically significant differences between normal transport and pneumatic delivery were observed. Real-time transmission of the original ROTEM(®) curves using local area network is feasible and easy to establish. At our institution, transport of blood samples by pneumatic delivery does not influence ROTEM(®) parameters. Blood samples can be analysed centrally, and results transmitted live via virtual network computing to emergency or operating rooms. Prior to analyse blood samples centrally, the type of sample transport should be tested to exclude in vitro blood activation by local pneumatic transport system. © 2011 Blackwell Publishing Ltd.
EML Gamma Spectrometry Data Evaluation Program
DOE Office of Scientific and Technical Information (OSTI.GOV)
Decker, Karin M.
2001-01-01
This report presents the results of the analyses for the third EML Gamma Spectrometry Data Evaluation Program (October 1999). This program assists laboratories in providing more accurate gamma spectra analysis results and provides a means for users of gamma data to assess how a laboratory performed on various types of gamma spectrometry analyses. This is accomplished through the use of synthetic gamma spectra. A calibration spectrum, a background spectrum, and three sample spectra are sent to each participant in the spectral file format requested by the laboratory. The calibration spectrum contains nuclides covering the energy range from 59.5 keV tomore » 1836 keV. The participants are told fallout and fission product nuclides could be present. The sample spectra are designed to test the ability of the software and user to properly resolve multiplets and to identify and quantify nuclides in a complicated fission product spectrum. The participants were asked to report values and uncertainties as Becquerel per sample with no decay correction. Thirty-one sets of results were reported from a total of 60 laboratories who received the spectra. Six foreign laboratories participated. The percentage of the results within 1 of the expected value was 68, 33, and 46 for samples 1, 2, and 3, respectively. From all three samples, 18% of the results were more than 3 from the expected value. Eighty-three (12%) values out of a total of 682 expected results were not reported for the three samples. Approximately 30% of these false negatives were due the laboratories not reporting 144Pr in sample 2 which was present at the minimum detectable activity level. There were 53 false positives reported with 25% of these responses due to problems with background subtraction. The results show improvement in the ability of the software or user to resolve peaks separated by 1 keV. Improvement is still needed either in the analysis report produced by the software or in the review of these results by the users.« less
Brooks, M.H.; Schroder, L.J.; Malo, B.A.
1985-01-01
Four laboratories were evaluated in their analysis of identical natural and simulated precipitation water samples. Interlaboratory comparability was evaluated using analysis of variance coupled with Duncan 's multiple range test, and linear-regression models describing the relations between individual laboratory analytical results for natural precipitation samples. Results of the statistical analyses indicate that certain pairs of laboratories produce different results when analyzing identical samples. Analyte bias for each laboratory was examined using analysis of variance coupled with Duncan 's multiple range test on data produced by the laboratories from the analysis of identical simulated precipitation samples. Bias for a given analyte produced by a single laboratory has been indicated when the laboratory mean for that analyte is shown to be significantly different from the mean for the most-probable analyte concentrations in the simulated precipitation samples. Ion-chromatographic methods for the determination of chloride, nitrate, and sulfate have been compared with the colorimetric methods that were also in use during the study period. Comparisons were made using analysis of variance coupled with Duncan 's multiple range test for means produced by the two methods. Analyte precision for each laboratory has been estimated by calculating a pooled variance for each analyte. Analyte estimated precisions have been compared using F-tests and differences in analyte precisions for laboratory pairs have been reported. (USGS)
7 CFR 91.19 - General requirements of suitable samples.
Code of Federal Regulations, 2011 CFR
2011-01-01
... the analyses requested. (b) Each sample must be identified with the following information: (1) Product... other information which is required by the specific program under which analysis or test is performed. ... LABORATORY TESTING PROGRAMS SERVICES AND GENERAL INFORMATION Samples § 91.19 General requirements of suitable...
7 CFR 91.19 - General requirements of suitable samples.
Code of Federal Regulations, 2012 CFR
2012-01-01
... the analyses requested. (b) Each sample must be identified with the following information: (1) Product... other information which is required by the specific program under which analysis or test is performed. ... LABORATORY TESTING PROGRAMS SERVICES AND GENERAL INFORMATION Samples § 91.19 General requirements of suitable...
7 CFR 91.19 - General requirements of suitable samples.
Code of Federal Regulations, 2013 CFR
2013-01-01
... the analyses requested. (b) Each sample must be identified with the following information: (1) Product... other information which is required by the specific program under which analysis or test is performed. ... LABORATORY TESTING PROGRAMS SERVICES AND GENERAL INFORMATION Samples § 91.19 General requirements of suitable...
7 CFR 91.19 - General requirements of suitable samples.
Code of Federal Regulations, 2010 CFR
2010-01-01
... the analyses requested. (b) Each sample must be identified with the following information: (1) Product... other information which is required by the specific program under which analysis or test is performed. ... LABORATORY TESTING PROGRAMS SERVICES AND GENERAL INFORMATION Samples § 91.19 General requirements of suitable...
7 CFR 91.19 - General requirements of suitable samples.
Code of Federal Regulations, 2014 CFR
2014-01-01
... the analyses requested. (b) Each sample must be identified with the following information: (1) Product... other information which is required by the specific program under which analysis or test is performed. ... LABORATORY TESTING PROGRAMS SERVICES AND GENERAL INFORMATION Samples § 91.19 General requirements of suitable...
Brooks, M.H.; Schroder, L.J.; Willoughby, T.C.
1987-01-01
The U.S. Geological Survey operated a blind audit sample program during 1974 to test the effects of the sample handling and shipping procedures used by the National Atmospheric Deposition Program and National Trends Network on the quality of wet deposition data produced by the combined networks. Blind audit samples, which were dilutions of standard reference water samples, were submitted by network site operators to the central analytical laboratory disguised as actual wet deposition samples. Results from the analyses of blind audit samples were used to calculate estimates of analyte bias associated with all network wet deposition samples analyzed in 1984 and to estimate analyte precision. Concentration differences between double blind samples that were submitted to the central analytical laboratory and separate analyses of aliquots of those blind audit samples that had not undergone network sample handling and shipping were used to calculate analyte masses that apparently were added to each blind audit sample by routine network handling and shipping procedures. These calculated masses indicated statistically significant biases for magnesium, sodium , potassium, chloride, and sulfate. Median calculated masses were 41.4 micrograms (ug) for calcium, 14.9 ug for magnesium, 23.3 ug for sodium, 0.7 ug for potassium, 16.5 ug for chloride and 55.3 ug for sulfate. Analyte precision was estimated using two different sets of replicate measures performed by the central analytical laboratory. Estimated standard deviations were similar to those previously reported. (Author 's abstract)
Wegner, S.J.
1989-01-01
Multiple water samples from 115 wells and 3 surface water sites were collected between 1980 and 1988 for the ongoing quality assurance program at the Idaho National Engineering Laboratory. The reported results from the six laboratories involved were analyzed for agreement using descriptive statistics. The constituents and properties included: tritium, plutonium-238, plutonium-239, -240 (undivided), strontium-90, americium-241, cesium-137, total dissolved chromium, selected dissolved trace metals, sodium, chloride, nitrate, selected purgeable organic compounds, and specific conductance. Agreement could not be calculated for purgeable organic compounds, trace metals, some nitrates and blank sample analyses because analytical uncertainties were not consistently reported. However, differences between results for most of these data were calculated. The blank samples were not analyzed for differences. The laboratory results analyzed using descriptive statistics showed a median agreement between all useable data pairs of 95%. (USGS)
Returning Samples from Enceladus
NASA Astrophysics Data System (ADS)
Tsou, P.; Kanik, I.; Brownlee, D.; McKay, C.; Anbar, A.; Glavin, D.; Yano, H.
2012-12-01
From the first half century of space exploration, we have obtained samples only from the Moon, comet Wild 2, the Solar Wind and the asteroid Itokawa. The in-depth analyses of these samples in terrestrial laboratories have yielded profound knowledge that could not have been obtained without the returned samples. While obtaining samples from Solar System bodies is crucial science, it is rarely done due to cost and complexity. Cassini's discovery of geysers on Enceladus and organic materials, indicate that there is an exceptional opportunity and science rational to do a low-cost flyby sample return mission, similar to what was done by the Stardust. The earliest low cost possible flight opportunity is the next Discovery Mission [Tsou et al 2012]. Enceladus Plume Discovery - While Voyager provided evidence for young surfaces on Enceladus, the existence of Enceladus plumes was discovered by Cassini. Enceladus and comets are the only known solar system bodies that have jets enabling sample collection without landing or surface contact. Cassini in situ Findings -Cassini's made many discoveries at Saturn, including the break up of large organics in the plumes of Enceladus. Four prime criteria for habitability are liquid water, a heat source, organics and nitrogen [McKay et al. 2008, Waite et al. 2009, Postberg et al. 2011]. Out of all the NASA designated habitability targets, Enceladus is the single body that presents evidence for all four criteria. Significant advancement in the exploration of the biological potential of Enceladus can be made on returned samples in terrestrial laboratories where the full power of state-of-the-art laboratory instrumentation and procedures can be used. Without serious limits on power, mass or even cost, terrestrial laboratories provide the ultimate in analytical capability, adaptability, reproducibility and reliability. What Questions can Samples Address? - Samples collected from the Enceladus plume will enable a thorough and replicated search for chemical biosignatures to understand the habitability potential of the subsurface ocean of Enceladus [Glavin et al. 2011]. By assessing the chiral excess among different amino acids, identifying chains of amino acids, isolate distinct sequences of these chains and the same for nucleic acids, we can formulate a new set of hypotheses to address some of the key science questions required for investigating the stage of extraterrestrial life at Enceladus beyond the four factors of habitability. Criticality of Analyses - For extraterrestrial organic matter analyses such as chirality and compound-specific isotopes, the repeatable robustness of laboratory measurements is a necessity. These analyses require a series of chemical extraction and derivatization steps prior to analysis that is adapted to the sample and procedures results-driven. The Stardust mission is an excellent example of the challenges in the analysis of organics. Confirmation of the cometary origin of the amino acid glycine from comet Wild 2 was obtained 3 years after the samples were returned to Earth. This long period of laboratory development allowed several modifications to the extraction protocol, multiple analytical techniques and instrumentations. Reference: Tsou et al., Astrobiology, in press 2012. McKay et al. Astrobiology 2008. Waite et al. Nature V 460 I 7254, 2009. Postberg et al. EPSC 642P 2011. Glavin et al., LPSC, #5002, 2011.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Shettel, D.L. Jr.; Langfeldt, S.L.; Youngquist, C.A.
This report presents a Hydrogeochemical and Stream Sediment Reconnaissance of the Christian NTMS Quadrangle, Alaska. In addition to this abbreviated data release, more complete data are available to the public in machine-readable form. These machine-readable data, as well as quarterly or semiannual program progress reports containing further information on the HSSR program in general, or on the Los Alamos National Laboratory portion of the program in particular, are available from DOE's Technical Library at its Grand Junction Area Office. Presented in this data release are location data, field analyses, and laboratory analyses of several different sample media. For the sakemore » of brevity, many field site observations have not been included in this volume; these data are, however, available on the magnetic tape. Appendices A through D describe the sample media and summarize the analytical results for each medium. The data have been subdivided by one of the Los Alamos National Laboratory sorting programs of Zinkl and others (1981a) into groups of stream-sediment, lake-sediment, stream-water, lake-water, and ground-water samples. For each group which contains a sufficient number of observations, statistical tables, tables of raw data, and 1:1,000,000 scale maps of pertinent elements have been included in this report. Also included are maps showing results of multivariate statistical analyses.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Haudebourg, Raphael; Fichet, Pascal; Goutelard, Florence
The detection (location and quantification) of nuclear facilities to be dismantled possible contamination with low-range particles emitters ({sup 3}H, other low-energy β emitters, a emitters) remains a tedious and expensive task. Indeed, usual remote counters show a too low sensitivity to these non-penetrating radiations, while conventional wipe tests are irrelevant for fixed radioactivity evaluation. The only method to accurately measure activity levels consists in sampling and running advanced laboratory analyses (spectroscopy, liquid scintillation counting, pyrolysis...). Such measurements generally induce sample preparation, waste production (destructive analyses, solvents), nuclear material transportation, long durations, and significant labor mobilization. Therefore, the search for themore » limitation of their number and cost easily conflicts with the necessity to perform a dense screening for sampling (to maximize the representativeness of the samples), in installations of thousands of square meters (floors, wells, ceilings), plus furniture, pipes, and other wastes. To overcome this contradiction, Digital Autoradiography (D. A.) was re-routed from bio molecular research to radiological mapping of nuclear installations under dismantling and to waste and sample analysis. After in-situ exposure to the possibly-contaminated areas to investigate, commercial reusable radiosensitive phosphor screens (of a few 100 cm{sup 2}) were scanned in the proper laboratory device and sharp quantitative images of the radioactivity could be obtained. The implementation of geostatistical tools in the data processing software enabled the exhaustive characterization of concrete floors at a rate of 2 weeks / 100 m{sup 2}, at lowest costs. Various samples such as drilled cores, or tank and wood pieces, were also successfully evaluated with this method, for decisive results. Thanks to the accurate location of potential contamination spots, this approach ensures relevant and representative sampling for further laboratory analyses and should be inserted in the range of common tools used in dismantling. (authors)« less
Chow, Judith C; Watson, John G; Robles, Jerome; Wang, Xiaoliang; Chen, L-W Antony; Trimble, Dana L; Kohl, Steven D; Tropp, Richard J; Fung, Kochy K
2011-12-01
Accurate, precise, and valid organic and elemental carbon (OC and EC, respectively) measurements require more effort than the routine analysis of ambient aerosol and source samples. This paper documents the quality assurance (QA) and quality control (QC) procedures that should be implemented to ensure consistency of OC and EC measurements. Prior to field sampling, the appropriate filter substrate must be selected and tested for sampling effectiveness. Unexposed filters are pre-fired to remove contaminants and acceptance tested. After sampling, filters must be stored in the laboratory in clean, labeled containers under refrigeration (<4 °C) to minimize loss of semi-volatile OC. QA activities include participation in laboratory accreditation programs, external system audits, and interlaboratory comparisons. For thermal/optical carbon analyses, periodic QC tests include calibration of the flame ionization detector with different types of carbon standards, thermogram inspection, replicate analyses, quantification of trace oxygen concentrations (<100 ppmv) in the helium atmosphere, and calibration of the sample temperature sensor. These established QA/QC procedures are applicable to aerosol sampling and analysis for carbon and other chemical components.
Powder X-ray diffraction laboratory, Reston, Virginia
Piatak, Nadine M.; Dulong, Frank T.; Jackson, John C.; Folger, Helen W.
2014-01-01
The powder x-ray diffraction (XRD) laboratory is managed jointly by the Eastern Mineral and Environmental Resources and Eastern Energy Resources Science Centers. Laboratory scientists collaborate on a wide variety of research problems involving other U.S. Geological Survey (USGS) science centers and government agencies, universities, and industry. Capabilities include identification and quantification of crystalline and amorphous phases, and crystallographic and atomic structure analysis for a wide variety of sample media. Customized laboratory procedures and analyses commonly are used to characterize non-routine samples including, but not limited to, organic and inorganic components in petroleum source rocks, ore and mine waste, clay minerals, and glassy phases. Procedures can be adapted to meet a variety of research objectives.
Magnuson, Matthew L; Satzger, R Duane; Alcaraz, Armando; Brewer, Jason; Fetterolf, Dean; Harper, Martin; Hrynchuk, Ronald; McNally, Mary F; Montgomery, Madeline; Nottingham, Eric; Peterson, James; Rickenbach, Michael; Seidel, Jimmy L; Wolnik, Karen
2012-05-01
Since the early 1990s, the FBI Laboratory has sponsored Scientific Working Groups to improve discipline practices and build consensus among the forensic community. The Scientific Working Group on the Forensic Analysis of Chemical, Biological, Radiological and Nuclear Terrorism developed guidance, contained in this document, on issues forensic laboratories encounter when accepting and analyzing unknown samples associated with chemical terrorism, including laboratory capabilities and analytical testing plans. In the context of forensic analysis of chemical terrorism, this guidance defines an unknown sample and addresses what constitutes definitive and tentative identification. Laboratory safety, reporting issues, and postreporting considerations are also discussed. Utilization of these guidelines, as part of planning for forensic analysis related to a chemical terrorism incident, may help avoid unfortunate consequences not only to the public but also to the laboratory personnel. 2011 American Academy of Forensic Sciences. Published 2011. This article is a U.S. Government work and is in the public domain in the U.S.A.
Preparations for ExoMars: Learning Lessons from Curiosity
NASA Astrophysics Data System (ADS)
Edwards, Peter Henry; Hutchinson, Ian; Morgan, Sally; McHugh, Melissa; Malherbe, Cedric; Lerman, Hannah; INGLEY, Richard
2016-10-01
In 2020, the European Space Agency will launch its first Mars rover mission, ExoMars. The rover will use a drill to obtain samples from up to 2m below the Martian surface that will then be analysed using a variety of analytical instruments, including the Raman Laser Spectrometer (RLS), which will be the first Raman spectrometer to be used on a planetary mission.To prepare for ExoMars RLS operations, we report on a series of experiments that have been performed in order to investigate the response of a representative Raman instrument to a number of analogue samples (selected based on the types of material known to be important, following investigations performed by NASA's Mars Science Laboratory, MSL, on the Curiosity rover). Raman spectroscopy will provide molecular and mineralogical information about the samples obtained from the drill cores on ExoMars. MSL acquires similar information using the CheMin XRD instrument which analyses samples acquired from drill holes several centimetres deep. Like Raman spectroscopy, XRD also provides information on the mineralogical makeup of the analysed samples.The samples in our study were selected based on CheMin data obtained from drill sites at Yellowknife Bay, one of the first locations visited by Curiosity (supplemented with additional fine scale elemental information obtained with the ChemCam LIBS laser instrument). Once selected (or produced), the samples were characterised using standard laboratory XRD and XRF instruments (in order to compare with the data obtained by CheMin) and a standard, laboratory based LIBS system (in order to compare with the ChemCam data). This characterisation provides confirmation that the analogue samples are representative of the materials likely to be encountered on Mars by the ExoMars rover.A representative, miniaturised Raman spectrometer was used to analyse the samples, using acquisition strategies and operating modes similar to those expected for the ExoMars instrument. The type of minerals detected are identified and compared to the information typically acquired using other analytical science techniques investigating in order to highlight the benefits and drawbacks of using Raman spectroscopy for planetary science applications.
NASA Astrophysics Data System (ADS)
McAdam, A.; Eigenbrode, J. L.; Young, K. E.; Bleacher, J. E.; Knudson, C. A.; Rogers, D.; Glotch, T. D.; Sutter, B.; Mahaffy, P. R.; Navarro-Gonzalez, R.; Downs, R. T.
2015-12-01
Samples of basaltic materials were collected during several traverses of the Kau Desert on the leeward side of the Kilauea Volcano, Hawaii, conducted by the Remote, In Situ, and Synchrotron Studies for Science and Exploration (RIS4E) team, a node of the Solar System Exploration and Research Virtual Institute (SSERVI) program. Some of these samples had been exposed to circumneutral to slightly acidic alteration conditions from exposure to fog/rain, and acidic fog/rain, while others had been exposed to more acidic conditions due to proximity to fumaroles. The samples consisted of basalts with coatings, sands and soils, and ash, and were collected using organically clean protocols to enable investigation of organic chemistry and organic-mineral associations, in addition to mineralogy. The Mars Science Laboratory (MSL) rover has analyzed basaltic materials inferred to have been altered under conditions ranging from circumneutral to acidic, but several aspects of the Sample Analysis at Mars (SAM) instrument suite results are still being investigated and analyses of relevant terrestrial analogs can play an important role in interpretation of the data. For example, all materials analyzed to date have a significant amorphous component. Comparisons of the mineralogy obtained with the MSL CheMin instrument and volatiles evolved during SAM analyses indicate that, by mass balance, some portion of the volatiles, such as SO2 and H2O, are likely associated with this component. Many of the RIS4E samples also have a significant amorphous component, and field x-ray diffraction (XRD) and x-ray fluorescence (XRF) data indicate differences in the chemistry of this material in samples exposed to different alteration conditions. Preliminary SAM-like analyses indicate that the amorphous materials in some of these samples evolve volatiles such as H2O and SO2 during heating. Here we will discuss these results, and others, obtained through SAM-like analyses of selected samples.
Ross, Donald S.; Bailiey, Scott W; Briggs, Russell D; Curry, Johanna; Fernandez, Ivan J.; Fredriksen, Guinevere; Goodale, Christine L.; Hazlett, Paul W.; Heine, Paul R; Johnson, Chris E.; Larson, John T; Lawrence, Gregory B.; Kolka, Randy K; Ouimet, Rock; Pare, D; Richter, Daniel D.; Shirmer, Charles D; Warby, Richard A.F.
2015-01-01
Long-term forest soil monitoring and research often requires a comparison of laboratory data generated at different times and in different laboratories. Quantifying the uncertainty associated with these analyses is necessary to assess temporal changes in soil properties. Forest soil chemical properties, and methods to measure these properties, often differ from agronomic and horticultural soils. Soil proficiency programs do not generally include forest soil samples that are highly acidic, high in extractable Al, low in extractable Ca and often high in carbon. To determine the uncertainty associated with specific analytical methods for forest soils, we collected and distributed samples from two soil horizons (Oa and Bs) to 15 laboratories in the eastern United States and Canada. Soil properties measured included total organic carbon and nitrogen, pH and exchangeable cations. Overall, results were consistent despite some differences in methodology. We calculated the median absolute deviation (MAD) for each measurement and considered the acceptable range to be the median 6 2.5 3 MAD. Variability among laboratories was usually as low as the typical variability within a laboratory. A few areas of concern include a lack of consistency in the measurement and expression of results on a dry weight basis, relatively high variability in the C/N ratio in the Bs horizon, challenges associated with determining exchangeable cations at concentrations near the lower reporting range of some laboratories and the operationally defined nature of aluminum extractability. Recommendations include a continuation of reference forest soil exchange programs to quantify the uncertainty associated with these analyses in conjunction with ongoing efforts to review and standardize laboratory methods.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Johnson, H.C.
1998-07-01
The Idaho National Engineering and Environmental Laboratory (INEEL) has several permitted treatment, storage and disposal facilities. The INEEL Sample Management Office (SMO) conducts all analysis subcontracting activities for Department of Energy Environmental Management programs at the INEEL. In this role, the INEEL SMO has had the opportunity to subcontract the analyses of various wastes (including ash from an interim status incinerator) requesting a target analyte list equivalent to the constituents listed in 40 Code of Federal Regulations. These analyses are required to ensure that treated wastes do not contain underlying hazardous constituents (UHC) at concentrations greater than the universal treatmentmore » standards (UTS) prior to land disposal. The INEEL SMO has conducted a good-faith effort by negotiating with several commercial laboratories to identify the lowest possible quantitation and detection limits that can be achieved for the organic UHC analytes. The results of this negotiating effort has been the discovery that no single laboratory (currently under subcontract with the INEEL SMO) can achieve a detection level that is within an order of magnitude of the UTS for all organic parameters on a clean sample matrix (e.g., sand). This does not mean that there is no laboratory that can achieve the order of magnitude requirements for all organic UHCs on a clean sample matrix. The negotiations held to date indicate that it is likely that no laboratory can achieve the order of magnitude requirements for a difficult sample matrix (e.g., an incinerator ash). The authors suggest that the regulation needs to be revised to address the disparity between what is achievable in the laboratory and the regulatory levels required by the UTS.« less
Fallon, Nevada FORGE Fluid Geochemistry
Blankenship, Doug; Ayling, Bridget
2018-03-13
Fluid geochemistry analysis for wells supporting the Fallon FORGE project. Samples were collected from geothermal wells using standard geothermal water sampling techniques, including filtration and acidification of the cation sample to pH < 2 prior to geochemical analysis. Analyses after 2005 were done in reputable commercial laboratories that follow standard protocols for aqueous chemistry analysis.
Conaway, Christopher; Thordsen, James J.; Manning, Michael A.; Cook, Paul J.; Trautz, Robert C.; Thomas, Burt; Kharaka, Yousif K.
2016-01-01
The chemical composition of formation water and associated gases from the lower Cretaceous Paluxy Formation was determined using four different sampling methods at a characterization well in the Citronelle Oil Field, Alabama, as part of the Southeast Regional Carbon Sequestration Partnership (SECARB) Phase III Anthropogenic Test, which is an integrated carbon capture and storage project. In this study, formation water and gas samples were obtained from well D-9-8 #2 at Citronelle using gas lift, electric submersible pump, U-tube, and a downhole vacuum sampler (VS) and subjected to both field and laboratory analyses. Field chemical analyses included electrical conductivity, dissolved sulfide concentration, alkalinity, and pH; laboratory analyses included major, minor and trace elements, dissolved carbon, volatile fatty acids, free and dissolved gas species. The formation water obtained from this well is a Na–Ca–Cl-type brine with a salinity of about 200,000 mg/L total dissolved solids. Differences were evident between sampling methodologies, particularly in pH, Fe and alkalinity. There was little gas in samples, and gas composition results were strongly influenced by sampling methods. The results of the comparison demonstrate the difficulty and importance of preserving volatile analytes in samples, with the VS and U-tube system performing most favorably in this aspect.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Streets, W.E.
As the need for rapid and more accurate determinations of gamma-emitting radionuclides in environmental and mixed waste samples grows, there is continued interest in the development of theoretical tools to eliminate the need for some laboratory analyses and to enhance the quality of information from necessary analyses. In gamma spectrometry the use of theoretical self-absorption coefficients (SACs) can eliminate the need to determine the SAC empirically by counting a known source through each sample. This empirical approach requires extra counting time and introduces another source of counting error, which must be included in the calculation of results. The empirical determinationmore » of SACs is routinely used when the nuclides of interest are specified; theoretical determination of the SAC can enhance the information for the analysis of true unknowns, where there may be no prior knowledge about radionuclides present in a sample. Determination of an exact SAC does require knowledge about the total composition of a sample. In support of the Department of Energy`s (DOE) Environmental Survey Program, the Analytical Chemistry Laboratory (ACL) at Argonne National Laboratory developed theoretical self-absorption models to estimate SACs for the determination of non-specified radionuclides in samples of unknown, widely-varying, compositions. Subsequently, another SAC model, in a different counting geometry and for specified nuclides, was developed for another application. These two models are now used routinely for the determination of gamma-emitting radionuclides in a wide variety of environmental and mixed waste samples.« less
Armbruster, David A; Overcash, David R; Reyes, Jaime
2014-01-01
The era of automation arrived with the introduction of the AutoAnalyzer using continuous flow analysis and the Robot Chemist that automated the traditional manual analytical steps. Successive generations of stand-alone analysers increased analytical speed, offered the ability to test high volumes of patient specimens, and provided large assay menus. A dichotomy developed, with a group of analysers devoted to performing routine clinical chemistry tests and another group dedicated to performing immunoassays using a variety of methodologies. Development of integrated systems greatly improved the analytical phase of clinical laboratory testing and further automation was developed for pre-analytical procedures, such as sample identification, sorting, and centrifugation, and post-analytical procedures, such as specimen storage and archiving. All phases of testing were ultimately combined in total laboratory automation (TLA) through which all modules involved are physically linked by some kind of track system, moving samples through the process from beginning-to-end. A newer and very powerful, analytical methodology is liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS). LC-MS/MS has been automated but a future automation challenge will be to incorporate LC-MS/MS into TLA configurations. Another important facet of automation is informatics, including middleware, which interfaces the analyser software to a laboratory information systems (LIS) and/or hospital information systems (HIS). This software includes control of the overall operation of a TLA configuration and combines analytical results with patient demographic information to provide additional clinically useful information. This review describes automation relevant to clinical chemistry, but it must be recognised that automation applies to other specialties in the laboratory, e.g. haematology, urinalysis, microbiology. It is a given that automation will continue to evolve in the clinical laboratory, limited only by the imagination and ingenuity of laboratory scientists. PMID:25336760
Armbruster, David A; Overcash, David R; Reyes, Jaime
2014-08-01
The era of automation arrived with the introduction of the AutoAnalyzer using continuous flow analysis and the Robot Chemist that automated the traditional manual analytical steps. Successive generations of stand-alone analysers increased analytical speed, offered the ability to test high volumes of patient specimens, and provided large assay menus. A dichotomy developed, with a group of analysers devoted to performing routine clinical chemistry tests and another group dedicated to performing immunoassays using a variety of methodologies. Development of integrated systems greatly improved the analytical phase of clinical laboratory testing and further automation was developed for pre-analytical procedures, such as sample identification, sorting, and centrifugation, and post-analytical procedures, such as specimen storage and archiving. All phases of testing were ultimately combined in total laboratory automation (TLA) through which all modules involved are physically linked by some kind of track system, moving samples through the process from beginning-to-end. A newer and very powerful, analytical methodology is liquid chromatography-mass spectrometry/mass spectrometry (LC-MS/MS). LC-MS/MS has been automated but a future automation challenge will be to incorporate LC-MS/MS into TLA configurations. Another important facet of automation is informatics, including middleware, which interfaces the analyser software to a laboratory information systems (LIS) and/or hospital information systems (HIS). This software includes control of the overall operation of a TLA configuration and combines analytical results with patient demographic information to provide additional clinically useful information. This review describes automation relevant to clinical chemistry, but it must be recognised that automation applies to other specialties in the laboratory, e.g. haematology, urinalysis, microbiology. It is a given that automation will continue to evolve in the clinical laboratory, limited only by the imagination and ingenuity of laboratory scientists.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Hu, T.A.
This is the final sample analysis report for tank 241-BX-104 (BX-104), cores 126 and 127. Two segments from each core yielded a total of 11 samples which were analyzed. The data quality objectives (DQOs) applicable to this sampling event were the Safety Screening DQO (Dukelow et al. 1995) and the Organic Safety DQO (Turner et al. 1995). The samples were received, extruded and analyzed at PNNL 325 Analytical Chemistry Laboratory (ACL). The analyses were performed in accordance with the Sample Analysis Plan (Gretsinger 1996) and indicated that the tank is safe with respect to the criteria in the Safety Screeningmore » and Organic DQO. Detailed analytical results were described in the analytical laboratory 45-day Report (Attachment 1, WHC-SD-WM-DP-171, REV. 0) and final report (Attachment 2, PNL-BX-104 REV.1) prepared by PNNL, 325 Laboratory. Corrections and/or exceptions to the PNNL final report are provided.« less
NASA Technical Reports Server (NTRS)
Stern, J. C.; Navarro-Gonzales, R.; Freissinet, C.; McKay, C. P.; Archer, P. D., Jr.; Buch, A.; Brunner, A. E.; Coll, P.; Eigenbrode, J. L.; Franz, H. B.;
2014-01-01
The Sample Analysis at Mars (SAM) instrument suite on the Mars Science Laboratory (MSL) Curiosity Rover detected both reduced and oxidized nitrogen-bearing compounds during the pyrolysis of surface materials at Yellowknife Bay in Gale Crater. Preliminary detections of nitrogen species include NO, HCN, ClCN, CH3CN, and TFMA (trifluoro-N-methyl-acetamide). Confirmation of indigenous Martian N-bearing compounds requires quantifying N contribution from the terrestrial derivatization reagents (e.g. N-methyl-N-tertbutyldimethylsilyltrifluoroacetamide, MTBSTFA and dimethylformamide, DMF) carried for SAM's wet chemistry experiment that contribute to the SAM background. Nitrogen species detected in the SAM solid sample analyses can also be produced during laboratory pyrolysis experiments where these reagents are heated in the presence of perchlorate, a compound that has also been identified by SAM in Mars solid samples.
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.
2015-10-08
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. Further results on the chemistry and other tests will be issued in the future.
The History of the AutoChemist®: From Vision to Reality.
Peterson, H E; Jungner, I
2014-05-22
This paper discusses the early history and development of a clinical analyser system in Sweden (AutoChemist, 1965). It highlights the importance of such high capacity system both for clinical use and health care screening. The device was developed to assure the quality of results and to automatically handle the orders, store the results in digital form for later statistical analyses and distribute the results to the patients' physicians by using the computer used for the analyser. The most important result of the construction of an analyser able to produce analytical results on a mass scale was the development of a mechanical multi-channel analyser for clinical laboratories that handled discrete sample technology and could prevent carry-over to the next test samples while incorporating computer technology to improve the quality of test results. The AutoChemist could handle 135 samples per hour in an 8-hour shift and up to 24 possible analyses channels resulting in 3,200 results per hour. Later versions would double this capacity. Some customers used the equipment 24 hours per day. With a capacity of 3,000 to 6,000 analyses per hour, pneumatic driven pipettes, special units for corrosive liquids or special activities, and an integrated computer, the AutoChemist system was unique and the largest of its kind for many years. Its follower - The AutoChemist PRISMA (PRogrammable Individually Selective Modular Analyzer) - was smaller in size but had a higher capacity. Both analysers established new standards of operation for clinical laboratories and encouraged others to use new technologies for building new analysers.
Imoh, Lucius C; Mutale, Mubanga; Parker, Christopher T; Erasmus, Rajiv T; Zemlin, Annalise E
2016-01-01
Timeliness of laboratory results is crucial to patient care and outcome. Monitoring turnaround times (TAT), especially for emergency tests, is important to measure the effectiveness and efficiency of laboratory services. Laboratory-based clinical audits reveal opportunities for improving quality. Our aim was to identify the most critical steps causing a high TAT for cerebrospinal fluid (CSF) chemistry analysis in our laboratory. A 6-month retrospective audit was performed. The duration of each operational phase across the laboratory work flow was examined. A process-mapping audit trail of 60 randomly selected requests with a high TAT was conducted and reasons for high TAT were tested for significance. A total of 1505 CSF chemistry requests were analysed. Transport of samples to the laboratory was primarily responsible for the high average TAT (median TAT = 170 minutes). Labelling accounted for most delays within the laboratory (median TAT = 71 minutes) with most delays occurring after regular work hours (P < 0.05). CSF chemistry requests without the appropriate number of CSF sample tubes were significantly associated with delays in movement of samples from the labelling area to the technologist's work station (caused by a preference for microbiological testing prior to CSF chemistry). A laboratory-based clinical audit identified sample transportation, work shift periods and use of inappropriate CSF sample tubes as drivers of high TAT for CSF chemistry in our laboratory. The results of this audit will be used to change pre-analytical practices in our laboratory with the aim of improving TAT and customer satisfaction.
Carson, Christine F; Inglis, Timothy JJ
2018-01-01
This study investigated aerosolized viable bacteria in a university research laboratory during operation of an acoustic-assisted flow cytometer for antimicrobial susceptibility testing by sampling room air before, during and after flow cytometer use. The aim was to assess the risk associated with use of an acoustic-assisted flow cytometer analyzing unfixed bacterial suspensions. Air sampling in a nearby clinical laboratory was conducted during the same period to provide context for the existing background of microorganisms that would be detected in the air. The three species of bacteria undergoing analysis by flow cytometer in the research laboratory were Klebsiella pneumoniae, Burkholderia thailandensis and Streptococcus pneumoniae. None of these was detected from multiple 1000 L air samples acquired in the research laboratory environment. The main cultured bacteria in both locations were skin commensal and environmental bacteria, presumed to have been disturbed or dispersed in laboratory air by personnel movements during routine laboratory activities. The concentrations of bacteria detected in research laboratory air samples were reduced after interventional cleaning measures were introduced and were lower than those in the diagnostic clinical microbiology laboratory. We conclude that our flow cytometric analyses of unfixed suspensions of K. pneumoniae, B. thailandensis and S. pneumoniae do not pose a risk to cytometer operators or other personnel in the laboratory but caution against extrapolation of our results to other bacteria and/or different flow cytometric experimental procedures. PMID:29608197
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
Determination of $sup 241$Am in soil using an automated nuclear radiation measurement laboratory
DOE Office of Scientific and Technical Information (OSTI.GOV)
Engstrom, D.E.; White, M.G.; Dunaway, P.B.
The recent completion of REECo's Automated Laboratory and associated software systems has provided a significant increase in capability while reducing manpower requirements. The system is designed to perform gamma spectrum analyses on the large numbers of samples required by the current Nevada Applied Ecology Group (NAEG) and Plutonium Distribution Inventory Program (PDIP) soil sampling programs while maintaining sufficient sensitivities as defined by earlier investigations of the same type. The hardware and systems are generally described in this paper, with emphasis being placed on spectrum reduction and the calibration procedures used for soil samples. (auth)
Intraoral Laser Welding (ILW): ultrastructural and mechanical analysis
NASA Astrophysics Data System (ADS)
Fornaini, Carlo; Passaretti, Francesca; Villa, Elena; Nammour, Samir
2010-05-01
Nd:YAG, currently used since 1970 in dental laboratories to weld metals on dental prostheses has some limits such great dimensions, high costs and fixed delivery system. Recently it was proposed the possibility to use the Nd:YAG laser device commonly utilised in dental office, to repair broken fixed, removable and orthodontic prostheses and to weld metals directly into the mouth. The aim of this work is to value, through SEM (Scanning Electron Microscope), EDS (Energy Dispersive X-Ray Spectroscopy) and DMA (Dynamic Mechanical Analysis), quality and mechanical strength of the welding process comparing a device normally used in dental lab and a device normally used in dental office for oral surgery. Sixteen CoCrMo metal plates and twenty steel orthodontic wires were divided in four groups: one was welded without metal apposition by laboratory laser, one was welded with metal apposition by laboratory laser, one was welded without metal apposition by office laser and one was welded with metal apposition by office laser. The welding process was analysed by SEM, EDS and DMA to compare the differences between the different samples. By SEM analysis it was seen that the plates welded by office laser without apposition metal showed a greater number of fissurations compared with the other samples. By EDS analysis it was seen a homogeneous composition of the metals in all the samples. The mechanical tests showed a similar elastic behaviour of the samples, with minimal differences between the two devices. No wire broke even under the maximum strength by the Analyser. This study seems to demonstrate that the welding process by office Nd:YAG laser device and the welding process by laboratory Nd:YAG laser device, analysed by SEM, EDS and DMA, showed minimal and not significant differences even if these data will be confirmed by a greater number of samples.
Kohlmann, Alexander; Kipps, Thomas J; Rassenti, Laura Z; Downing, James R; Shurtleff, Sheila A; Mills, Ken I; Gilkes, Amanda F; Hofmann, Wolf-Karsten; Basso, Giuseppe; Dell’Orto, Marta Campo; Foà, Robin; Chiaretti, Sabina; De Vos, John; Rauhut, Sonja; Papenhausen, Peter R; Hernández, Jesus M; Lumbreras, Eva; Yeoh, Allen E; Koay, Evelyn S; Li, Rachel; Liu, Wei-min; Williams, Paul M; Wieczorek, Lothar; Haferlach, Torsten
2008-01-01
Gene expression profiling has the potential to enhance current methods for the diagnosis of haematological malignancies. Here, we present data on 204 analyses from an international standardization programme that was conducted in 11 laboratories as a prephase to the Microarray Innovations in LEukemia (MILE) study. Each laboratory prepared two cell line samples, together with three replicate leukaemia patient lysates in two distinct stages: (i) a 5-d course of protocol training, and (ii) independent proficiency testing. Unsupervised, supervised, and r2 correlation analyses demonstrated that microarray analysis can be performed with remarkably high intra-laboratory reproducibility and with comparable quality and reliability. PMID:18573112
Schroder, LeRoy J.; Malo, Bernard A.; ,
1985-01-01
The purpose of the National Trends Network is to delineate the major inorganic constituents in the wet deposition in the United States. The approach chosen to monitor the Nation's wet deposition is to install approximately 150 automatic sampling devices with at least one collector in each state. Samples are collected at one week intervals, removed from collectors, and transported to an analytical laboratory for chemical analysis. The quality assurance program has divided wet deposition monitoring into 5 parts: (1) Sampling site selection, (2) sampling device, (3) sample container, (4) sample handling, and (5) laboratory analysis. Each of these five components is being examined using existing designs or new designs. Each existing or proposed sampling site is visited and a criteria audit is performed.
Wetherbee, Gregory A.; Martin, RoseAnn
2017-02-06
The U.S. Geological Survey Branch of Quality Systems operates the Precipitation Chemistry Quality Assurance Project (PCQA) for the National Atmospheric Deposition Program/National Trends Network (NADP/NTN) and National Atmospheric Deposition Program/Mercury Deposition Network (NADP/MDN). Since 1978, various programs have been implemented by the PCQA to estimate data variability and bias contributed by changing protocols, equipment, and sample submission schemes within NADP networks. These programs independently measure the field and laboratory components which contribute to the overall variability of NADP wet-deposition chemistry and precipitation depth measurements. The PCQA evaluates the quality of analyte-specific chemical analyses from the two, currently (2016) contracted NADP laboratories, Central Analytical Laboratory and Mercury Analytical Laboratory, by comparing laboratory performance among participating national and international laboratories. Sample contamination and stability are evaluated for NTN and MDN by using externally field-processed blank samples provided by the Branch of Quality Systems. A colocated sampler program evaluates the overall variability of NTN measurements and bias between dissimilar precipitation gages and sample collectors.This report documents historical PCQA operations and general procedures for each of the external quality-assurance programs from 2007 to 2016.
In-depth analyses of paleolithic pigments in cave climatic conditions
NASA Astrophysics Data System (ADS)
Touron, Stéphanie; Trichereau, Barbara; Syvilay, Delphine
2017-07-01
Painted caves are a specific environment which preservation needs multidisciplinary studies carried out within the different actors. The actions set-up must follow national and European ethics and treaties and be as less invasive as possible to preserve the integrity of the site. Studying colorants in caves should meet these expectations and take into account on-field conditions: high humidity rate, reduced access to electricity, etc. Therefore, non-invasive analyses should be preferred. However, their limits restrict the field of application and sometimes sampling and laboratory analyses must be used to answer the problematic. It is especially true when the pigment is covered by calcite. For this purpose, the Laser-Induced Breakdown Spectroscopy (LIBS) has been assessed to identify the composition with stratigraphic analyses. This study carries out in-depth profile on laboratory samples in conditions close to the ones meet in caves. Samples were prepared on a calcareous substrate using three pigments: red ochre, manganese black and carbon black and two binding media: water and saliva. All samples have been covered by calcite. Four sets of measurements have then been done using the LIBS instrument. The in-depth profiles were obtained using the Standard Normal Variate (SNV) normalization. For all the samples, the pigment layer was identified in the second or third shot, the calcite layer being quite thin. However, the results remain promising with the carbon black pigment but not really conclusive, the carbon being generally quite difficult to quantify.
Wang, Jin-Sook; Kee, Mee-Kyung; Choi, Byeong-Sun; Kim, Chan-Wha; Kim, Hyon-Suk; Kim, Sung Soon
2012-01-01
The external quality assessment schemes (EQAS) organizer provides a suitable program to monitor and improve the quality of human immunodeficiency virus (HIV) testing laboratories with EQAS panels prepared under various conditions. The aim of the current study was to investigate the effects of human plasma samples on the EQAS results of HIV obtained from hospital-based clinical laboratories. From 2007 to 2009, HIV EQAS panels consisted of four to six samples that consisted of undiluted positive and negative samples and were provided to laboratories twice per year. Up until the first half EQAS in 2008, EQAS panel materials were obtained by converting acid citrate dextrose treated plasma to serum via chemical treatment with CaCl2. Beginning with the second EQAS in 2008, all materials were prepared without the defibrination process. Approximately 300 HIV clinical laboratories participated in this program. The overall performance of clinical laboratories was shown to be improved when using unrecalcified plasma panels compared with recalcified panels. Significant differences were observed in EIA analyses of plasma for both positive (p<0.001) and negative (p<0.001) samples between the recalcified and unrecalcified groups. Our finding suggested that defibrination status of EQAS panels might affect the results of anti-HIV EQAS of Korean HIV testing laboratories.
Rodier, C; Vandenabeele-Trambouze, O; Sternberg, R; Coscia, D; Coll, P; Szopa, C; Raulin, F; Vidal-Madjar, C; Cabane, M; Israel, G; Grenier-Loustalot, M F; Dobrijevic, M; Despois, D
2001-01-01
If there is, or ever was, life in our solar system beyond the Earth, Mars is the most likely place to search for. Future space missions will have then to take into account the detection of prebiotic molecules or molecules of biological significance such as amino acids. Techniques of analysis used for returned samples have to be very sensitive and avoid any chemical or biological contamination whereas in situ techniques have to be automated, fast and low energy consuming. Several possible methods could be used for in situ amino acid analyses on Mars, but gas chromatography would likely be the most suitable. Returned samples could be analyzed by any method in routine laboratory use such as gas chromatography, already successfully performed for analyses of organic matter including amino acids from martian meteorites. The derivatization step, which volatilizes amino acids to perform both in situ and laboratory analysis by gas chromatography, is discussed here. c2001 COSPAR. Published by Elsevier Science Ltd. All rights reserved.
Harden, Stephen L.; Rogers, Shane W.; Jahne, Michael A.; Shaffer, Carrie E.; Smith, Douglas G.
2012-01-01
Study sites were sampled for laboratory analysis of nutrients, total suspended solids (TSS), and (or) fecal indicator bacteria (FIB). Nutrient analyses included measurement of dissolved ammonia, total and dissolved ammonia + organic nitrogen, dissolved nitrate + nitrite, dissolved orthophosphate, and total phosphorus. The FIB analyses included measurement of Escherichia coli and enterococci. Samples of wastewater at the swine facility were collected from a pipe outfall from the swine housing units, two storage lagoons, and the spray fields for analysis of nutrients, TSS, and FIB. Soil samples collected from a spray field were analyzed for FIB. Monitoring locations were established for collecting discharge and water-quality data during storm events at three in-field runoff sites and two sites on the headwater stream (one upstream and one downstream) next to the swine facility. Stormflow samples at the five monitoring locations were collected for four storm events during 2009 to 2010 and analyzed for nutrients, TSS, and FIB. Monthly water samples also were collected during base-flow conditions at all four stream sites for laboratory analysis of nutrients, TSS, and (or) FIB.
Dowall, Stuart D; Graham, Victoria A; Tipton, Thomas R W; Hewson, Roger
2009-08-31
Work with highly pathogenic material mandates the use of biological containment facilities, involving microbiological safety cabinets and specialist laboratory engineering structures typified by containment level 3 (CL3) and CL4 laboratories. Consequences of working in high containment are the practical difficulties associated with containing specialist assays and equipment often essential for experimental analyses. In an era of increased interest in biodefence pathogens and emerging diseases, immunological analysis has developed rapidly alongside traditional techniques in virology and molecular biology. For example, in order to maximise the use of small sample volumes, multiplexing has become a more popular and widespread approach to quantify multiple analytes simultaneously, such as cytokines and chemokines. The luminex microsphere system allows for the detection of many cytokines and chemokines in a single sample, but the detection method of using aligned lasers and fluidics means that samples often have to be analysed in low containment facilities. In order to perform cytokine analysis in materials from high containment (CL3 and CL4 laboratories), we have developed an appropriate inactivation methodology after staining steps, which although results in a reduction of median fluorescent intensity, produces statistically comparable outcomes when judged against non-inactivated samples. This methodology thus extends the use of luminex technology for material that contains highly pathogenic biological agents.
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
Melching, C.S.; Coupe, R.H.
1995-01-01
During water years 1985-91, the U.S. Geological Survey (USGS) and the Illinois Environmental Protection Agency (IEPA) cooperated in the collection and analysis of concurrent and split stream-water samples from selected sites in Illinois. Concurrent samples were collected independently by field personnel from each agency at the same time and sent to the IEPA laboratory, whereas the split samples were collected by USGS field personnel and divided into aliquots that were sent to each agency's laboratory for analysis. The water-quality data from these programs were examined by means of the Wilcoxon signed ranks test to identify statistically significant differences between results of the USGS and IEPA analyses. The data sets for constituents and properties identified by the Wilcoxon test as having significant differences were further examined by use of the paired t-test, mean relative percentage difference, and scattergrams to determine if the differences were important. Of the 63 constituents and properties in the concurrent-sample analysis, differences in only 2 (pH and ammonia) were statistically significant and large enough to concern water-quality engineers and planners. Of the 27 constituents and properties in the split-sample analysis, differences in 9 (turbidity, dissolved potassium, ammonia, total phosphorus, dissolved aluminum, dissolved barium, dissolved iron, dissolved manganese, and dissolved nickel) were statistically significant and large enough to con- cern water-quality engineers and planners. The differences in concentration between pairs of the concurrent samples were compared to the precision of the laboratory or field method used. The differences in concentration between pairs of the concurrent samples were compared to the precision of the laboratory or field method used. The differences in concentration between paris of split samples were compared to the precision of the laboratory method used and the interlaboratory precision of measuring a given concentration or property. Consideration of method precision indicated that differences between concurrent samples were insignificant for all concentrations and properties except pH, and that differences between split samples were significant for all concentrations and properties. Consideration of interlaboratory precision indicated that the differences between the split samples were not unusually large. The results for the split samples illustrate the difficulty in obtaining comparable and accurate water-quality data.
Specimen rejection in laboratory medicine: Necessary for patient safety?
Dikmen, Zeliha Gunnur; Pinar, Asli; Akbiyik, Filiz
2015-01-01
The emergency laboratory in Hacettepe University Hospitals receives specimens from emergency departments (EDs), inpatient services and intensive care units (ICUs). The samples are accepted according to the rejection criteria of the laboratory. In this study, we aimed to evaluate the sample rejection ratios according to the types of pre-preanalytical errors and collection areas. The samples sent to the emergency laboratory were recorded during 12 months between January to December, 2013 in which 453,171 samples were received and 27,067 specimens were rejected. Rejection ratios was 2.5% for biochemistry tests, 3.2% for complete blood count (CBC), 9.8% for blood gases, 9.2% for urine analysis, 13.3% for coagulation tests, 12.8% for therapeutic drug monitoring, 3.5% for cardiac markers and 12% for hormone tests. The most frequent rejection reasons were fibrin clots (28%) and inadequate volume (9%) for biochemical tests. Clotted samples (35%) and inadequate volume (13%) were the major causes for coagulation tests, blood gas analyses and CBC. The ratio of rejected specimens was higher in the EDs (40%) compared to ICUs (30%) and inpatient services (28%). The highest rejection ratio was observed in neurology ICU (14%) among the ICUs and internal medicine inpatient service (10%) within inpatient clinics. We detected an overall specimen rejection rate of 6% in emergency laboratory. By documentation of rejected samples and periodic training of healthcare personnel, we expect to decrease sample rejection ratios below 2%, improve total quality management of the emergency laboratory and promote patient safety.
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...
Laboratory analyses of micron-sized solid grains: Experimental techniques and recent results
NASA Technical Reports Server (NTRS)
Colangeli, L.; Bussoletti, E.; Blanco, A.; Borghesi, A.; Fonti, S.; Orofino, V.; Schwehm, G.
1989-01-01
Morphological and spectrophotometric investigations have been extensively applied in the past years to various kinds of micron and/or submicron-sized grains formed by materials which are candidate to be present in space. The samples are produced in the laboratory and then characterized in their physio-chemical properties. Some of the most recent results obtained on various kinds of carbonaceous materials are reported. Main attention is devoted to spectroscopic results in the VUV and IR wavelength ranges, where many of the analyzed samples show typical fingerprints which can be identified also in astrophysical and cometary materials. The laboratory methodologies used so far are also critically discussed in order to point out capabilities and present limitations, in the view of possible application to returned comet samples. Suggestions are given to develop new techniques which should overcome some of the problems faced in the manipulation and analysis of micron solid samples.
Imoh, Lucius C; Mutale, Mubanga; Parker, Christopher T; Erasmus, Rajiv T; Zemlin, Annalise E
2016-01-01
Introduction Timeliness of laboratory results is crucial to patient care and outcome. Monitoring turnaround times (TAT), especially for emergency tests, is important to measure the effectiveness and efficiency of laboratory services. Laboratory-based clinical audits reveal opportunities for improving quality. Our aim was to identify the most critical steps causing a high TAT for cerebrospinal fluid (CSF) chemistry analysis in our laboratory. Materials and methods A 6-month retrospective audit was performed. The duration of each operational phase across the laboratory work flow was examined. A process-mapping audit trail of 60 randomly selected requests with a high TAT was conducted and reasons for high TAT were tested for significance. Results A total of 1505 CSF chemistry requests were analysed. Transport of samples to the laboratory was primarily responsible for the high average TAT (median TAT = 170 minutes). Labelling accounted for most delays within the laboratory (median TAT = 71 minutes) with most delays occurring after regular work hours (P < 0.05). CSF chemistry requests without the appropriate number of CSF sample tubes were significantly associated with delays in movement of samples from the labelling area to the technologist’s work station (caused by a preference for microbiological testing prior to CSF chemistry). Conclusion A laboratory-based clinical audit identified sample transportation, work shift periods and use of inappropriate CSF sample tubes as drivers of high TAT for CSF chemistry in our laboratory. The results of this audit will be used to change pre-analytical practices in our laboratory with the aim of improving TAT and customer satisfaction. PMID:27346964
Spectroscopic and x-ray diffraction analyses of asbestos in the World Trade Center dust:
Swayze, Gregg A.; Clark, Roger N.; Sutley, Stephen J.; Hoefen, Todd M.; Plumlee, Geoffrey S.; Meeker, Gregory P.; Brownfield, Isabelle; Livo, Keith E.; Morath, Laurie C.
2009-01-01
On September 17 and 18, 2001, samples of settled dust and airfall debris were collected from 34 sites within a 1-km radius of the WTC collapse site, including a sample from an indoor location unaffected by rainfall, and samples of insulation from two steel beams at Ground Zero. Laboratory spectral and x-ray diffraction analyses of the field samples detected trace levels of serpentine minerals, including chrysotile asbestos, in about two-thirds of the dust samples at concentrations at or below ~1 wt%. One sample of a beam coating material contained up to 20 wt% chrysotile asbestos. Analyses indicate that trace levels of chrysotile were distributed with the dust radially to distances greater than 0.75 km from Ground Zero. The chrysotile content of the dust is variable and may indicate that chrysotile asbestos was not distributed uniformly during the three collapse events.
Uranium hydrogeochemical and stream sediment reconnaissance of the Solomon NTMS quadrangle, Alaska
DOE Office of Scientific and Technical Information (OSTI.GOV)
Langfeldt, S.L.; Youngquist, C.A.; D'Andrea, R.F. Jr.
This report presents results of a Hydrogeochemical and Stream Sediment Reconnaissance (HSSR) of the Solomon NTMS quadrangle, Alaska. In addition to this abbreviated data release, more complete data are available to the public in machine-readable form through the Grand Junction Office Information System at Oak Ridge National Laboratory. Presented in this data release are location data, field analyses, and laboratory analyses of several different sample media. For the sake of brevity, many field site observations have not been included in this volume. These data are, however, available on the magnetic tape. Appendices A and B describe the sample media andmore » summarize the analytical results for each medium. The data were subdivided by one of the Los Alamos National Laboratory (LANL) sorting programs of Zinkl and others into groups of stream sediment and stream water samples. For each group which contains a sufficient number of observations, statistical tables, tables of raw data, and 1:1000000 scale maps of pertinent elements have been included in this report. In addition, maps showing results of multivariate statistical analyses have been included. Further information about the HSSR program in general, or about the LANL portion of the program in particular, can be obtained in quarterly or semiannual program progress reports on open-file at DOE's Technical Library in Grand Junction. Information about the field and analytical procedures used by LANL during sample collection and analysis may be found in any HSSR data release prepared by the LANL and will not be included in this report.« less
Hardie, Diana Ruth; Korsman, Stephen N; Hsiao, Nei-Yuan; Morobadi, Molefi Daniel; Vawda, Sabeehah; Goedhals, Dominique
2017-01-01
In South Africa where the prevalence of HIV infection is very high, 4th generation HIV antibody/p24 antigen combo immunoassays are the tests of choice for laboratory based screening. Testing is usually performed in clinical pathology laboratories on automated analysers. To investigate the cause of false positive results on 4th generation HIV testing platforms in public sector laboratories, the performance of two automated platforms was compared in a clinical pathology setting, firstly on routine diagnostic specimens and secondly on known sero-negative samples. Firstly, 1181 routine diagnostic specimens were sequentially tested on Siemens and Roche automated 4th generation platforms. HIV viral load, western blot and follow up testing were used to determine the true status of inconclusive specimens. Subsequently, known HIV seronegative samples from a single donor were repeatedly tested on both platforms and an analyser was tested for surface contamination with HIV positive serum to identify how suspected specimen contamination could be occurring. Serial testing of diagnostic specimens yielded 163 weakly positive or discordant results. Only 3 of 163 were conclusively shown to indicate true HIV infection. Specimen contamination with HIV antibody was suspected, based on the following evidence: the proportion of positive specimens increased on repeated passage through the analysers; viral loads were low or undetectable and western blots negative or indeterminate on problem specimens; screen negative, 2nd test positive specimens tested positive when reanalysed on the screening assay; follow up specimens (where available) were negative. Similarly, an increasing number of known negative specimens became (repeatedly) sero-positive on serial passage through one of the analysers. Internal and external analyser surfaces were contaminated with HIV serum, evidence that sample splashes occur during testing. Due to the extreme sensitivity of these assays, contamination with minute amounts of HIV antibody can cause a negative sample to test positive. Better contamination control measures are needed on analysers used in clinical pathology environments, especially in regions where HIV sero-prevalence is high.
Stability of mercury concentration measurements in archived soil and peat samples
Navrátil, Tomáš; Burns, Douglas; Nováková, Tereza; Kaňa, Jiří; Rohovec, Jan; Roll, Michal; Ettler, Vojtěch
2018-01-01
Archived soil samples can provide important information on the history of environmental contamination and by comparison with recently collected samples, temporal trends can be inferred. Little previous work has addressed whether mercury (Hg) concentrations in soil samples are stable with long-term storage under standard laboratory conditions. In this study, we have re-analyzed using cold vapor atomic adsorption spectroscopy a set of archived soil samples that ranged from relatively pristine mountainous sites to a polluted site near a non-ferrous metal smelter with a wide range of Hg concentrations (6 - 6485 µg kg-1). Samples included organic and mineral soils and peats with a carbon content that ranged from 0.2 to 47.7%. Soil samples were stored in polyethylene bags or bottles and held in laboratory rooms where temperature was not kept to a constant value. Mercury concentrations in four subsets of samples were originally measured in 2000, 2005, 2006 and 2007, and re-analyzed in 2017, i.e. after 17, 12, 11 and 10 years of storage. Statistical analyses of either separated or lumped data yielded no significant differences between the original and current Hg concentrations. Based on these analyses, we show that archived soil and peat samples can be used to evaluate historical soil mercury contamination.
Flint, M.R.; Bencala, K.E.; Zellweger, G.W.; Hammermeister, D.P.
1985-01-01
A twenty-four hour injection of chloride and sodium was made into Leviathan Creek, Alpine County, California to aid interpretation of the coupled interactions between physical transport processes and geochemical reactions. Leviathan Creek was chosen because it receives acid mine drainage from Leviathan Mine, an abandoned open-pit sulfur mine. Water samples were collected at 15 sites along a 4.39 kilometer reach and analyzed for chloride, sodium, sulfate and fluoride. Dissolved concentrations are presented in tabular format and time-series plots. Duplicate samples were analyzed by two laboratories: the Central Laboratory, Denver, Colorado and a research laboratory in Menlo Park, California. A tabular comparison of the analyses and plots of the differences between the two laboratories is presented. Hydrographs and instantaneous discharge measurements are included. (USGS)
LABORATORY ANALYSES: WATER AND ENVIRONMENTAL SAMPLES
To be presented at the Workshop for Improving the Recognition, Investigation, and Reporting of Waterborne Disease Outbreaks Associated with Drinking, Recreational and Other Waters in Nashville, TN, May 29 - June 1, 2007
Coplen, Tyler B.
2000-01-01
The reliability and accuracy of isotopic data can be improved by utilizing database software to (i) store information about samples, (ii) store the results of mass spectrometric isotope-ratio analyses of samples, (iii) calculate analytical results using standardized algorithms stored in a database, (iv) normalize stable isotopic data to international scales using isotopic reference materials, and (v) generate multi-sheet paper templates for convenient sample loading of automated mass-spectrometer sample preparation manifolds. Such a database program, the Laboratory Information Management System (LIMS) for Light Stable Isotopes, is presented herein. Major benefits of this system include (i) a dramatic improvement in quality assurance, (ii) an increase in laboratory efficiency, (iii) a reduction in workload due to the elimination or reduction of retyping of data by laboratory personnel, and (iv) a decrease in errors in data reported to sample submitters. Such a database provides a complete record of when and how often laboratory reference materials have been analyzed and provides a record of what correction factors have been used through time. It provides an audit trail for laboratories. LIMS for Light Stable Isotopes is available for both Microsoft Office 97 Professional and Microsoft Office 2000 Professional as versions 7 and 8, respectively. Both source code (mdb file) and precompiled executable files (mde) are available. Numerous improvements have been made for continuous flow isotopic analysis in this version (specifically 7.13 for Microsoft Access 97 and 8.13 for Microsoft Access 2000). It is much easier to import isotopic results from Finnigan ISODAT worksheets, even worksheets on which corrections for amount of sample (linearity corrections) have been added. The capability to determine blank corrections using isotope mass balance from analyses of elemental analyzer samples has been added. It is now possible to calculate and apply drift corrections to isotopic data based on the time of day of analysis. Whereas Finnigan ISODAT software is confined to using only a single peak for calculating delta values, LIMS now enables one to use the mean of two or more reference injections during a continuous flow analysis to calculate delta values. This is useful with Finnigan?s GasBench II online sample preparation system. Concentrations of carbon, nitrogen, and sulfur can be calculated based one or more isotopic reference materials analyzed with a group of samples. Both sample data and isotopic analysis data can now be exported to Excel files. A calculator for determining the amount of sample needed for isotopic analysis based on a previous amount of sample and continuous flow area is now an integral part of LIMS for Light Stable Isotopes. LIMS for Light Stable Isotopes can now assign an error code to Finnigan elemental analyzer analyses in which one of the electrometers has saturated due to analysis of too much sample material, giving rise to incorrect isotopic abundances. Information on downloading this report and downloading code and databases is provided at the Internet addresses: http://water.usgs.gov/software/geochemical.html or http://www.geogr.uni-jena.de/software/geochemical.html in the Eastern Hemisphere.
[The actual possibilities of robotic microscopy in analysis automation and laboratory telemedicine].
Medovyĭ, V S; Piatnitskiĭ, A M; Sokolinskiĭ, B Z; Balugian, R Sh
2012-10-01
The article discusses the possibilities of automation microscopy complexes manufactured by Cellavision and MEKOS to perform the medical analyses of blood films and other biomaterials. The joint work of the complex and physician in the regimen of automatic load stages, screening, sampling and sorting on types with simple morphology, visual sorting of sub-sample with complex morphology provides significant increase of method sensitivity, load decrease and enhancement of physician work conditions. The information technologies, the virtual slides and laboratory telemedicine included permit to develop the representative samples of rare types and pathologies to promote automation methods and medical research targets.
Measurement of the sound absorption coefficient for an advanced undergraduate physics laboratory
NASA Astrophysics Data System (ADS)
Macho-Stadler, E.; Elejalde-García, M. J.
2017-09-01
We present a simple experiment that allows advanced undergraduates to learn the basics of the acoustic properties of materials. The impedance tube-standing wave method is applied to study the normal absorption coefficient of acoustics insulators. The setup includes a tube, a speaker, a microphone, a digital function generator and an oscilloscope, material available in an undergraduate laboratory. Results of the change of the absorption coefficient with the frequency, the sample thickness and the sample density are analysed and compared with those obtained with a commercial system.
Analysis report for 241-BY-104 Auger samples
DOE Office of Scientific and Technical Information (OSTI.GOV)
Beck, M.A.
1994-11-10
This report describes the analysis of the surface crust samples taken from single-shell tank (SST) BY-104, suspected of containing ferrocyanide wastes. This sampling and analysis will assist in ascertaining whether there is any hazard due to combustion (burning) or explosion of these solid wastes. These characteristics are important to future efforts to characterize the salt and sludge in this type of waste tank. This report will outline the methodology and detail the results of analyses performed during the characterization of this material. All analyses were performed by Westinghouse Hanford Company at the 222-S laboratory unless stated otherwise.
Anti-doping analyses at the Sochi Olympic and Paralympic Games 2014.
Sobolevsky, Tim; Krotov, Grigory; Dikunets, Marina; Nikitina, Maria; Mochalova, Elena; Rodchenkov, Grigory
2014-01-01
The laboratory anti-doping services during XXII Winter Olympic and XI Paralympic games in Sochi in 2014 were provided by a satellite laboratory facility located within the strictly secured Olympic Park. This laboratory, established and operated by the personnel of Antidoping Center, Moscow, has been authorized by the World Anti-Doping Agency (WADA) to conduct doping control analyses. The 4-floor building accommodated the most advanced analytical instrumentation and became a place of attraction for more than 50 Russian specialists and 25 foreign experts, including independent observers. In total, 2134 urine and 479 blood samples were delivered to the laboratory and analyzed during the Olympic Games (OG), and 403 urine and 108 blood samples - during the Paralympic Games (PG). The number of erythropoietin tests requested in urine was 946 and 166 at the OG and PG, respectively. Though included in the test distribution plan, a growth hormone analysis was cancelled by the Organizing Committee just before the Games. Several adverse analytical findings have been reported including pseudoephedrine (1 case), methylhexaneamine (4 cases), trimetazidine (1 case), dehydrochloromethyltestosterone (1 case), clostebol (1 case), and a designer stimulant N-ethyl-1-phenylbutan-2-amine (1 case). Copyright © 2014 John Wiley & Sons, Ltd.
In Situ Raman Analyses of Natural Gas and Gas Hydrates at Hydrate Ridge, Oregon
NASA Astrophysics Data System (ADS)
Peltzer, E. T.; White, S. N.; Dunk, R. M.; Brewer, P. G.; Sherman, A. D.; Schmidt, K.; Hester, K. C.; Sloan, E. D.
2004-12-01
During a July 2004 cruise to Hydrate Ridge, Oregon, MBARI's sea-going laser Raman spectrometer was used to obtain in situ Raman spectra of natural gas hydrates and natural gas venting from the seafloor. This was the first in situ analysis of gas hydrates on the seafloor. The hydrate spectra were compared to laboratory analyses performed at the Center for Hydrate Research, Colorado School of Mines. The natural gas spectra were compared to MBARI gas chromatography (GC) analyses of gas samples collected at the same site. DORISS (Deep Ocean Raman In Situ Spectrometer) is a laboratory model laser Raman spectrometer from Kaiser Optical Systems, Inc modified at MBARI for deployment in the deep ocean. It has been successfully deployed to depths as great as 3600 m. Different sampling optics provide flexibility in adapting the instrument to a particular target of interest. An immersion optic was used to analyze natural gas venting from the seafloor at South Hydrate Ridge ( ˜780 m depth). An open-bottomed cube was placed over the vent to collect the gas. The immersion optic penetrated the side of the cube as did a small heater used to dissociate any hydrate formed during sample collection. To analyze solid hydrates at both South and North Hydrate Ridge ( ˜590 m depth), chunks of hydrate were excavated from the seafloor and collected in a glass cylinder with a mesh top. A stand-off optic was used to analyze the hydrate inside the cylinder. Due to the partial opacity of the hydrate and the small focal volume of the sampling optic, a precision underwater positioner (PUP) was used to focus the laser spot onto the hydrate. PUP is a stand-alone system with three degrees-of-freedom, capable of moving the DORISS probe head with a precision of 0.1 mm. In situ Raman analyses of the gas indicate that it is primarily methane. This is verified by GC analyses of samples collected from the same site. Other minor constituents (such as CO2 and higher hydrocarbons) are present but may be in concentrations too low to be detected by the current DORISS instrument. In situ analyses of the hydrates show them to be structure I hydrates with methane as the primary guest molecule; the data compare well to laboratory data.
Romero-Montoya, Lydia; Martínez-Rodríguez, Hugo; Pérez, Miguel Antonio; Argüello-García, Raúl
2011-03-20
In the forensic laboratory the biological analyses for rape investigation commonly include vaginal swabs as sample material combined to biochemical tests including sperm cytology (SC) and detection of acid phosphatase activity (AP) and prostate-specific antigen (PSA, p30) for the conclusive identification of semen components. Most reports comparing these tests relied on analysis of semen samples or donor swabs taken under controlled conditions; however their individual or combined efficacy under real live sampling conditions in different laboratories is largely unknown. We carried out SC, APA and PSA analyses in vaginal swabs collected from casework rapes submitted to Mexican Forensic Laboratories at Texcoco and Toluca. On the basis of positive and negative results from each assay and sample, data were classified into eight categories (I-VIII) and compared with those obtained in the two only similar studies reported in Toronto, Canada and Hong Kong, China. SC and APA assays had the higher overall positivity in Toluca and Texcoco samples respectively and otherwise PSA had a lower but very similar positivity between these two laboratories. When compared to the previous studies some similarities were found, namely similar frequencies (at a ratio of approximately 1 out of 3) of samples being positive or negative by all techniques (Categories I and VI respectively) and a comparable overall positivity of APA and SC but higher than that of PSA. Indeed the combined results of using SC, APA and PSA tests was considered as conclusive for semen detection from approximately 1 out of 3 cases (Category I) to approximately 1 out of 2 cases in a scenario where at least SC is positive, strongly presumptive in 2 out of 3 cases (with at least one test positive) and the remainder 1 out of 3 cases (Category VI) suggested absence of semen. By determining Y-STR polymorphisms (12-loci) in additional samples obtained at Toluca laboratory, complete DNA profiles were determined from all Category I samples, none marker was detected from all Category VI samples and mostly partial profiles were obtained from samples of other categories. These observations give an overview on the variability in efficacy of each test performed at different laboratories and provide a general notion about the in praxis contribution of SC, APA and PSA tests for further DNA typing in the forensic analysis of rape. Copyright © 2010 Elsevier Ireland Ltd. All rights reserved.
[Point-of-care-testing--the intensive care laboratory].
Müller, M M; Hackl, W; Griesmacher, A
1999-01-01
After successful centralization of laboratory analyses since more than 30 years, advances in biosensors, microprocessors, measurement of undiluted whole blood and miniaturization of laboratory analyzers are leading nowadays more and more to a re-decentralization in the laboratory medicine. Point-of-care-testing (POCT), which is defined as any laboratory test performed outside central or decentralized laboratories, is becoming more and more popular. The theoretical advantages of POCT are faster turn-around-times (TAT), more rapid medical decisions, avoidance of sample identification and sample transport problems and the need of only small specimen volumes. These advantages are frequently mentioned, but are not associated with a clear clinical benefit. The disadvantages of POCT such as incorrect handling and/or maintenance of the analyzers by nontrained clinical staff, inadequate or even absent calibrations and/or quality controls, lack of cost-effectiveness because of an increased number of analyzers and more expensive reagents, insufficient documentation and difficult comparability of the obtained POCT-results with routine laboratory results, are strongly evident. According to the authors' opinion the decision for the establishing of POCT has only to be made in a close co-operation between physicians and laboratorians in order to vouch for necessity and high quality of the analyses. Taking the local situation into consideration (24-h-central laboratory, etc.) the spectrum of parameters measured by means of POCT should be rigorously restricted to the vital functions. Such analytes should be: hemoglobin or hematocrit, activated whole blood clotting time, blood gases, sodium, potassium, ionized calcium, glucose, creatinine, ammonia and lactate.
Rheology and TIC/TOC results of ORNL tank samples
DOE Office of Scientific and Technical Information (OSTI.GOV)
Pareizs, J. M.; Hansen, E. K.
2013-04-26
The Savannah River National Laboratory (SRNL)) was requested by Oak Ridge National Laboratory (ORNL) to perform total inorganic carbon (TIC), total organic carbon (TOC), and rheological measurements for several Oak Ridge tank samples. As received slurry samples were diluted and submitted to SRNL-Analytical for TIC and TOC analyses. Settled solids yield stress (also known as settled shear strength) of the as received settled sludge samples were determined using the vane method and these measurements were obtained 24 hours after the samples were allowed to settled undisturbed. Rheological or flow properties (Bingham Plastic viscosity and Bingham Plastic yield stress) were determinedmore » from flow curves of the homogenized or well mixed samples. Other targeted total suspended solids (TSS) concentrations samples were also analyzed for flow properties and these samples were obtained by diluting the as-received sample with de-ionized (DI) water.« less
A manual for a laboratory information management system (LIMS) for light stable isotopes
Coplen, Tyler B.
1997-01-01
The reliability and accuracy of isotopic data can be improved by utilizing database software to (i) store information about samples, (ii) store the results of mass spectrometric isotope-ratio analyses of samples, (iii) calculate analytical results using standardized algorithms stored in a database, (iv) normalize stable isotopic data to international scales using isotopic reference materials, and (v) generate multi-sheet paper templates for convenient sample loading of automated mass-spectrometer sample preparation manifolds. Such a database program is presented herein. Major benefits of this system include (i) an increase in laboratory efficiency, (ii) reduction in the use of paper, (iii) reduction in workload due to the elimination or reduction of retyping of data by laboratory personnel, and (iv) decreased errors in data reported to sample submitters. Such a database provides a complete record of when and how often laboratory reference materials have been analyzed and provides a record of what correction factors have been used through time. It provides an audit trail for stable isotope laboratories. Since the original publication of the manual for LIMS for Light Stable Isotopes, the isotopes 3 H, 3 He, and 14 C, and the chlorofluorocarbons (CFCs), CFC-11, CFC-12, and CFC-113, have been added to this program.
A manual for a Laboratory Information Management System (LIMS) for light stable isotopes
Coplen, Tyler B.
1998-01-01
The reliability and accuracy of isotopic data can be improved by utilizing database software to (i) store information about samples, (ii) store the results of mass spectrometric isotope-ratio analyses of samples, (iii) calculate analytical results using standardized algorithms stored in a database, (iv) normalize stable isotopic data to international scales using isotopic reference materials, and (v) generate multi-sheet paper templates for convenient sample loading of automated mass-spectrometer sample preparation manifolds. Such a database program is presented herein. Major benefits of this system include (i) an increase in laboratory efficiency, (ii) reduction in the use of paper, (iii) reduction in workload due to the elimination or reduction of retyping of data by laboratory personnel, and (iv) decreased errors in data reported to sample submitters. Such a database provides a complete record of when and how often laboratory reference materials have been analyzed and provides a record of what correction factors have been used through time. It provides an audit trail for stable isotope laboratories. Since the original publication of the manual for LIMS for Light Stable Isotopes, the isotopes 3 H, 3 He, and 14 C, and the chlorofluorocarbons (CFCs), CFC-11, CFC-12, and CFC-113, have been added to this program.
Detection of Campylobacter in human faecal samples in Fiji.
Devi, Aruna; Wilkinson, Jenny; Mahony, Timothy; Vanniasinkam, Thiru
2014-01-01
Data on campylobacteriosis in developed countries are well documented; in contrast, few studies on campylobacteriosis have been conducted in developing countries. This study was undertaken to test for Campylobacter in human faecal samples sent to the two major pathology laboratories in Fiji. A total of 408 diarrhoeal faecal samples were collected from the two major hospital pathology laboratories in Central Fiji (Suva) and Western Fiji (Lautoka) between December 2012 and February 2013 and from June to July 2013. Samples were analysed for the presence of Campylobacter using polymerase chain reaction (PCR) based methods. Campylobacter was detected in 241/408 (59.1%) of samples tested using PCR. Samples from children aged less than five accounted for 21.6% of positive cases. Campylobacter was detected in 59.1% of diarrhoeal samples collected from the two main laboratories in Fiji. A high proportion of children under five years with Campylobacter has been reported in other countries and could be due to parents being more likely to seek medical attention. Further studies are required to confirm the species of Campylobacter that are predominantly associated with gastroenteritis in Fiji.
Code of Federal Regulations, 2013 CFR
2013-01-01
... United States of America to another country in the course of trade. Laboratory. An AMS Science and..., microbiological, or physical analyses on a sample to determine presence and levels or amounts of a substance or...
Code of Federal Regulations, 2014 CFR
2014-01-01
... United States of America to another country in the course of trade. Laboratory. An AMS Science and..., microbiological, or physical analyses on a sample to determine presence and levels or amounts of a substance or...
Code of Federal Regulations, 2011 CFR
2011-01-01
... United States of America to another country in the course of trade. Laboratory. An AMS Science and..., microbiological, or physical analyses on a sample to determine presence and levels or amounts of a substance or...
Code of Federal Regulations, 2012 CFR
2012-01-01
... United States of America to another country in the course of trade. Laboratory. An AMS Science and..., microbiological, or physical analyses on a sample to determine presence and levels or amounts of a substance or...
Changes to Idaho's statewide surface-water quality monitoring program since 1995
O'Dell, Ivalou; Maret, Terry R.; Moore, Susan E.
1998-01-01
The program design included chemical analyses of water samples collected at 56 sites on the Bear, Clearwater, Kootenai, Pend Oreille, Salmon, Snake, and Spokane Rivers and their tributaries (fig. 1). Samples were collected every year (1990 through 1995) at 5 sites (annual sites), every other year at 19 sites (biennial sites), and every third year at 32 sites (triennial sites). Each year, 25 of the 56 sites were sampled. During water years 1990–95 (October 1, 1989, to September 30, 1995), samples were collected bimonthly. Onsite analyses consisted of discharge, specific conductance, pH, temperature, dissolved oxygen, bacteria (fecal coliform and fecal streptococci), and alkalinity. Laboratory analyses consisted of major ions, nutrients, trace elements, turbidity, and suspended sediment. Analytical results from the five annual sites sampled during water years 1990–93 are presented in a report by O’Dell and Berenbrock (1994).
DOE Office of Scientific and Technical Information (OSTI.GOV)
Not Available
1981-09-01
Results of a hydrogeochemical and stream sediment reconnaissance of the Philip Smith Mountains NTMS quadrangle, Alaska are presented. In addition to this abbreviated data release, more complete data are available to the public in machine-readable form. In this data release are location data, field analyses, and laboratory analyses of several different sample media. For the sake of brevity, many field site observations have not been included in this volume. These data are, however, available on the magnetic tape. Appendices A and B describe the sample media and summarize the analytical results for each medium. The data were subsetted by onemore » of the Los Alamos National Laboratory (LANL) sorting programs into groups of stream sediment and lake sediment samples. For each group which contains a sufficient number of observations, statistical tables, tables of raw data, and 1:1000000 scale maps of pertinent elements have been included in this report.« less
Analysis of graphical representation among freshmen in undergraduate physics laboratory
NASA Astrophysics Data System (ADS)
Adam, A. S.; Anggrayni, S.; Kholiq, A.; Putri, N. P.; Suprapto, N.
2018-03-01
Physics concept understanding is the importance of the physics laboratory among freshmen in the undergraduate program. These include the ability to interpret the meaning of the graph to make an appropriate conclusion. This particular study analyses the graphical representation among freshmen in an undergraduate physics laboratory. This study uses empirical study with quantitative approach. The graphical representation covers 3 physics topics: velocity of sound, simple pendulum and spring system. The result of this study shows most of the freshmen (90% of the sample) make a graph based on the data from physics laboratory. It means the transferring process of raw data which illustrated in the table to physics graph can be categorised. Most of the Freshmen use the proportional principle of the variable in graph analysis. However, Freshmen can't make the graph in an appropriate variable to gain more information and can't analyse the graph to obtain the useful information from the slope.
Optimization of analytical laboratory work using computer networking and databasing
DOE Office of Scientific and Technical Information (OSTI.GOV)
Upp, D.L.; Metcalf, R.A.
1996-06-01
The Health Physics Analysis Laboratory (HPAL) performs around 600,000 analyses for radioactive nuclides each year at Los Alamos National Laboratory (LANL). Analysis matrices vary from nasal swipes, air filters, work area swipes, liquids, to the bottoms of shoes and cat litter. HPAL uses 8 liquid scintillation counters, 8 gas proportional counters, and 9 high purity germanium detectors in 5 laboratories to perform these analyses. HPAL has developed a computer network between the labs and software to produce analysis results. The software and hardware package includes barcode sample tracking, log-in, chain of custody, analysis calculations, analysis result printing, and utility programs.more » All data are written to a database, mirrored on a central server, and eventually written to CD-ROM to provide for online historical results. This system has greatly reduced the work required to provide for analysis results as well as improving the quality of the work performed.« less
Comparison of radium-228 determination in water among Australian laboratories.
Zawadzki, Atun; Cook, Megan; Cutmore, Brodie; Evans, Fiona; Fierro, Daniela; Gedz, Alicea; Harrison, Jennifer J; Loosz, Tom; Medley, Peter; Mokhber-Shahin, Lida; Mullins, Sarah; Sdraulig, Sandra
2017-11-01
The National Health and Medical Research Council and Natural Resource Management Ministerial Council of Australia developed the current Australian Drinking Water Guidelines which recommend an annual radiation dose value of 1 mSv year -1 . One of the potential major contributors to the radiation dose from drinking water is radium-228, a naturally occurring radionuclide arising from the thorium decay series. Various methods of analysing for radium-228 in water have been established and adapted by analytical radiochemistry laboratories. Seven laboratories in Australia participated in analysing radium-228 spiked water samples with activity concentrations ranging from 6 mBq L -1 to 20 Bq L -1 . The aim of the exercise was to compare and evaluate radium-228 results reported by the participating laboratories, the methods used and the detection limits. This paper presents the outcome of the exercise. Crown Copyright © 2017. Published by Elsevier Ltd. All rights reserved.
Magnuson, Matthew; Ernst, Hiba; Griggs, John; Fitz-James, Schatzi; Mapp, Latisha; Mullins, Marissa; Nichols, Tonya; Shah, Sanjiv; Smith, Terry; Hedrick, Elizabeth
2014-11-01
Catastrophic incidents, such as natural disasters, terrorist attacks, and industrial accidents, can occur suddenly and have high impact. However, they often occur at such a low frequency and in unpredictable locations that planning for the management of the consequences of a catastrophe can be difficult. For those catastrophes that result in the release of contaminants, the ability to analyze environmental samples is critical and contributes to the resilience of affected communities. Analyses of environmental samples are needed to make appropriate decisions about the course of action to restore the area affected by the contamination. Environmental samples range from soil, water, and air to vegetation, building materials, and debris. In addition, processes used to decontaminate any of these matrices may also generate wastewater and other materials that require analyses to determine the best course for proper disposal. This paper summarizes activities and programs the United States Environmental Protection Agency (USEPA) has implemented to ensure capability and capacity for the analysis of contaminated environmental samples following catastrophic incidents. USEPA's focus has been on building capability for a wide variety of contaminant classes and on ensuring national laboratory capacity for potential surges in the numbers of samples that could quickly exhaust the resources of local communities. USEPA's efforts have been designed to ensure a strong and resilient laboratory infrastructure in the United States to support communities as they respond to contamination incidents of any magnitude. The efforts include not only addressing technical issues related to the best-available methods for chemical, biological, and radiological contaminants, but also include addressing the challenges of coordination and administration of an efficient and effective response. Laboratory networks designed for responding to large scale contamination incidents can be sustained by applying their resources during incidents of lesser significance, for special projects, and for routine surveillance and monitoring as part of ongoing activities of the environmental laboratory community. Published by Elsevier Ltd.
Stratigraphic sections of the Phosphoria formation in Utah, 1947-48
McKelvey, Vincent Ellis; Smith, L.E.; Kinney, D.M.; Huddle, J.W.; Hosford, G.F.; Sears, R.S.; Sprouse, D.P.; Steward, M.D.
1952-01-01
As part of a comprehensive investigation of the phosphate deposits of the western field begun in 1947, the U. S. Geological survey has measured an sampled the full thickness of the Permian Phosphoria formation and its partial correlative, the Park City formation, at many localities in Utah and other western states. Although these data will not be fully analyzed for several years, segments of the data, accompanied by little or no interpretation, will be published as preliminary reports. This report, which contains abstracts of many of the sections measured in northeastern Utah (pl. 1), is one of this series. The field and laboratory procedures adopted in these investigations are described rather fully in a companion report (McKelvey and others, 1952). A large number of people have taken part in this investigation. J. B. Collins, R. A. Gulbrandsen, R. A. Hoppin, J. A. Noel, F. W. O'Malley, O. A. Payne, J. F. Rominger, R. P. Sheldon, J. E. Smedley, and R. G. Waring participated in the description of strata and collection of samples referred to in this report. D. B. Dimick, H. A. Larsen, and T. K. Rigby assisted in the preparation of trenches and the crushing and splitting of samples in the field. The laboratory preparation of samples for chemical analysis was done in Denver, Colo., under the direction of W. P. Huleatt. Most of the chemical analyses reported herein were made for the Survey by the U. S. Bureau of Mines at the Northwest Electrodevelopment Laboratory, Albany, Oreg., under the direction of S. M. Shelton and M. L. Wright. All the samples from one locality (Brazer Canyon) were analyzed in the Chemical Laboratory of the Tennessee Valley Authority at Wilson Dam, Ala. Some of the Al2O3, Fe2O3, and loss-on-ignition analyses were made in the Trace Elements Section laboratory of the Survey in Washington, D. C., under the direction of J. C. Rabbitt by chemists I. Barlow, A Caemmerer, J. Greene, N. Guttag, and E. H. Humphrey. The spectrographic analyses were made by D. M. Mortimer, of the Bureau of Mines in Albany. Compilation of the data has been largely by R. P. Sheldon and F. D. Frieske under the supervision of R. W. Swanson. Organization of the tabular data has been largely by Anita Cozzetto.
Specimen rejection in laboratory medicine: Necessary for patient safety?
Dikmen, Zeliha Gunnur; Pinar, Asli; Akbiyik, Filiz
2015-01-01
Introduction The emergency laboratory in Hacettepe University Hospitals receives specimens from emergency departments (EDs), inpatient services and intensive care units (ICUs). The samples are accepted according to the rejection criteria of the laboratory. In this study, we aimed to evaluate the sample rejection ratios according to the types of pre-preanalytical errors and collection areas. Materials and methods The samples sent to the emergency laboratory were recorded during 12 months between January to December, 2013 in which 453,171 samples were received and 27,067 specimens were rejected. Results Rejection ratios was 2.5% for biochemistry tests, 3.2% for complete blood count (CBC), 9.8% for blood gases, 9.2% for urine analysis, 13.3% for coagulation tests, 12.8% for therapeutic drug monitoring, 3.5% for cardiac markers and 12% for hormone tests. The most frequent rejection reasons were fibrin clots (28%) and inadequate volume (9%) for biochemical tests. Clotted samples (35%) and inadequate volume (13%) were the major causes for coagulation tests, blood gas analyses and CBC. The ratio of rejected specimens was higher in the EDs (40%) compared to ICUs (30%) and inpatient services (28%). The highest rejection ratio was observed in neurology ICU (14%) among the ICUs and internal medicine inpatient service (10%) within inpatient clinics. Conclusions We detected an overall specimen rejection rate of 6% in emergency laboratory. By documentation of rejected samples and periodic training of healthcare personnel, we expect to decrease sample rejection ratios below 2%, improve total quality management of the emergency laboratory and promote patient safety. PMID:26527231
Maloney, T.J.; Ludtke, A.S.; Krizman, T.L.
1994-01-01
The US. Geological Survey operates a quality- assurance program based on the analyses of reference samples for the National Water Quality Laboratory in Arvada, Colorado, and the Quality of Water Service Unit in Ocala, Florida. Reference samples containing selected inorganic, nutrient, and low ionic-strength constituents are prepared and disguised as routine samples. The program goal is to determine precision and bias for as many analytical methods offered by the participating laboratories as possible. The samples typically are submitted at a rate of approximately 5 percent of the annual environmental sample load for each constituent. The samples are distributed to the laboratories throughout the year. Analytical data for these reference samples reflect the quality of environmental sample data produced by the laboratories because the samples are processed in the same manner for all steps from sample login through data release. The results are stored permanently in the National Water Data Storage and Retrieval System. During water year 1991, 86 analytical procedures were evaluated at the National Water Quality Laboratory and 37 analytical procedures were evaluated at the Quality of Water Service Unit. An overall evaluation of the inorganic (major ion and trace metal) constituent data for water year 1991 indicated analytical imprecision in the National Water Quality Laboratory for 5 of 67 analytical procedures: aluminum (whole-water recoverable, atomic emission spectrometric, direct-current plasma); calcium (atomic emission spectrometric, direct); fluoride (ion-exchange chromatographic); iron (whole-water recoverable, atomic absorption spectrometric, direct); and sulfate (ion-exchange chromatographic). The results for 11 of 67 analytical procedures had positive or negative bias during water year 1991. Analytical imprecision was indicated in the determination of two of the five National Water Quality Laboratory nutrient constituents: orthophosphate as phosphorus and phosphorus. A negative or positive bias condition was indicated in three of five nutrient constituents. There was acceptable precision and no indication of bias for the 14 low ionic-strength analytical procedures tested in the National Water Quality Laboratory program and for the 32 inorganic and 5 nutrient analytical procedures tested in the Quality of Water Service Unit during water year 1991.
Herbicide Orange Site Characterization Study Naval Construction Battalion Center
1987-01-01
U.S. Testing Laboratories for analysis. Over 200 additional analyses were performed for a variety of quality assurance criteria. The resultant data...TABLE 9. NCBC PERFORMANCE AUDIT SAMPLE ANALYSIS SUNMARYa (SERIES 1) TCDD Sppb ) Reported Detection Relative b Sample Number Concentration Limit...limit rather than estimating the variance of the results. The sample results were transformed using the natural logarithm. The Shapiro-Wilk W test
Consideration of sample return and the exploration strategy for Mars
NASA Technical Reports Server (NTRS)
Bogard, D. C.; Duke, M. B.; Gibson, E. K.; Minear, J. W.; Nyquist, L. E.; Phinney, W. C.
1979-01-01
The scientific rationale and requirements for a Mars surface sample return were examined and the experience gained from the analysis and study of the returned lunar samples were incorporated into the science requirements and engineering design for the Mars sample return mission. The necessary data sets for characterizing Mars are presented. If further analyses of surface samples are to be made, the best available method is for the analysis to be conducted in terrestrial laboratories.
2018-01-01
This work presents the results of an international interlaboratory comparison on ex situ passive sampling in sediments. The main objectives were to map the state of the science in passively sampling sediments, identify sources of variability, provide recommendations and practical guidance for standardized passive sampling, and advance the use of passive sampling in regulatory decision making by increasing confidence in the use of the technique. The study was performed by a consortium of 11 laboratories and included experiments with 14 passive sampling formats on 3 sediments for 25 target chemicals (PAHs and PCBs). The resulting overall interlaboratory variability was large (a factor of ∼10), but standardization of methods halved this variability. The remaining variability was primarily due to factors not related to passive sampling itself, i.e., sediment heterogeneity and analytical chemistry. Excluding the latter source of variability, by performing all analyses in one laboratory, showed that passive sampling results can have a high precision and a very low intermethod variability (
Results of the Excreta Bioassay Quality Control Program for April 1, 2009 through March 31, 2010
DOE Office of Scientific and Technical Information (OSTI.GOV)
Antonio, Cheryl L.
2012-07-19
A total of 58 urine samples and 10 fecal samples were submitted during the report period (April 1, 2009 through March 31, 2010) to General Engineering Laboratories, South Carolina by the Hanford Internal Dosimetry Program (IDP) to check the accuracy, precision, and detection levels of their analyses. Urine analyses for Sr, 238Pu, 239Pu, 241Am, 243Am 235U, 238U, elemental uranium and fecal analyses for 241Am, 238Pu and 239Pu were tested this year as well as four tissue samples for 238Pu, 239Pu, 241Am and 241Pu. The number of QC urine samples submitted during the report period represented 1.3% of the total samplesmore » submitted. In addition to the samples provided by IDP, GEL was also required to conduct their own QC program, and submit the results of analyses to IDP. About 33% of the analyses processed by GEL during the third year of this contract were quality control samples. GEL tested the performance of 21 radioisotopes, all of which met or exceeded the specifications in the Statement of Work within statistical uncertainty (Table 4).« less
Results of The Excreta Bioassay Quality Control Program For April 1, 2010 Through March 31, 2011
DOE Office of Scientific and Technical Information (OSTI.GOV)
Antonio, Cheryl L.
2012-07-19
A total of 76 urine samples and 10 spiked fecal samples were submitted during the report period (April 1, 2010 through March 31, 2011) to GEL Laboratories, LLC in South Carolina by the Hanford Internal Dosimetry Program (IDP) to check the accuracy, precision, and detection levels of their analyses. Urine analyses for 14C, Sr, for 238Pu, 239Pu, 241Am, 243Am, 235U, 238U, 238U-mass and fecal analyses for 241Am, 238Pu and 239Pu were tested this year. The number of QC urine samples submitted during the report period represented 1.1% of the total samples submitted. In addition to the samples provided by IDP,more » GEL was also required to conduct their own QC program, and submit the results of analyses to IDP. About 31% of the analyses processed by GEL during the first year of contract 112512 were quality control samples. GEL tested the performance of 23 radioisotopes, all of which met or exceeded the specifications in the Statement of Work within statistical uncertainty except the slightly elevated relative bias for 243,244Cm (Table 4).« less
Automation of a Large Analytical Chemistry Laboratory
1990-12-01
Division Brooks Air Force Base , Texas 78235-5501 NOTICES When Government drawings, specifications, or other data are used for any purpose other than a...been reviewed and is approved for publication. Air Force installations may direct requests for copies of this report to: Air Force Occupational and...remaining for the analyses. Our laboratory serves worldwide Air Force installations and therefore comes up against these sample holding time requirements
Tank 241-U-103, grab samples 3U-99-1, 3u-99-2 and 3U-99-3
DOE Office of Scientific and Technical Information (OSTI.GOV)
STEEN, F.H.
This document is the final report for tank 241-U-103 grab samples. Three grab samples were collected from riser 13 on March 12, 1999 and received by the 222-S laboratory on March 15, 1999. Analyses were performed in accordance with the Compatibility Grab Sampling and Analysis Plan for Fiscal year 1999 (TSAP) and the Data Quality Objectives for Tank Farms Waste Compatibility Program (DQO). The analytical results are presented in the data summary report. None of the subsamples submitted for differential scanning calorimetry (DSC), total organic carbon (TOC) and plutonium 239 (Pu239) analyses exceeded the notification limits as stated in TSAP.
Alves, Cíntia; Pereira, Rui; Prieto, Lourdes; Aler, Mercedes; Amaral, Cesar R L; Arévalo, Cristina; Berardi, Gabriela; Di Rocco, Florencia; Caputo, Mariela; Carmona, Cristian Hernandez; Catelli, Laura; Costa, Heloísa Afonso; Coufalova, Pavla; Furfuro, Sandra; García, Óscar; Gaviria, Anibal; Goios, Ana; Gómez, Juan José Builes; Hernández, Alexis; Hernández, Eva Del Carmen Betancor; Miranda, Luís; Parra, David; Pedrosa, Susana; Porto, Maria João Anjos; Rebelo, Maria de Lurdes; Spirito, Matteo; Torres, María Del Carmen Villalobos; Amorim, António; Pereira, Filipe
2017-05-01
DNA is a powerful tool available for forensic investigations requiring identification of species. However, it is necessary to develop and validate methods able to produce results in degraded and or low quality DNA samples with the high standards obligatory in forensic research. Here, we describe a voluntary collaborative exercise to test the recently developed Species Identification by Insertions/Deletions (SPInDel) method. The SPInDel kit allows the identification of species by the generation of numeric profiles combining the lengths of six mitochondrial ribosomal RNA (rRNA) gene regions amplified in a single reaction followed by capillary electrophoresis. The exercise was organized during 2014 by a Working Commission of the Spanish and Portuguese-Speaking Working Group of the International Society for Forensic Genetics (GHEP-ISFG), created in 2013. The 24 participating laboratories from 10 countries were asked to identify the species in 11 DNA samples from previous GHEP-ISFG proficiency tests using a SPInDel primer mix and control samples of the 10 target species. A computer software was also provided to the participants to assist the analyses of the results. All samples were correctly identified by 22 of the 24 laboratories, including samples with low amounts of DNA (hair shafts) and mixtures of saliva and blood. Correct species identifications were obtained in 238 of the 241 (98.8%) reported SPInDel profiles. Two laboratories were responsible for the three cases of misclassifications. The SPInDel was efficient in the identification of species in mixtures considering that only a single laboratory failed to detect a mixture in one sample. This result suggests that SPInDel is a valid method for mixture analyses without the need for DNA sequencing, with the advantage of identifying more than one species in a single reaction. The low frequency of wrong (5.0%) and missing (2.1%) alleles did not interfere with the correct species identification, which demonstrated the advantage of using a method based on the analysis of multiple loci. Overall, the SPInDel method was easily implemented by laboratories using different genotyping platforms, the interpretation of results was straightforward and the SPInDel software was used without any problems. The results of this collaborative exercise indicate that the SPInDel method can be applied successfully in forensic casework investigations. Copyright © 2017 Elsevier B.V. All rights reserved.
Hullstein, Ingunn R; Malerod-Fjeld, Helle; Dehnes, Yvette; Hemmersbach, Peter
2015-01-01
Doping agents are widely and illicitly distributed through the Internet. Analysis of these preparations is useful in order to monitor the availability of prohibited substances on the market, and more importantly to predict which substances are expected to be found in urine samples collected from athletes and to aid clinical and forensic investigations. Based on a close collaboration with the Norwegian police and the Norwegian custom authorities, the Norwegian Doping Control Laboratory has performed analyses of confiscated material suspected of containing doping agents. The analyses were performed using gas chromatography (GC) and liquid chromatography (LC) combined with mass spectrometry (MS). The majority (67%) of the analyzed black market products contained anabolic- androgenic steroids (AAS) as expected, whereas peptide- and protein-based doping substances were identified in 28% of the preparations. The Norwegian Doping Control Laboratory receives samples collected from recreational and elite athletes in addition to samples collected in clinical and forensic investigations. The findings in the seized material reflected the findings in the urine samples analyzed regarding the anabolic steroids. Thus, analyzing material seized in Norway may give a good indication of doping agents available on the local market. Copyright © 2015 John Wiley & Sons, Ltd.
Lociciro, S; Esseiva, P; Hayoz, P; Dujourdy, L; Besacier, F; Margot, P
2008-05-20
Harmonisation and optimization of analytical and statistical methodologies were carried out between two forensic laboratories (Lausanne, Switzerland and Lyon, France) in order to provide drug intelligence for cross-border cocaine seizures. Part I dealt with the optimization of the analytical method and its robustness. This second part investigates statistical methodologies that will provide reliable comparison of cocaine seizures analysed on two different gas chromatographs interfaced with a flame ionisation detectors (GC-FIDs) in two distinct laboratories. Sixty-six statistical combinations (ten data pre-treatments followed by six different distance measurements and correlation coefficients) were applied. One pre-treatment (N+S: area of each peak is divided by its standard deviation calculated from the whole data set) followed by the Cosine or Pearson correlation coefficients were found to be the best statistical compromise for optimal discrimination of linked and non-linked samples. The centralisation of the analyses in one single laboratory is not a required condition anymore to compare samples seized in different countries. This allows collaboration, but also, jurisdictional control over data.
Abdel Massih, M; Planchon, V; Polet, M; Dierick, K; Mahillon, J
2016-02-01
Based on the results of 19 food microbiology proficiency testing (PT) schemes, this study aimed to assess the laboratory performances, to highlight the main sources of unsatisfactory analytical results and to suggest areas of improvement. The 2009-2015 results of REQUASUD and IPH PT, involving a total of 48 laboratories, were analysed. On average, the laboratories failed to detect or enumerate foodborne pathogens in 3·0% of the tests. Thanks to a close collaboration with the PT participants, the causes of outliers could be identified in 74% of the cases. The main causes of erroneous PT results were either pre-analytical (handling of the samples, timing of analysis), analytical (unsuitable methods, confusion of samples, errors in colony counting or confirmation) or postanalytical mistakes (calculation and encoding of results). PT schemes are a privileged observation post to highlight analytical problems, which would otherwise remain unnoticed. In this perspective, this comprehensive study of PT results provides insight into the sources of systematic errors encountered during the analyses. This study draws the attention of the laboratories to the main causes of analytical errors and suggests practical solutions to avoid them, in an educational purpose. The observations support the hypothesis that regular participation to PT, when followed by feed-back and appropriate corrective actions, can play a key role in quality improvement and provide more confidence in the laboratory testing results. © 2015 The Society for Applied Microbiology.
Tormey, William P; O'Hagan, Christopher
2015-01-01
Cerebrospinal fluid (CSF) protein and glucose examinations are usually performed in chemical pathology departments on autoanalysers. Tuberculosis (TB) is a group 3 biological agent under Directive 2000/54/EC of the European Parliament but in the biochemistry laboratory, no extra precautions are taken in its analysis in possible TB cases. The issue of laboratory practice and safety in the biochemical analyses of CSF specimens, when tuberculosis infection is in question is addressed in the context of ambiguity in the implementation of current national and international health and safety regulations. Additional protective measures for laboratory staff during the analysis of CSF TB samples should force a change in current laboratory practice and become a regulatory issue under ISO 15189. Annual Mantoux skin test or an interferon-γ release assay for TB should be mandatory for relevant staff. This manuscript addresses the issue of biochemistry laboratory practice and safety in the biochemical analyses of CSF specimens when tuberculosis infection is in question in the context of the ambiguity of statutory health and safety regulations.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Nichols, T.
The Nuclear Forensics Analysis Center (NFAC) is part of Savannah River National Laboratory (SRNL) and is one of only two USG National Laboratories accredited to perform nuclear forensic analyses to the requirements of ISO 17025. SRNL NFAC is capable of analyzing nuclear and radiological samples from bulk material to ultra-trace samples. NFAC provides analytical support to the FBI's Radiological Evidence Examination Facility (REEF), which is located within SRNL. REEF gives the FBI the capability to perform traditional forensics on material that is radiological and/or is contaminated. SRNL is engaged in research and development efforts to improve the USG technical nuclearmore » forensics capabilities. Research includes improving predictive signatures and developing a database containing comparative samples.« less
DOE-OES-EML quality assurance program
DOE Office of Scientific and Technical Information (OSTI.GOV)
Sanderson, C.G.
1980-01-01
Contractor laboratories handling radioactive materials for the US Department of Energy (DOE) are required to monitor the environmental exposure and publish annual reports for the Division of Operational and Environmental Safety (OES). In order to determine the validity of the data contained in these reports the Environmental Measurements Laboratory (EML) was requested to develop, coordinate, and conduct an Environmental Quality Assurance Program (QAP). There are four major phases to the DOE-OES-EML Quality Assurance Program: sample collection and preparation, sample analyses at EML, quarterly sample distribution, and reporting the data returned by the participants. The various phases of the QAP andmore » the data reported during the first year of the program are discussed.« less
[Comparability study of analytical results between a group of clinical laboratories].
Alsius-Serra, A; Ballbé-Anglada, M; López-Yeste, M L; Buxeda-Figuerola, M; Guillén-Campuzano, E; Juan-Pereira, L; Colomé-Mallolas, C; Caballé-Martín, I
2015-01-01
To describe the study of the comparability of the measurements levels of biological tests processed in biochemistry in Catlab's 4 laboratories. Quality requirements, coefficients of variation and total error (CV% and TE %) were established. Controls were verified with the precision requirements (CV%) in each test and each individual laboratory analyser. Fresh serum samples were used for the comparability study. The differences were analysed using a Microsoft Access® application that produces modified Bland-Altman plots. The comparison of 32 biological parameters that are performed in more than one laboratory and/or analyser generated 306 Bland-Altman graphs. Of these, 101 (33.1%) fell within the accepted range of values based on biological variability, and 205 (66.9%) required revision. Data were re-analysed based on consensus minimum specifications for analytical quality (consensus of the Asociación Española de Farmacéuticos Analistas (AEFA), the Sociedad Española de Bioquímica Clínica y Patología Molecular (SEQC), the Asociación Española de Biopatología Médica (AEBM) and the Sociedad Española de Hematología y Hemoterapia (SEHH), October 2013). With the new specifications, 170 comparisons (56%) fitted the requirements and 136 (44%) required additional review. Taking into account the number of points that exceeded the requirement, random errors, range of results in which discrepancies were detected, and range of clinical decision, it was shown that the 44% that required review were acceptable, and the 32 tests were comparable in all laboratories and analysers. The analysis of the results showed that the consensus requirements of the 4 scientific societies were met. However, each laboratory should aim to meet stricter criteria for total error. Copyright © 2015 SECA. Published by Elsevier Espana. All rights reserved.
Witt, E. C.; Hippe, D.J.; Giovannitti, R.M.
1992-01-01
A total of 304 nutrient samples were collected from May 1990 through September 1991 to determine concentrations and loads of nutrients in water discharged from two spring basins in Cumberland County, Pa. Fifty-four percent of these nutrient samples were for the evaluation of (1) laboratory consistency, (2) container and preservative cleanliness, (3) maintenance of analyte representativeness as affected by three different preservation methods, and (4) comparison of analyte results with the "Most Probable Value" for Standard Reference Water Samples. Results of 37 duplicate analyses indicate that the Pennsylvania Department of Environmental Resources, Bureau of Laboratories (principal laboratory) remained within its ±10 percent goal for all but one analyte. Results of the blank analysis show that the sampling containers did not compromise the water quality. However, mercuric-chloride-preservation blanks apparently contained measurable ammonium in four of five samples and ammonium plus organic nitrogen in two of five samples. Interlaboratory results indicate substantial differences in the determination of nitrate and ammonium plus organic nitrogen between the principal laboratory and the U.S. Geological Survey National Water-Quality Laboratory. In comparison with the U.S. Environmental Protection Agency Quality-Control Samples, the principal laboratory was sufficiently accurate in its determination of nutrient anafytes. Analysis of replicate samples indicated that sulfuric-acid preservative best maintained the representativeness of the anafytes nitrate and ammonium plus organic nitrogen, whereas, mercuric chloride best maintained the representativeness of orthophosphate. Comparison of nutrient analyte determinations with the Most Probable Value for each preservation method shows that two of five analytes with no chemical preservative compare well, three of five with mercuric-chloride preservative compare well, and three of five with sulfuricacid preservative compare well.
Evaluation of the Technicon Axon analyser.
Martínez, C; Márquez, M; Cortés, M; Mercé, J; Rodriguez, J; González, F
1990-01-01
An evaluation of the Technicon Axon analyser was carried out following the guidelines of the 'Sociedad Española de Química Clínica' and the European Committee for Clinical Laboratory Standards.A photometric study revealed acceptable results at both 340 nm and 404 nm. Inaccuracy and imprecision were lower at 404 nm than at 340 nm, although poor dispersion was found at both wavelengths, even at low absorbances. Drift was negligible, the imprecision of the sample pipette delivery system was greater for small sample volumes, the reagent pipette delivery system imprecision was acceptable and the sample diluting system study showed good precision and accuracy.Twelve analytes were studied for evaluation of the analyser under routine working conditions. Satisfactory results were obtained for within-run imprecision, while coefficients of variation for betweenrun imprecision were much greater than expected. Neither specimenrelated nor specimen-independent contamination was found in the carry-over study. For all analytes assayed, when comparing patient sample results with those obtained in a Hitachi 737 analyser, acceptable relative inaccuracy was observed.
Core vs. Bulk Samples in Soil-Moisture Tension Analyses
Walter M. Broadfoot
1954-01-01
The usual laboratory procedure in determining soil-moisture tension values is to use "undisturbed" soil cores for tensions up to 60 cm. of water and bulk soil samples for higher tensions. Low tensions are usually obtained with a tension table and the higher tensions by use of pressure plate apparatus. In tension analysis at the Vicksburg Infiltration Project...
New technologies are creating the potential for using nucleic acid sequence detection to perform routine microbiological analyses of environmental samples. Our laboratory has recently reported on the development of a method for the quantitative detection of Stachybotrys chartarum...
Glass-Kaastra, Shiona K.; Pearl, David L.; Reid-Smith, Richard J.; McEwen, Beverly; Slavic, Durda; McEwen, Scott A.; Fairles, Jim
2014-01-01
Antimicrobial susceptibility data on Escherichia coli F4, Pasteurella multocida, and Streptococcus suis isolates from Ontario swine (January 1998 to October 2010) were acquired from a comprehensive diagnostic veterinary laboratory in Ontario, Canada. In relation to the possible development of a surveillance system for antimicrobial resistance, data were assessed for ease of management, completeness, consistency, and applicability for temporal and spatial statistical analyses. Limited farm location data precluded spatial analyses and missing demographic data limited their use as predictors within multivariable statistical models. Changes in the standard panel of antimicrobials used for susceptibility testing reduced the number of antimicrobials available for temporal analyses. Data consistency and quality could improve over time in this and similar diagnostic laboratory settings by encouraging complete reporting with sample submission and by modifying database systems to limit free-text data entry. These changes could make more statistical methods available for disease surveillance and cluster detection. PMID:24688133
Glass-Kaastra, Shiona K; Pearl, David L; Reid-Smith, Richard J; McEwen, Beverly; Slavic, Durda; McEwen, Scott A; Fairles, Jim
2014-04-01
Antimicrobial susceptibility data on Escherichia coli F4, Pasteurella multocida, and Streptococcus suis isolates from Ontario swine (January 1998 to October 2010) were acquired from a comprehensive diagnostic veterinary laboratory in Ontario, Canada. In relation to the possible development of a surveillance system for antimicrobial resistance, data were assessed for ease of management, completeness, consistency, and applicability for temporal and spatial statistical analyses. Limited farm location data precluded spatial analyses and missing demographic data limited their use as predictors within multivariable statistical models. Changes in the standard panel of antimicrobials used for susceptibility testing reduced the number of antimicrobials available for temporal analyses. Data consistency and quality could improve over time in this and similar diagnostic laboratory settings by encouraging complete reporting with sample submission and by modifying database systems to limit free-text data entry. These changes could make more statistical methods available for disease surveillance and cluster detection.
Bogun, Ben; Moore, Sarah
2017-09-01
In this study, the use of benchtop NMR spectroscopy in the analysis of solids and liquids used and/or produced during the HI reduction of pseudoephedrine was evaluated. The study focused on identifying organic precursors and phosphorus containing compounds used in and/or produced during the manufacturing process. Samples taken from clandestine laboratories, where this synthesis process was suspected of occurring, were also analysed and evaluated. Benchtop NMR was able to distinguish between ephedrine, pseudoephedrine and methamphetamine as the free base and hydrochloride salt. This technique was also effective at identifying and distinguishing between phosphorus containing compounds used and/or produced during the manufacture of methamphetamine. Benchtop NMR was also determined to be effective at analysing samples from suspected clandestine laboratories. Copyright © 2017 Elsevier B.V. All rights reserved.
Steigen, Terje K; Claudio, Cheryl; Abbott, David; Schulzer, Michael; Burton, Jeff; Tymchak, Wayne; Buller, Christopher E; John Mancini, G B
2008-06-01
To assess reproducibility of core laboratory performance and impact on sample size calculations. Little information exists about overall reproducibility of core laboratories in contradistinction to performance of individual technicians. Also, qualitative parameters are being adjudicated increasingly as either primary or secondary end-points. The comparative impact of using diverse indexes on sample sizes has not been previously reported. We compared initial and repeat assessments of five quantitative parameters [e.g., minimum lumen diameter (MLD), ejection fraction (EF), etc.] and six qualitative parameters [e.g., TIMI myocardial perfusion grade (TMPG) or thrombus grade (TTG), etc.], as performed by differing technicians and separated by a year or more. Sample sizes were calculated from these results. TMPG and TTG were also adjudicated by a second core laboratory. MLD and EF were the most reproducible, yielding the smallest sample size calculations, whereas percent diameter stenosis and centerline wall motion require substantially larger trials. Of the qualitative parameters, all except TIMI flow grade gave reproducibility characteristics yielding sample sizes of many 100's of patients. Reproducibility of TMPG and TTG was only moderately good both within and between core laboratories, underscoring an intrinsic difficulty in assessing these. Core laboratories can be shown to provide reproducibility performance that is comparable to performance commonly ascribed to individual technicians. The differences in reproducibility yield huge differences in sample size when comparing quantitative and qualitative parameters. TMPG and TTG are intrinsically difficult to assess and conclusions based on these parameters should arise only from very large trials.
Stacey, Peter; Butler, Owen
2008-06-01
This paper emphasizes the need for occupational hygiene professionals to require evidence of the quality of welding fume data from analytical laboratories. The measurement of metals in welding fume using atomic spectrometric techniques is a complex analysis often requiring specialist digestion procedures. The results from a trial programme testing the proficiency of laboratories in the Workplace Analysis Scheme for Proficiency (WASP) to measure potentially harmful metals in several different types of welding fume showed that most laboratories underestimated the mass of analyte on the filters. The average recovery was 70-80% of the target value and >20% of reported recoveries for some of the more difficult welding fume matrices were <50%. This level of under-reporting has significant implications for any health or hygiene studies of the exposure of welders to toxic metals for the types of fumes included in this study. Good laboratories' performance measuring spiked WASP filter samples containing soluble metal salts did not guarantee good performance when measuring the more complex welding fume trial filter samples. Consistent rather than erratic error predominated, suggesting that the main analytical factor contributing to the differences between the target values and results was the effectiveness of the sample preparation procedures used by participating laboratories. It is concluded that, with practice and regular participation in WASP, performance can improve over time.
Contaminant Attenuation and Transport Characterization of 200-DV-1 Operable Unit Sediment Samples
DOE Office of Scientific and Technical Information (OSTI.GOV)
Truex, Michael J.; Szecsody, James E.; Qafoku, Nikolla
2017-05-15
A laboratory study was conducted to quantify contaminant attenuation processes and associated contaminant transport parameters that are needed to evaluate transport of contaminants through the vadose zone to the groundwater. The laboratory study information, in conjunction with transport analyses, can be used as input to evaluate the feasibility of Monitored Natural Attenuation and other remedies for the 200-DV-1 Operable Unit at the Hanford Site.
Analytical methods of the U.S. Geological Survey's New York District Water-Analysis Laboratory
Lawrence, Gregory B.; Lincoln, Tricia A.; Horan-Ross, Debra A.; Olson, Mark L.; Waldron, Laura A.
1995-01-01
The New York District of the U.S. Geological Survey (USGS) in Troy, N.Y., operates a water-analysis laboratory for USGS watershed-research projects in the Northeast that require analyses of precipitation and of dilute surface water and soil water for major ions; it also provides analyses of certain chemical constituents in soils and soil gas samples.This report presents the methods for chemical analyses of water samples, soil-water samples, and soil-gas samples collected in wateshed-research projects. The introduction describes the general materials and technicques for each method and explains the USGS quality-assurance program and data-management procedures; it also explains the use of cross reference to the three most commonly used methods manuals for analysis of dilute waters. The body of the report describes the analytical procedures for (1) solution analysis, (2) soil analysis, and (3) soil-gas analysis. The methods are presented in alphabetical order by constituent. The method for each constituent is preceded by (1) reference codes for pertinent sections of the three manuals mentioned above, (2) a list of the method's applications, and (3) a summary of the procedure. The methods section for each constitutent contains the following categories: instrumentation and equipment, sample preservation and storage, reagents and standards, analytical procedures, quality control, maintenance, interferences, safety considerations, and references. Sufficient information is presented for each method to allow the resulting data to be appropriately used in environmental investigations.
Tank 241-AP-105, cores 208, 209 and 210, analytical results for the final report
DOE Office of Scientific and Technical Information (OSTI.GOV)
Nuzum, J.L.
1997-10-24
This document is the final laboratory report for Tank 241-AP-105. Push mode core segments were removed from Risers 24 and 28 between July 2, 1997, and July 14, 1997. Segments were received and extruded at 222-S Laboratory. Analyses were performed in accordance with Tank 241-AP-105 Push Mode Core Sampling and Analysis Plan (TSAP) (Hu, 1997) and Tank Safety Screening Data Quality Objective (DQO) (Dukelow, et al., 1995). None of the subsamples submitted for total alpha activity (AT), differential scanning calorimetry (DSC) analysis, or total organic carbon (TOC) analysis exceeded the notification limits as stated in TSAP and DQO. The statisticalmore » results of the 95% confidence interval on the mean calculations are provided by the Tank Waste Remediation Systems Technical Basis Group, and are not considered in this report. Appearance and Sample Handling Two cores, each consisting of four segments, were expected from Tank 241-AP-105. Three cores were sampled, and complete cores were not obtained. TSAP states core samples should be transported to the laboratory within three calendar days from the time each segment is removed from the tank. This requirement was not met for all cores. Attachment 1 illustrates subsamples generated in the laboratory for analysis and identifies their sources. This reference also relates tank farm identification numbers to their corresponding 222-S Laboratory sample numbers.« less
Hanford analytical sample projections FY 1998--FY 2002
DOE Office of Scientific and Technical Information (OSTI.GOV)
Joyce, S.M.
1998-02-12
Analytical Services projections are compiled for the Hanford site based on inputs from the major programs for the years 1998 through 2002. Projections are categorized by radiation level, protocol, sample matrix and program. Analyses requirements are also presented. This document summarizes the Hanford sample projections for fiscal years 1998 to 2002. Sample projections are based on inputs submitted to Analytical Services covering Environmental Restoration, Tank Waste Remediation Systems (TWRS), Solid Waste, Liquid Effluents, Spent Nuclear Fuels, Transition Projects, Site Monitoring, Industrial Hygiene, Analytical Services and miscellaneous Hanford support activities. In addition, details on laboratory scale technology (development) work, Sample Management,more » and Data Management activities are included. This information will be used by Hanford Analytical Services (HAS) and the Sample Management Working Group (SMWG) to assure that laboratories and resources are available and effectively utilized to meet these documented needs.« less
DATA QUALITY OBJECTIVES FOR SELECTING WASTE SAMPLES FOR THE BENCH STEAM REFORMER TEST
DOE Office of Scientific and Technical Information (OSTI.GOV)
BANNING DL
2010-08-03
This document describes the data quality objectives to select archived samples located at the 222-S Laboratory for Fluid Bed Steam Reformer testing. The type, quantity and quality of the data required to select the samples for Fluid Bed Steam Reformer testing are discussed. In order to maximize the efficiency and minimize the time to treat Hanford tank waste in the Waste Treatment and Immobilization Plant, additional treatment processes may be required. One of the potential treatment processes is the fluid bed steam reformer (FBSR). A determination of the adequacy of the FBSR process to treat Hanford tank waste is required.more » The initial step in determining the adequacy of the FBSR process is to select archived waste samples from the 222-S Laboratory that will be used to test the FBSR process. Analyses of the selected samples will be required to confirm the samples meet the testing criteria.« less
Anderson, Anita L.; Campbell, David L.; Beanland, Shay
2001-01-01
Individual mine waste samples were collected and combined to form one composite sample at each of eight mine dump sites in Colorado and New Mexico. The samples were air-dried and sieved to determine the geochemical composition of their <2mm size fraction. Splits of the samples were then rehydrated and their electrical properties were measured in the US Geological Survey Petrophysical Laboratory, Denver, Colorado (PetLab). The PetLab measurements were done twice: in 1999, using convenient amounts of rehydration water ranging from 5% to 8%; and in 2000, using carefully controlled rehydrations to 5% and 10% water. This report gives geochemical analyses of the <2mm size fraction of the composite samples (Appendix A), PetLab graphs of the 1999 measurements (Appendix B), Petlab graphs of the 2000 measurements (Appendix C), and Cole-Cole models of the PetLab data from the 2000 measurements (Appendix D).
Ivahnenko, Tamara; Szabo, Zoltan; Hall, G.S.
1996-01-01
Water samples were collected during 1993 from 22 public supply wells screened in the Kirkwood-Cohansey aquifer system; concentrations of 18 trace elements were determined primarily by using inductively coupled plasma-mass spectrometry (ICP-MS) techniques, though graphite furnace atomic adsorption, hydride generation, and cold- vapor flameless atomic adsorption techniques were used for thallium, arsenic, and mercury, respectively, at the U.S. Geological Survey (USGS) National Water Quality Laboratory (NWQL). In addition, laboratory measurements of alkalinity and turbidity were made. The ground-water samples were collected by using ultra-clean sampling protocols developed by the USGS for collecting ground-water samples in areas with water containing low concentrations of trace elements. This technique is based on recently gained experience in sampling surface water for these elements. Field parameters (water temperature, specific conductance, pH, and dissolved-oxygen concentration) were monitored prior to sample collection. Three equipment blanks were collected to ensure that low-level trace-element contamination did not occur during sample collection. One split sample and a commercially- prepared reference standard were submitted to the NWQL o evaluate laboratory precision and accuracy, respectively. Trace-element concentrations in 10 sample splits and one equipment blank were also determined at the Rutgers University Chemistry Department laboratory. Results of the ICP-MS analyses and cold vapor flameless atomic absorption indicated that five trace elements-- cobalt, copper, lead, mercury, and nickel--were detectable in low concentrations (<0.1-29 mg/L) in most of the samples from the 22 wells, and four elements--aluminum, barium, manganese and zinc--were detected in higher concentrations than the other elements (30-710 mg/L for aluminum; 4-180 mg/L for barium, manganese, and zinc). The remaining nine trace elements were present in concentrations consistently lower than the minimum reporting limit. Turbidity was low (less than 1 nephelometric turbidity unit (NTU)), indicating that the trace-element concentrations were present in the dissolved phase and ideally would be reproducible in the absence of highly variable concentrations of particulates. The concentration of lead in one sample exceeded the U.S. Environmental Protection Agency (USEPA) action level of 15 mg/L; concentrations ranged from <1 to 16 mg/L. Mercury was frequently detected; concentrations ranged from <0.1 to 1.1 mg/L but did not exceed the USEPA maximum contaminant level. Results of analyses of the equipment blanks indicated that samples collected by using the new ultra-clean sampling protocols were free of low-level (< 1mg/L) trace-element contamination. The analysis of the split sample sent to the NWQL had a difference of 5 percent or less for all constituents except aluminum, for which the analysis had a difference of 10 percent. Results of ICP-MS analyses of split water samples sent to the Rutgers University Chemistry Department laboratory were, in general, in good agreement (within 10 percent) with those of the NWQL. Results of the analysis of the commercial standard agreed (within 5 percent) with the known concentrations of the trace elements. The quality-assurance data (three blanks, one split sample, and one standard), although not statistically evaluated because of the small data set, indicate that the measured trace-element concentrations are precise and accurate and that the samples were free of contamination at the microgram-per-liter level of contamination.
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
New Ca-Tims and La-Icp Analyses of GJ-1, Plesovice, and FC1 Reference Materials
NASA Astrophysics Data System (ADS)
Feldman, J. D.; Möller, A.; Walker, J. D.
2014-12-01
Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) U-Pb zircon geochronology relies on external reference standards to monitor and correct for different mass fractionation effects and instrument drift. Common zircon reference materials used within the community, including the KU Isotope Geochemistry Laboratory, are GJ-1 (207Pb/206Pb age: 608.53 +/- 0.37Ma; Jackson et al., 2004), Plesovice (337.13 +/- 0.37 Ma; Slama et al., 2008), and FC-1 (1099.0 +/-0.6 Ma; Paces and Miller, 1993). The age distribution of zircon reference material varies slightly from sample fraction to sample fraction, and the published results for GJ-1 are slightly discordant. As a result, using the published data for the distributed standard splits can lead to small systematic variations when comparing datasets from different labs, and more high precision data are needed to evaluate potential inhomogeneity of sample splits used in different laboratories. Here we characterize these reference materials with cathodoluminescence, LA-ICP-MS traverses across grains, and high precision CA-TIMS to better constrain the ages and assess zoning of these standards, and present the data for comparison with other laboratories. Reducing systematic error by dating our own reference material lends confidence to our analyses and allows for inter-laboratory age reproducibility of unknowns. Additionally, the reduction in propagated uncertainties (especially in GJ-1, for which both the red and yellow variety will be analyzed) will be used to improve long-term reproducibility, comparisons between samples of similar age, detrital populations and composite pluton zircons. Jackson, S.E., et al., 2004, Chemical Geology, v. 211, p. 47-69. Paces, J.B. & Miller, J.D., 1993, Journal of Geophysical Research, v. 80, p. 13997-14013. Slama, J., et al., 2008, Chemical Geology, v. 249. p. 1-35.
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
The purpose of this presentation is to present an overview of the quality control (QC) sections of a draft EPA document entitled, "Quality Assurance/Quality Control Guidance for Laboratories Performing PCR Analyses on Environmental Samples." This document has been prepared by th...
González-Estecha, Montserrat; Bodas-Pinedo, Andrés; Martínez-García, María José; Trasobares-Iglesias, Elena M; Bermejo-Barrera, Pilar; Ordóñez-Iriarte, José María; Llorente-Ballesteros, María Teresa; Prieto-Menchero, Santiago; Guillén-Pérez, José Jesús; Martell-Claros, Nieves; Cuadrado-Cenzual, María Ángeles; Rubio-Herrera, Miguel Ángel; Martínez-Álvarez, Jesús Román; Calvo-Manuel, Elpidio; Farré-Rovira, Rosaura; Herráiz-Martínez, Miguel Ángel; Bretón Lesmes, Irene; García-Donaire, José Antonio; Sáinz-Martín, María; Martínez-Astorquiza, Txantón; Gallardo-Pino, Carmen; Moreno-Rojas, Rafael; Salas-Salvadó, Jordi; Blanco Fuentes, María; Arroyo-Fernández, Manuel; Calle Pascual, Alfonso
2014-11-04
The beneficial effects of fish consumption are well- known. Nevertheless, there is worldwide concern regard methylmercury concentrations in fish, which is why many countries such as the United States, Australia, New Zealand, Canada and numerous European countries have made fish consumption recommendations for their populations, particularly vulnerable groups, in order to México methylmercury intake. Blood and hair are the best biological samples for measuring methylmercury. The most widely-used method to analyse methylmercury is cold vapor atomic absorption spectrometry, although there are also direct methods based on the thermal decomposition of the sample. In recent years, the number of laboratories that measure mercury by inductively coupled plasma mass spectrometry has increased. In addition, the different kinds of mercury can be distinguished by coupling chromatography methods of separation. Laboratories that analyse mercury in biological samples need to participate in external quality control programmes. Even if mercury emissions are reduced, mercury may remain in the environment for many years, so dietary recommendations are fundamental in order to reduce exposure. It is necessary to propose public health measures aimed at decreasing mercury exposure and to evaluate the benefits of such measures from the economic and social standpoints. Copyright AULA MEDICA EDICIONES 2014. Published by AULA MEDICA. All rights reserved.
In situ semi-quantitative analysis of polluted soils by laser-induced breakdown spectroscopy (LIBS).
Ismaël, Amina; Bousquet, Bruno; Michel-Le Pierrès, Karine; Travaillé, Grégoire; Canioni, Lionel; Roy, Stéphane
2011-05-01
Time-saving, low-cost analyses of soil contamination are required to ensure fast and efficient pollution removal and remedial operations. In this work, laser-induced breakdown spectroscopy (LIBS) has been successfully applied to in situ analyses of polluted soils, providing direct semi-quantitative information about the extent of pollution. A field campaign has been carried out in Brittany (France) on a site presenting high levels of heavy metal concentrations. Results on iron as a major component as well as on lead and copper as minor components are reported. Soil samples were dried and prepared as pressed pellets to minimize the effects of moisture and density on the results. LIBS analyses were performed with a Nd:YAG laser operating at 1064 nm, 60 mJ per 10 ns pulse, at a repetition rate of 10 Hz with a diameter of 500 μm on the sample surface. Good correlations were obtained between the LIBS signals and the values of concentrations deduced from inductively coupled plasma atomic emission spectroscopy (ICP-AES). This result proves that LIBS is an efficient method for optimizing sampling operations. Indeed, "LIBS maps" were established directly on-site, providing valuable assistance in optimizing the selection of the most relevant samples for future expensive and time-consuming laboratory analysis and avoiding useless analyses of very similar samples. Finally, it is emphasized that in situ LIBS is not described here as an alternative quantitative analytical method to the usual laboratory measurements but simply as an efficient time-saving tool to optimize sampling operations and to drastically reduce the number of soil samples to be analyzed, thus reducing costs. The detection limits of 200 ppm for lead and 80 ppm for copper reported here are compatible with the thresholds of toxicity; thus, this in situ LIBS campaign was fully validated for these two elements. Consequently, further experiments are planned to extend this study to other chemical elements and other matrices of soils.
Daugaard, Iben; Kjeldsen, Tina E; Hager, Henrik; Hansen, Lise Lotte; Wojdacz, Tomasz K
2015-12-01
Readily accessible formalin-fixed paraffin embedded (FFPE) tissues are a highly valuable source of genetic material for molecular analyses in both research and in vitro diagnostics but frequently genetic material in those samples is highly degraded. With locus-specific methylation changes being widely investigated for use as biomarkers in various aspects of clinical disease management, we aimed to evaluate to what extent standard laboratory procedures can approximate the quality of the DNA extracted from FFPE samples prior to methylation analyses. DNA quality in 107 FFPE non-small cell lung cancer (NSCLC) samples was evaluated using spectrophotometry and gel electrophoresis. Subsequently, the quality assessment results were correlated with the results of locus specific methylation assessment with methylation sensitive high resolution melting (MS-HRM). The correlation of template quality with PCR amplification performance and HRM based methylation detection indicated a significant influence of DNA quality on PCR amplification but not on methylation assessment. In conclusion, standard laboratory procedures fairly well approximate DNA degradation of FFPE samples and DNA degradation does not seem to considerably affect locus-specific methylation assessment by MS-HRM. Copyright © 2015 Elsevier Inc. All rights reserved.
Rice, Karen C.
2008-01-01
Data on the chemical composition of water were collected at least once from 47 amphibian research sites in Maryland, Washington, D.C., and Virginia, from 2005 through 2007. One hundred twenty-five water samples were collected from vernal pools and streams and analyzed as part of long-term monitoring projects of the U.S. Geological Survey Amphibian Research and Monitoring Initiative in the Northeast Region. Field measurements of water temperature, specific conductance, and pH were made. Laboratory analyses of the water samples included acid-neutralizing capacity, total Kjeldahl nitrogen (ammonium plus organic nitrogen), nitrite plus nitrate, total nitrogen, and total phosphorus concentrations. Field and laboratory analytical results of water samples and quality-assurance data are presented.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Pool, K.H.; Evans, J.C.; Olsen, K.B.
1997-08-01
This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-S-102 (Tank S-102) at the Hanford Site in Washington State. Tank headspace samples collected by SGN Eurisys Service Corporation (SESC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by SESC. Ammonia was determined to be above the immediate notification limit of 150 ppm as specified by the sampling and analysis planmore » (SAP). Hydrogen was the principal flammable constituent of the Tank S-102 headspace, determined to be present at approximately 2.410% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.973% of its lower flammability limit (LFL). Total headspace flammability was estimated to be <2.973% of the LFL. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in Table S.1. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0.« less
[On the way to national reference system of laboratory medicine].
Muravskaia, N P; Men'shikov, V V
2014-10-01
The application of standard samples and reference techniques of implementation of measurements is needed for a valid support of reliability of analyses applied in clinical diagnostic laboratories. They play role of landmarks under metrologic monitoring, calibration of devices and control of quality of results. The article presents analysis of shortcomings interfering with formation of national reference system in Russia harmonized with possibilities provided by international organizations. Among them are the joint Committee on metrologic monitoring in laboratory medicine under the auspices of the International Bureau of Weights and Measures, the International Federation of clinical chemistry and laboratory medicine, etc. The results of the recent development of national normative documents, standard samples and techniques assisted by the authors of article are considered. They are the first steps to organization of national reference system which would comprise all range of modern analytical technologies of laboratory medicine. The national and international measures are proposed to enhance the promptest resolving of task of organization of national reference system for laboratory medicine in the interests of increasing of effectiveness of medical care to citizen of Russia.
Vandenabeele-Trambouze, O; Claeys-Bruno, M; Dobrijevic, M; Rodier, C; Borruat, G; Commeyras, A; Garrelly, L
2005-02-01
The need for criteria to compare different analytical methods for measuring extraterrestrial organic matter at ultra-trace levels in relatively small and unique samples (e.g., fragments of meteorites, micrometeorites, planetary samples) is discussed. We emphasize the need to standardize the description of future analyses, and take the first step toward a proposed international laboratory network for performance testing.
Nilles, M.A.; Gordon, J.D.; Schroder, L.J.
1994-01-01
A collocated, wet-deposition sampler program has been operated since October 1988 by the U.S. Geological Survey to estimate the overall sampling precision of wet atmospheric deposition data collected at selected sites in the National Atmospheric Deposition Program and National Trends Network (NADP/NTN). A duplicate set of wet-deposition sampling instruments was installed adjacent to existing sampling instruments at four different NADP/NTN sites for each year of the study. Wet-deposition samples from collocated sites were collected and analysed using standard NADP/NTN procedures. Laboratory analyses included determinations of pH, specific conductance, and concentrations of major cations and anions. The estimates of precision included all variability in the data-collection system, from the point of sample collection through storage in the NADP/NTN database. Sampling precision was determined from the absolute value of differences in the analytical results for the paired samples in terms of median relative and absolute difference. The median relative difference for Mg2+, Na+, K+ and NH4+ concentration and deposition was quite variable between sites and exceeded 10% at most sites. Relative error for analytes whose concentrations typically approached laboratory method detection limits were greater than for analytes that did not typically approach detection limits. The median relative difference for SO42- and NO3- concentration, specific conductance, and sample volume at all sites was less than 7%. Precision for H+ concentration and deposition ranged from less than 10% at sites with typically high levels of H+ concentration to greater than 30% at sites with low H+ concentration. Median difference for analyte concentration and deposition was typically 1.5-2-times greater for samples collected during the winter than during other seasons at two northern sites. Likewise, the median relative difference in sample volume for winter samples was more than double the annual median relative difference at the two northern sites. Bias accounted for less than 25% of the collocated variability in analyte concentration and deposition from weekly collocated precipitation samples at most sites.A collocated, wet-deposition sampler program has been operated since OCtober 1988 by the U.S Geological Survey to estimate the overall sampling precision of wet atmospheric deposition data collected at selected sites in the National Atmospheric Deposition Program and National Trends Network (NADP/NTN). A duplicate set of wet-deposition sampling instruments was installed adjacent to existing sampling instruments four different NADP/NTN sites for each year of the study. Wet-deposition samples from collocated sites were collected and analysed using standard NADP/NTN procedures. Laboratory analyses included determinations of pH, specific conductance, and concentrations of major cations and anions. The estimates of precision included all variability in the data-collection system, from the point of sample collection through storage in the NADP/NTN database.
Friesen, J; Fuhrmann, J; Kietzmann, H; Tannich, E; Müller, M; Ignatius, R
2018-03-23
Multiplex PCR assays offer highly sensitive and specific tools for the detection of enteric pathogens. This prospective study aimed at comparing the novel Roche LightMix Modular Assay Gastro Parasites (LMAGP) detecting Giardia duodenalis, Entamoeba histolytica, Cryptosporidium spp., Blastocystishominis, and Dientamoebafragilis with routine laboratory procedures. Stool specimens (n = 1062 from 1009 patients) were consecutively examined by LMAGP, R-Biopharm Ridascreen enzyme immunoassays (EIAs) detecting G. duodenalis or E. histolytica/dispar, and microscopy of wet mounts. Discrepant results were analysed by in-house PCR. D. fragilis or B. hominis were detected by LMAGP in 131 (14.4%) and 179 (19.9%; 16 samples positive by microscopy; p < 0.0001) of 909 samples, respectively. Of 918 samples analysed for Cryptosporidium spp., six were positive by LMAGP (three could be confirmed by Kinyoun staining and one by in-house PCR). G. duodenalis was detected by LMAGP, EIA, or microscopy in 20, 16, or 9 of 1039 stool samples, respectively; all four samples missed by EIA were confirmed by in-house PCR. In total, 938 stool samples were analysed for E. histolytica/dispar. Nine of ten EIA-positive samples were negative by LMAGP but positive by in-house PCR for E. dispar. One E. histolytica infection (positive by both LMAGP and in-house PCR) was missed by EIA and microscopy. Parasites only detected by microscopy included Enterobius vermicularis eggs (n = 3) and apathogenic amoebae (n = 27). The data call for routine use of multiplex PCR assays for the detection of enteric protozoan parasites in laboratory diagnostics. Copyright © 2018 European Society of Clinical Microbiology and Infectious Diseases. Published by Elsevier Ltd. All rights reserved.
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
DiFrancesco, Robin; Rosenkranz, Susan L; Taylor, Charlene R; Pande, Poonam G; Siminski, Suzanne M; Jenny, Richard W; Morse, Gene D
2013-10-01
Among National Institutes of Health HIV Research Networks conducting multicenter trials, samples from protocols that span several years are analyzed at multiple clinical pharmacology laboratories (CPLs) for multiple antiretrovirals. Drug assay data are, in turn, entered into study-specific data sets that are used for pharmacokinetic analyses, merged to conduct cross-protocol pharmacokinetic analysis, and integrated with pharmacogenomics research to investigate pharmacokinetic-pharmacogenetic associations. The CPLs participate in a semiannual proficiency testing (PT) program implemented by the Clinical Pharmacology Quality Assurance program. Using results from multiple PT rounds, longitudinal analyses of recovery are reflective of accuracy and precision within/across laboratories. The objectives of this longitudinal analysis of PT across multiple CPLs were to develop and test statistical models that longitudinally: (1) assess the precision and accuracy of concentrations reported by individual CPLs and (2) determine factors associated with round-specific and long-term assay accuracy, precision, and bias using a new regression model. A measure of absolute recovery is explored as a simultaneous measure of accuracy and precision. Overall, the analysis outcomes assured 97% accuracy (±20% of the final target concentration of all (21) drug concentration results reported for clinical trial samples by multiple CPLs). Using the Clinical Laboratory Improvement Act acceptance of meeting criteria for ≥2/3 consecutive rounds, all 10 laboratories that participated in 3 or more rounds per analyte maintained Clinical Laboratory Improvement Act proficiency. Significant associations were present between magnitude of error and CPL (Kruskal-Wallis P < 0.001) and antiretroviral (Kruskal-Wallis P < 0.001).
Siener, Roswitha; Buchholz, Noor; Daudon, Michel; Hess, Bernhard; Knoll, Thomas; Osther, Palle J.; Reis-Santos, José; Sarica, Kemal; Traxer, Olivier; Trinchieri, Alberto
2016-01-01
After stone removal, accurate analysis of urinary stone composition is the most crucial laboratory diagnostic procedure for the treatment and recurrence prevention in the stone-forming patient. The most common techniques for routine analysis of stones are infrared spectroscopy, X-ray diffraction and chemical analysis. The aim of the present study was to assess the quality of urinary stone analysis of laboratories in Europe. Nine laboratories from eight European countries participated in six quality control surveys for urinary calculi analyses of the Reference Institute for Bioanalytics, Bonn, Germany, between 2010 and 2014. Each participant received the same blinded test samples for stone analysis. A total of 24 samples, comprising pure substances and mixtures of two or three components, were analysed. The evaluation of the quality of the laboratory in the present study was based on the attainment of 75% of the maximum total points, i.e. 99 points. The methods of stone analysis used were infrared spectroscopy (n = 7), chemical analysis (n = 1) and X-ray diffraction (n = 1). In the present study only 56% of the laboratories, four using infrared spectroscopy and one using X-ray diffraction, fulfilled the quality requirements. According to the current standard, chemical analysis is considered to be insufficient for stone analysis, whereas infrared spectroscopy or X-ray diffraction is mandatory. However, the poor results of infrared spectroscopy highlight the importance of equipment, reference spectra and qualification of the staff for an accurate analysis of stone composition. Regular quality control is essential in carrying out routine stone analysis. PMID:27248840
Siener, Roswitha; Buchholz, Noor; Daudon, Michel; Hess, Bernhard; Knoll, Thomas; Osther, Palle J; Reis-Santos, José; Sarica, Kemal; Traxer, Olivier; Trinchieri, Alberto
2016-01-01
After stone removal, accurate analysis of urinary stone composition is the most crucial laboratory diagnostic procedure for the treatment and recurrence prevention in the stone-forming patient. The most common techniques for routine analysis of stones are infrared spectroscopy, X-ray diffraction and chemical analysis. The aim of the present study was to assess the quality of urinary stone analysis of laboratories in Europe. Nine laboratories from eight European countries participated in six quality control surveys for urinary calculi analyses of the Reference Institute for Bioanalytics, Bonn, Germany, between 2010 and 2014. Each participant received the same blinded test samples for stone analysis. A total of 24 samples, comprising pure substances and mixtures of two or three components, were analysed. The evaluation of the quality of the laboratory in the present study was based on the attainment of 75% of the maximum total points, i.e. 99 points. The methods of stone analysis used were infrared spectroscopy (n = 7), chemical analysis (n = 1) and X-ray diffraction (n = 1). In the present study only 56% of the laboratories, four using infrared spectroscopy and one using X-ray diffraction, fulfilled the quality requirements. According to the current standard, chemical analysis is considered to be insufficient for stone analysis, whereas infrared spectroscopy or X-ray diffraction is mandatory. However, the poor results of infrared spectroscopy highlight the importance of equipment, reference spectra and qualification of the staff for an accurate analysis of stone composition. Regular quality control is essential in carrying out routine stone analysis.
The case for planetary sample return missions. 2. History of Mars.
Gooding, J L; Carr, M H; McKay, C P
1989-08-01
Principal science goals for exploration of Mars are to establish the chemical, isotopic, and physical state of Martian material, the nature of major surface-forming processes and their time scales, and the past and present biological potential of the planet. Many of those goals can only be met by detailed analyses of atmospheric gases and carefully selected samples of fresh rocks, weathered rocks, soils, sediments, and ices. The high-fidelity mineral separations, complex chemical treatments, and ultrasensitive instrument systems required for key measurements, as well as the need to adapt analytical strategies to unanticipated results, point to Earth-based laboratory analyses on returned Martian samples as the best means for meeting the stated objectives.
Schot, Marjolein J C; van Delft, Sanne; Kooijman-Buiting, Antoinette M J; de Wit, Niek J; Hopstaken, Rogier M
2015-01-01
Objective Various point-of-care testing (POCT) urine analysers are commercially available for routine urine analysis in general practice. The present study compares analytical performance, agreement and user-friendliness of six different POCT urine analysers for diagnosing urinary tract infection in general practice. Setting All testing procedures were performed at a diagnostic centre for primary care in the Netherlands. Urine samples were collected at four general practices. Primary and secondary outcome measures Analytical performance and agreement of the POCT analysers regarding nitrite, leucocytes and erythrocytes, with the laboratory reference standard, was the primary outcome measure, and analysed by calculating sensitivity, specificity, positive and negative predictive value, and Cohen's κ coefficient for agreement. Secondary outcome measures were the user-friendliness of the POCT analysers, in addition to other characteristics of the analysers. Results The following six POCT analysers were evaluated: Uryxxon Relax (Macherey Nagel), Urisys 1100 (Roche), Clinitek Status (Siemens), Aution 11 (Menarini), Aution Micro (Menarini) and Urilyzer (Analyticon). Analytical performance was good for all analysers. Compared with laboratory reference standards, overall agreement was good, but differed per parameter and per analyser. Concerning the nitrite test, the most important test for clinical practice, all but one showed perfect agreement with the laboratory standard. For leucocytes and erythrocytes specificity was high, but sensitivity was considerably lower. Agreement for leucocytes varied between good to very good, and for the erythrocyte test between fair and good. First-time users indicated that the analysers were easy to use. They expected higher productivity and accuracy when using these analysers in daily practice. Conclusions The overall performance and user-friendliness of all six commercially available POCT urine analysers was sufficient to justify routine use in suspected urinary tract infections in general practice. PMID:25986635
Ladwig, R; Vigo, A; Fedeli, L M G; Chambless, L E; Bensenor, I; Schmidt, M I; Vidigal, P G; Castilhos, C D; Duncan, B B
2016-08-01
Multi-center epidemiological studies must ascertain that their measurements are accurate and reliable. For laboratory measurements, reliability can be assessed through investigation of reproducibility of measurements in the same individual. In this paper, we present results from the quality control analysis of the baseline laboratory measurements from the ELSA-Brasil study. The study enrolled 15,105 civil servants at 6 research centers in 3 regions of Brazil between 2008-2010, with multiple biochemical analytes being measured at a central laboratory. Quality control was ascertained through standard laboratory evaluation of intra- and inter-assay variability and test-retest analysis in a subset of randomly chosen participants. An additional sample of urine or blood was collected from these participants, and these samples were handled in the same manner as the original ones, locally and at the central laboratory. Reliability was assessed with the intraclass correlation coefficient (ICC), estimated through a random effects model. Coefficients of variation (CV) and Bland-Altman plots were additionally used to assess measurement variability. Laboratory intra and inter-assay CVs varied from 0.86% to 7.77%. From test-retest analyses, the ICCs were high for the majority of the analytes. Notably lower ICCs were observed for serum sodium (ICC=0.50; 95%CI=0.31-0.65) and serum potassium (ICC=0.73; 95%CI=0.60-0.83), due to the small biological range of these analytes. The CVs ranged from 1 to 14%. The Bland-Altman plots confirmed these results. The quality control analyses showed that the collection, processing and measurement protocols utilized in the ELSA-Brasil produced reliable biochemical measurements.
Scaling ice microstructures from the laboratory to nature: cryo-EBSD on large samples.
NASA Astrophysics Data System (ADS)
Prior, David; Craw, Lisa; Kim, Daeyeong; Peyroux, Damian; Qi, Chao; Seidemann, Meike; Tooley, Lauren; Vaughan, Matthew; Wongpan, Pat
2017-04-01
Electron backscatter diffraction (EBSD) has extended significantly our ability to conduct detailed quantitative microstructural investigations of rocks, metals and ceramics. EBSD on ice was first developed in 2004. Techniques have improved significantly in the last decade and EBSD is now becoming more common in the microstructural analysis of ice. This is particularly true for laboratory-deformed ice where, in some cases, the fine grain sizes exclude the possibility of using a thin section of the ice. Having the orientations of all axes (rather than just the c-axis as in an optical method) yields important new information about ice microstructure. It is important to examine natural ice samples in the same way so that we can scale laboratory observations to nature. In the case of ice deformation, higher strain rates are used in the laboratory than those seen in nature. These are achieved by increasing stress and/or temperature and it is important to assess that the microstructures produced in the laboratory are comparable with those observed in nature. Natural ice samples are coarse grained. Glacier and ice sheet ice has a grain size from a few mm up to several cm. Sea and lake ice has grain sizes of a few cm to many metres. Thus extending EBSD analysis to larger sample sizes to include representative microstructures is needed. The chief impediments to working on large ice samples are sample exchange, limitations on stage motion and temperature control. Large ice samples cannot be transferred through a typical commercial cryo-transfer system that limits sample sizes. We transfer through a nitrogen glove box that encloses the main scanning electron microscope (SEM) door. The nitrogen atmosphere prevents the cold stage and the sample from becoming covered in frost. Having a long optimal working distance for EBSD (around 30mm for the Otago cryo-EBSD facility) , by moving the camera away from the pole piece, enables the stage to move without crashing into either the EBSD camera or the SEM pole piece (final lens). In theory a sample up to 100mm perpendicular to the tilt axis by 150mm parallel to the tilt axis can be analysed. In practice, the motion of our stage is restricted to maximum dimensions of 100 by 50mm by a conductive copper braid on our cold stage. Temperature control becomes harder as the samples become larger. If the samples become too warm then they will start to sublime and the quality of EBSD data will reduce. Large samples need to be relatively thin ( 5mm or less) so that conduction of heat to the cold stage is more effective at keeping the surface temperature low. In the Otago facility samples of up to 40mm by 40mm present little problem and can be analysed for several hours without significant sublimation. Larger samples need more care, e.g. fast sample transfer to keep the sample very cold. The largest samples we work on routinely are 40 by 60mm in size. We will show examples of EBSD data from glacial ice and sea ice from Antarctica and from large laboratory ice samples.
Organic solutes in ground water at the Idaho National Engineering Laboratory
Leenheer, Jerry A.; Bagby, Jefferson C.
1982-01-01
In August 1980, the U.S. Geological Survey started a reconnaissance survey of organic solutes in drinking water sources, ground-water monitoring wells, perched water table monitoring wells, and in select waste streams at the Idaho National Engineering Laboratory (INEL). The survey was to be a two-phase program. In the first phase, 77 wells and 4 potential point sources were sampled for dissolved organic carbon (DOC). Four wells and several potential point sources of insecticides and herbicides were sampled for insecticides and herbicides. Fourteen wells and four potential organic sources were sampled for volatile and semivolatile organic compounds. The results of the DOC analyses indicate no high level (>20 mg/L DOC) organic contamination of ground water. The only detectable insecticide or herbicide was a DDT concentration of 10 parts per trillion (0.01 microgram per liter) in one observation well. The volatile and semivolatile analyses do not indicate the presence of hazardous organic contaminants in significant amounts (>10 micrograms per liter) in the samples taken. Due to the lack of any significant organic ground-water contamination in this reconnaissance survey, the second phase of the study, which was to follow up the first phase by additional sampling of any contaminated wells, was canceled.
A human fecal contamination index for ranking impaired ...
Human fecal pollution of surface water remains a public health concern worldwide. As a result, there is a growing interest in the application of human-associated fecal source identification quantitative real-time PCR (qPCR) technologies for recreational water quality risk management. The transition from a research subject to a management tool requires the integration of standardized water sampling, laboratory, and data analysis procedures. In this study, a standardized HF183/BacR287 qPCR method was combined with a water sampling strategy and Bayesian data algorithm to establish a human fecal contamination index that can be used to rank impaired recreational water sites polluted with human waste. Stability and bias of index predictions were investigated under various parameters including siteswith different pollution levels, sampling period time range (1-15 weeks), and number of qPCR replicates per sample (2-14 replicates). Sensitivity analyses were conducted with simulated data sets (100 iterations) seeded with HF183/BacR287 qPCR laboratory measurements from water samples collected from three Southern California sites (588 qPCR measurements). Findings suggest that site ranking is feasible and that all parameters tested influence stability and bias in human fecal contamination indexscoring. Trends identified by sensitivity analyses will provide managers with the information needed to design and conduct field studies to rank impaired recreational water sites based
Laboratory theory and methods for sediment analysis
Guy, Harold P.
1969-01-01
The diverse character of fluvial sediments makes the choice of laboratory analysis somewhat arbitrary and the pressing of sediment samples difficult. This report presents some theories and methods used by the Water Resources Division for analysis of fluvial sediments to determine the concentration of suspended-sediment samples and the particle-size distribution of both suspended-sediment and bed-material samples. Other analyses related to these determinations may include particle shape, mineral content, and specific gravity, the organic matter and dissolved solids of samples, and the specific weight of soils. The merits and techniques of both the evaporation and filtration methods for concentration analysis are discussed. Methods used for particle-size analysis of suspended-sediment samples may include the sieve pipet, the VA tube-pipet, or the BW tube-VA tube depending on the equipment available, the concentration and approximate size of sediment in the sample, and the settling medium used. The choice of method for most bed-material samples is usually limited to procedures suitable for sand or to some type of visual analysis for large sizes. Several tested forms are presented to help insure a well-ordered system in the laboratory to handle the samples, to help determine the kind of analysis required for each, to conduct the required processes, and to assist in the required computations. Use of the manual should further 'standardize' methods of fluvial sediment analysis among the many laboratories and thereby help to achieve uniformity and precision of the data.
Mubemba, B; Thompson, P N; Odendaal, L; Coetzee, P; Venter, E H
2017-05-01
Rift Valley fever (RVF), caused by an arthropod borne Phlebovirus in the family Bunyaviridae, is a haemorrhagic disease that affects ruminants and humans. Due to the zoonotic nature of the virus, a biosafety level 3 laboratory is required for isolation of the virus. Fresh and frozen samples are the preferred sample type for isolation and acquisition of sequence data. However, these samples are scarce in addition to posing a health risk to laboratory personnel. Archived formalin-fixed, paraffin-embedded (FFPE) tissue samples are safe and readily available, however FFPE derived RNA is in most cases degraded and cross-linked in peptide bonds and it is unknown whether the sample type would be suitable as reference material for retrospective phylogenetic studies. A RT-PCR assay targeting a 490 nt portion of the structural G N glycoprotein encoding gene of the RVFV M-segment was applied to total RNA extracted from archived RVFV positive FFPE samples. Several attempts to obtain target amplicons were unsuccessful. FFPE samples were then analysed using next generation sequencing (NGS), i.e. Truseq ® (Illumina) and sequenced on the Miseq ® genome analyser (Illumina). Using reference mapping, gapped virus sequence data of varying degrees of shallow depth was aligned to a reference sequence. However, the NGS did not yield long enough contigs that consistently covered the same genome regions in all samples to allow phylogenetic analysis. Copyright © 2017 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Delay, Jacques; Distinguin, Marc
ANDRA (Agence Nationale pour la Gestion de Déchets Radioactifs) has developed an integrated approach to characterizing the hydrogeology of the carbonate strata that encase the Callovo-Oxfordian argillite at the Meuse/Haute-Marne Laboratory site. The argillites are difficult to characterize due to their low permeability. The barrier properties of the argillites can be inferred from the flow and chemistry properties of the encasing Oxfordian and Dogger carbonates. Andras deep hole approach uses reverse air circulation drilling, geophysical logging, flow meter logging, geochemical sampling, and analyses of the pumping responses during sampling. The data support numerical simulations that evaluate the argillites hydraulic behaviour.
Implementing self sustained quality control procedures in a clinical laboratory.
Khatri, Roshan; K C, Sanjay; Shrestha, Prabodh; Sinha, J N
2013-01-01
Quality control is an essential component in every clinical laboratory which maintains the excellence of laboratory standards, supplementing to proper disease diagnosis, patient care and resulting in overall strengthening of health care system. Numerous quality control schemes are available, with combinations of procedures, most of which are tedious, time consuming and can be "too technical" whereas commercially available quality control materials can be expensive especially for laboratories in developing nations like Nepal. Here, we present a procedure performed at our centre with self prepared control serum and use of simple statistical tools for quality assurance. The pooled serum was prepared as per guidelines for preparation of stabilized liquid quality control serum from human sera. Internal Quality Assessment was performed on this sample, on a daily basis which included measurement of 12 routine biochemical parameters. The results were plotted on Levey-Jennings charts and analysed with quality control rules, for a period of one month. The mean levels of biochemical analytes in self prepared control serum were within normal physiological range. This serum was evaluated every day along with patients' samples. The results obtained were plotted on control charts and analysed using common quality control rules to identify possible systematic and random errors. Immediate mitigation measures were taken and the dispatch of erroneous reports was avoided. In this study we try to highlight on a simple internal quality control procedure which can be performed by laboratories, with minimum technology, expenditure, and expertise and improve reliability and validity of the test reports.
Reddy, Michael M.; Gunther, Charmaine D.
2012-01-01
This report presents results of chemical analysis for samples collected during March, 1995, as part of a study to quantify the interaction of aquatic organic material (referred to here as dissolved organic carbon with dissolved metal ions). The work was done in conjunction with the South Florida Water Management District, the U.S. Environmental Protection Agency, the U.S. Geological Survey South Florida Ecosystems Initiative, and the South Florida National Water Quality Assessment Study Unit. Samples were collected from surface canals and from marsh sites. Results are based on onsite and laboratory measurements for 27 samples collected at 10 locations. The data file contains sample description, dissolved organic carbon concentration and specific ultraviolet absorbance, and additional analytical data for samples collected at several sites in the Water Conservation Areas, the Everglades, south Florida.
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.
Multicomponent blood lipid analysis by means of near infrared spectroscopy, in geese.
Bazar, George; Eles, Viktoria; Kovacs, Zoltan; Romvari, Robert; Szabo, Andras
2016-08-01
This study provides accurate near infrared (NIR) spectroscopic models on some laboratory determined clinicochemical parameters (i.e. total lipid (5.57±1.95 g/l), triglyceride (2.59±1.36 mmol/l), total cholesterol (3.81±0.68 mmol/l), high density lipoprotein (HDL) cholesterol (2.45±0.58 mmol/l)) of blood serum samples of fattened geese. To increase the performance of multivariate chemometrics, samples significantly deviating from the regression models implying laboratory error were excluded from the final calibration datasets. Reference data of excluded samples having outlier spectra in principal component analysis were not marked as false. Samples deviating from the regression models but having non outlier spectra in PCA were identified as having false reference constituent values. Based on the NIR selection methods, 5% of the reference measurement data were rated as doubtful. The achieved models reached R(2) of 0.864, 0.966, 0.850, 0.793, and RMSE of 0.639 g/l, 0.232 mmol/l, 0.210 mmol/l, 0.241 mmol/l for total lipid, triglyceride, total cholesterol and HDL cholesterol, respectively, during independent validation. Classical analytical techniques focus on single constituents and often require chemicals, time-consuming measurements, and experienced technicians. NIR technique provides a quick, cost effective, non-hazardous alternative method for analysis of several constituents based on one single spectrum of each sample, and it also offers the possibility for looking at the laboratory reference data critically. Evaluation of reference data to identify and exclude falsely analyzed samples can provide warning feedback to the reference laboratory, especially in the case of analyses where laboratory methods are not perfectly suited to the subjected material and there is an increased chance of laboratory error. Copyright © 2016 Elsevier B.V. All rights reserved.
Resolution of plasma sample mix-ups through comparison of patient antibody patterns to E. coli.
Vetter, Beatrice N; Orlowski, Vanessa; Schüpbach, Jörg; Böni, Jürg; Rühe, Bettina; Huder, Jon B
2015-12-01
Accidental sample mix-ups and the need for their swift resolution is a challenge faced by every analytical laboratory. To this end, we developed a simple immunoblot-based method, making use of a patient's characteristic plasma antibody profile to Escherichia coli (E. coli) proteins. Nitrocellulose strips of size-separated proteins from E. coli whole-cell lysates were incubated with patient plasma and visualised with an enzyme-coupled secondary antibody and substrate. Plasma samples of 20 random patients as well as five longitudinal samples of three patients were analysed for antibody band patterns, to evaluate uniqueness and consistency over time, respectively. For sample mix-ups, antibody band patterns of questionable samples were compared with samples of known identity. Comparison of anti-E. coli antibody patterns of 20 random patients showed a unique antibody profile for each patient. Antibody profiles remained consistent over time, as shown for three patients over several years. Three example cases demonstrate the use of this methodology in mis-labelling or -pipetting incidences. Our simple method for resolving plasma sample mix-ups between non-related individuals can be performed with basic laboratory equipment and thus can easily be adopted by analytical laboratories. Copyright © 2015 Elsevier B.V. All rights reserved.
DOE Office of Scientific and Technical Information (OSTI.GOV)
none, none; Tuchman, Nancy
The U.S. Department of Energy awarded Loyola University Chicago and the Institute of Environmental Sustainability (IES) $486,000.00 for the proposal entitled “Chicago clean air, clean water project: Environmental monitoring for a healthy, sustainable urban future.” The project supported the purchase of analytical instruments for the development of an environmental analytical laboratory. The analytical laboratory is designed to support the testing of field water and soil samples for nutrients, industrial pollutants, heavy metals, and agricultural toxins, with special emphasis on testing Chicago regional soils and water affected by coal-based industry. Since the award was made in 2010, the IES has beenmore » launched (fall 2013), and the IES acquired a new state-of-the-art research and education facility on Loyola University Chicago’s Lakeshore campus. Two labs were included in the research and education facility. The second floor lab is the Ecology Laboratory where lab experiments and analyses are conducted on soil, plant, and water samples. The third floor lab is the Environmental Toxicology Lab where lab experiments on environmental toxins are conducted, as well as analytical tests conducted on water, soil, and plants. On the south end of the Environmental Toxicology Lab is the analytical instrumentation collection purchased from the present DOE grant, which is overseen by a full time Analytical Chemist (hired January 2016), who maintains the instruments, conducts analyses on samples, and helps to train faculty and undergraduate and graduate student researchers.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Oji, L. N.
The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) Engineering (SRR-E) to provide sample characterization and analyses of Tank 51 sludge samples in support of Sludge Batch (SB) 10. The two Tank 51 sludge samples were sampled and delivered to SRNL in May of 2017. These two tank 51 sludge samples were combined into one composite sample and analyzed for corrosion controls analytes, select radionuclides, chemical elements, density and weight percent total solids and aluminum hydroxides (gibbsite and boehmite) by x-ray diffraction.
MSL SAM-Like Evolved Gas Analyses of Si-rich Amorphous Materials
NASA Technical Reports Server (NTRS)
McAdam, Amy; Knudson, Christine; Sutter, Brad; Andrejkovicova, Slavka; Archer, P. Douglas; Franz, Heather; Eigenbrode, Jennifer; Morris, Richard; Ming, Douglas; Sun, Vivian;
2016-01-01
Chemical and mineralogical analyses of several samples from Murray Formation mudstones and Stimson Formation sandstones by the Mars Science Laboratory (MSL) revealed the presence of Si-rich amorphous or poorly ordered materials. It is possible to identify the presence of high-SiO2 vs. lower SiO2 amorphous materials (e.g., basaltic glasses), based on the position of the resulting wide diffraction features in XRD patterns from the Chemistry and Mineralogy (CheMin) instrument, but it is not possible to distinguish between several candidate high-SiO2 amorphous materials such as opal-A or rhyolitic glass. In the Buckskin (BS) sample from the upper Murray Formation, and the Big Sky (BY) and Greenhorn (GH) samples from the Stimson Formation, analyses by the Sample Analysis at Mars (SAM) instrument showed very broad H2O evolutions during sample heating at temperatures >450-500degC which had not been observed from previous samples. BS also had a significant broad evolution <450-500degC. We have undertaken a laboratory study targeted at understanding if the data from SAM can be used to place constraints on the nature of the amorphous phases. SAM-like evolved gas analyses have been performed on several opal and rhyolitic glass samples. Opal-A samples exhibited wide <500degC H2O evolutions, with lesser H2O evolved above 500degC. H2O evolution traces from rhyolitic glasses varied, having either two broad H2O peaks, <300degC and >500degC, or a broad peak centered around 400degC. For samples that produced two evolutions, the lower temperature peak is more intense than the higher temperature peak, a trend also exhibited by opal-A. This trend is consistent with data from BS, but does not seem consistent with data from BY and GH which evolved most of their H2O >500degC. It may be that dehydration of opal-A and/or rhyolitic glass can result in some preferential loss of lower temperature H2O, to produce traces that more closely resemble BY and GH. This is currently under investigation and results will be reported.
Collection analysis and interpretation of data on relationship between drugs and driving
DOT National Transportation Integrated Search
1972-02-01
The purpose of this study was to determine if drug usage is relate to driving history. Laboratory analyses of urine samples, in-dept interviews, and public driving records were obtained to investigate the relationship of traffic accidents and violati...
AIR DRYING AND PRETREATMENT EFFECTS ON SOIL SULFATE SORPTION
Drying, freezing, and refrigeration are commonly employed to facilitate the handling and storage of soil samples on which chemical, biological and physical analyses are to be performed. hese laboratory protocol have the potential to alter soil chemical characteristics and may res...
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)
Thomas, B.L.; Pool, K.H.; Evans, J.C.
1997-01-01
This report describes the analytical results of vapor samples taken from the headspace of waste storage tank 241-BY-108 (Tank BY-108) at the Hanford Site in Washington State. The results described in this report is the second in a series comparing vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling (ISVS) system without high efficiency particulate air (HEPA) prefiltration. The results include air concentrations of water (H{sub 2}O) and ammonia (NH{sub 3}), permanent gases, total non-methane organic compounds (TO-12), and individual organic analytes collected in SUMMA{trademark} canisters and on triple sorbent traps (TSTs).more » Samples were collected by Westinghouse Hanford Company (WHC) and analyzed by Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volume measurements provided by WHC.« less
Sampling and analysis plan for sludge located on the floor and in the pits of the 105-K basins
DOE Office of Scientific and Technical Information (OSTI.GOV)
BAKER, R.B.
1998-11-20
This Sampling and Analysis Plan (SAP) provides direction for the sampling of the sludge found on the floor and in the remote pits of the 105-K Basins to provide: (1) basic data for the sludges that have not been characterized to-date and (2) representative Sludge material for process tests to be made by the SNF Project/K Basins sludge treatment process subproject. The sampling equipment developed will remove representative samples of the radioactive sludge from underwater at the K Basins, depositing them in shielded containers for transport to the Hanford Site laboratories. Included in the present document is the basic backgroundmore » logic for selection of the samples to meet the requirements established in the Data Quality Objectives (DQO), HNF-2033, for this sampling activity. The present document also includes the laboratory analyses, methods, procedures, and reporting that will be required to meet the DQO.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Hutton, Rick
2011-12-01
Annual sampling was conducted at the Rio Blanco, Colorado, site for the Long-Term Hydrologic Monitoring Program May 16-17, 2011, to monitor groundwater and surface water for potential radionuclide contamination. Sampling and analyses were conducted as specified in Sampling and Analysis Plan for the U.S. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated). A duplicate sample was collected from location Johnson Artesian WL. 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 spectrometry, and for tritium using the conventional method.more » Tritium was not measured using the enrichment method because the EPA laboratory no longer offers that service. Results of this monitoring at the Rio Blanco site demonstrate that groundwater and surface water outside the boundaries have not been affected by project-related contaminants.« less
NASA Technical Reports Server (NTRS)
Mittlefehldt, D. W.
2012-01-01
The capability of scientific instrumentation flown on planetary orbiters and landers has made great advances since the signature Viking mission of the seventies. At some point, however, the science return from orbital remote sensing, and even in situ measurements, becomes incremental, rather than revolutionary. This is primarily caused by the low spatial resolution of such measurements, even for landed instrumentation, the incomplete mineralogical record derived from such measurements, the inability to do the detailed textural, mineralogical and compositional characterization needed to demonstrate equilibrium or reaction paths, and the lack of chronological characterization. For the foreseeable future, flight instruments will suffer from this limitation. In order to make the next revolutionary breakthrough in understanding the early geological and climatological history of Mars, samples must be available for interrogation using the full panoply of laboratory-housed analytical instrumentation. Laboratory studies of samples allow for determination of parageneses of rocks through microscopic identification of mineral assemblages, evaluation of equilibrium through electron microbeam analyses of mineral compositions and structures, determination of formation temperatures through secondary ion or thermal ionization mass spectrometry (SIMS or TIMS) analyses of stable isotope compositions. Such details are poorly constrained by orbital data (e.g. phyllosilicate formation at Mawrth Vallis), and incompletely described by in situ measurements (e.g. genesis of Burns formation sediments at Meridiani Planum). Laboratory studies can determine formation, metamorphism and/or alteration ages of samples through SIMS or TIMS of radiogenic isotope systems; a capability well-beyond flight instrumentation. Ideally, sample return should be from a location first scouted by landers such that fairly mature hypotheses have been formulated that can be tested. However, samples from clastic sediments derived from an extensive region of Mars can provide important, detailed understanding of early martian geological and climatological history. Interrogating clastic "sediments" from the Earth, Moon and asteroids has allowed discovery of new crustal units, identification of now-vanished crust, and determination of the geological history of extensive, remote regions. Returned sample of martian fluvial and/or aeolian sediments, for example from Gale crater, could be "read like a book" in terrestrial laboratories to provide truly revolutionary new insights into early martian geological and climatological evolution.
Kristin Bunte; Steven R. Abt
2001-01-01
This document provides guidance for sampling surface and subsurface sediment from wadable gravel-and cobble-bed streams. After a short introduction to streams types and classifications in gravel-bed rivers, the document explains the field and laboratory measurement of particle sizes and the statistical analysis of particle-size distributions. Analysis of particle...
NASA Astrophysics Data System (ADS)
Managadze, G. G.; Safronova, A. A.; Luchnikov, K. A.; Vorobyova, E. A.; Duxbury, N. S.; Wurz, P.; Managadze, N. G.; Chumikov, A. E.; Khamizov, R. Kh.
2017-05-01
We propose a new technique for the detection of microorganisms by elemental composition analyses of a sample extracted from regolith, permafrost, and ice of extraterrestrial bodies. We also describe the design of the ABIMAS instrument, which consists of the onboard time-of-flight laser mass-reflectron (TOF LMR) and the sample preparation unit (SPU) for biomass extraction. This instrument was initially approved to fly on board the ExoMars 2020 lander mission. The instrument can be used to analyze the elemental composition of possible extraterrestrial microbial communities and compare it to that of terrestrial microorganisms. We have conducted numerous laboratory studies to confirm the possibility of biomass identification via the following biomarkers: P/S and Ca/K ratios, and C and N abundances. We underline that only the combination of these factors will allow one to discriminate microbial samples from geological ones. Our technique has been tested experimentally in numerous laboratory trials on cultures of microorganisms and polar permafrost samples as terrestrial analogues for martian polar soils. We discuss various methods of extracting microorganisms and sample preparation. The developed technique can be used to search for and identify microorganisms in different martian samples and in the subsurface of other planets, satellites, comets, and asteroids—in particular, Europa, Ganymede, and Enceladus.
NASA Astrophysics Data System (ADS)
Jordan, B.
2016-12-01
Field-based petrologic research projects often involve multiple field seasons, with geochemical analysis of samples collected in one season informing aspects of subsequent field seasons. To simulate this approach in the Iceland Volcanology Field Camp (South Dakota School of Mines & Technology) a portable X-ray fluorescence spectrometer (pXRF) was employed to provide "laboratory analyses" in support of a course mapping project. The project was conducted in the Árnes central volcano in the Neogene plateau lava succession in the West Fjords of northwestern Iceland. The field area has a wide compositional spectrum from basalt to rhyolite, with abundant intermediates. The pXRF is particularly helpful in the study of these kinds of rocks in Iceland because lithologies can be quite similar across a wide range of compositions (often lacking diagnostic macroscopic phenocryst assemblages, and having similar groundmass characteristics). A Bruker Tracer III-SD pXRF was utilized, operating at 40 KeV and 11.2 μA with no filter. Analyses were conducted at basecamp in the evenings on relatively flat fresh surfaces, with three 30 s analyses of different spots for each sample. A basic empirical calibration was generated with six aphyric samples previously analyzed by laboratory XRF. Light elements Na, Mg, and Al were not determined directly, but were estimated based on linear or polynomial correlations with other elements or elemental ratios (K, Ca, and Sr/Y respectively) determined from a previously obtained laboratory XRF data set for this central volcano. The resulting chemical analyses (normalized to sum to 100%) provided full major and minor element compositions to be used for classification, and several trace elements (V, Sr, Y, Zr) that could potentially distinguish different lavas of similar major element composition. The approach is coarse, and has pitfalls particularly regarding porphyritic rocks, but serves the objectives of the field camp project.
Gómez-Sucerquia, Leysa Jackeline; Triana-Chávez, Omar; Jaramillo-Ocampo, Nicolás
2009-09-01
Previous studies have reported genetic differences between wild-caught sylvatic, domestic and laboratory pop-ulations of several Triatominae species. The differences between sylvatic and laboratory colonies parallel are similar to the differences observed between sylvatic and domestic populations. Laboratory colonies are frequently used as references for field populations, but the consequences of founder events on the genetic makeup of laboratory or domestic populations are rarely quantified. Our goal was to quantify the genetic change in Rhodnius pallescens populations artificially submitted to founder effects via laboratory colonization. We compared the genetic makeup of two sylvatic populations and their laboratory descendants using a panel of 10 microsatellite markers. Both sylvatic populations were initially collected from palm trees, but the colonies differed in the number of founder insects and amount of time kept in the laboratory. We evaluated allelic polymorphism, differences between expected and observed heterozygosity, estimates of population differentiation (Fst) and inbreeding (Fis, Fit) and cluster analyses based on Nei's distances. We found a unique genetic structure for each sample population, with significant differentiation between the field insects and each of the laboratory generations. These analyses showed strong founder effects and showed that genetic drift had led to a genetic equilibrium over several generations of isolation. Our results suggest that laboratory colonies of R. pallescens have a different genetic structure than their wild relatives and similar processes likely affect other Triatominae laboratory stocks.
Cosmic veto gamma-spectrometry for Comprehensive Nuclear-Test-Ban Treaty samples
NASA Astrophysics Data System (ADS)
Burnett, J. L.; Davies, A. V.
2014-05-01
The Comprehensive Nuclear-Test-Ban Treaty (CTBT) is supported by a global network of monitoring stations that perform high-resolution gamma-spectrometry on air filter samples for the identification of 85 radionuclides. At the UK CTBT Radionuclide Laboratory (GBL15), a novel cosmic veto gamma-spectrometer has been developed to improve the sensitivity of station measurements, providing a mean background reduction of 80.8% with mean MDA improvements of 45.6%. The CTBT laboratory requirement for a 140Ba MDA is achievable after 1.5 days counting compared to 5-7 days using conventional systems. The system consists of plastic scintillation plates that detect coincident cosmic-ray interactions within an HPGe gamma-spectrometer using the Canberra LynxTM multi-channel analyser. The detector is remotely configurable using a TCP/IP interface and requires no dedicated coincidence electronics. It would be especially useful in preventing false-positives at remote station locations (e.g. Halley, Antarctica) where sample transfer to certified laboratories is logistically difficult. The improved sensitivity has been demonstrated for a CTBT air filter sample collected after the Fukushima incident.
Dobecki, Marek
2012-01-01
This paper reviews the requirements for measurement methods of chemical agents in the air at workstations. European standards, which have a status of Polish standards, comprise some requirements and information on sampling strategy, measuring techniques, type of samplers, sampling pumps and methods of occupational exposure evaluation at a given technological process. Measurement methods, including air sampling and analytical procedure in a laboratory, should be appropriately validated before intended use. In the validation process, selected methods are tested and budget of uncertainty is set up. The validation procedure that should be implemented in the laboratory together with suitable statistical tools and major components of uncertainity to be taken into consideration, were presented in this paper. Methods of quality control, including sampling and laboratory analyses were discussed. Relative expanded uncertainty for each measurement expressed as a percentage, should not exceed the limit of values set depending on the type of occupational exposure (short-term or long-term) and the magnitude of exposure to chemical agents in the work environment.
NASA Astrophysics Data System (ADS)
Ma, Jin; Kong, Xiang-Zhao; Saar, Martin O.
2017-04-01
Fluid-rock interactions play an important role in the engineering processes such as chemical stimulation of enhanced geothermal systems and carbon capture, utilization, and storage. However, these interactions highly depend on the accessible reactive surface area of the minerals that are generally poorly constrained for natural geologic samples. In particular, quantifying surface area of each reacting mineral within whole rock samples is challenging due to the heterogeneous distribution of minerals and pore space. In this study, detailed laboratory analyses were performed on sandstone samples from deep geothermal sites in Lithuania. We measure specific surface area of whole rock samples using a gas adsorption method (so-called B.E.T.) with N2 at a temperature of 77.3K. We also quantify their porosity and pore size distribution by a Helium gas pycnometer and a Hg porosimetry, respectively. Rock compositions are determined by a combination of X-ray fluorescence (XRF) and quantitative scanning electron microscopy (SEM) - Energy-dispersive X-ray spectroscopy (EDS), which are later geometrically mapped on images of two-dimensional SEM- Backscattered electrons (BSE) with a resolution of 1.2 μm and three-dimensional micro-CT with a resolution of 10.3 μm to produce a digital mineral map for further constraining the accessibility of reactive minerals. Moreover, we attempt to link the whole rock porosity, pore size distribution, and B.E.T. specific surface area with the digital mineral maps. We anticipate these necessary analyses to provide in-depth understanding of fluid sample chemistry from later hydrothermal reactive flow-through experiments on whole rock samples at elevated pressure and temperature.
Neogi, Sutapa Bandyopadhyay; Negandhi, Preeti H; Ganguli, Abhijit; Chopra, Sapna; Sandhu, Navraj; Gupta, Ravi Kant; Zodpey, Sanjay; Singh, Amarjeet; Singh, Arun; Gupta, Rakesh
2015-09-04
Sex ratio is an important indicator of development. Despite all the measures undertaken for improvement, it remains an issue of concern in India, with Haryana having a very low sex ratio in the country. Studies have been conducted indicating that consumption of indigenous drugs used for sex selection (SSD) could be strongly associated with adverse effects on the foetal development, including congenital malformations. Some samples of SSDs were collected from parts of North India and analysed in a standard laboratory for its components. Thirty SSDs used by the local community were procured from various sources in north India through a rigorous process of collection. These were subjected to laboratory tests to investigate the presence of phytoestrogen and testosterone. Following sample extraction, thin layer chromatography and high performance liquid chromatography were carried out for analysing phytoestrogen content. SSDs were available in various forms such as powder, tablets, mostly from faith healers. Around 87% of the samples collected from sources like doctors, quacks and faith healers were to be taken by the pregnant women after conception; 63% drugs were strongly positive for phytoestrogens (genistein, daidzein, formononetin) and 20% drugs were positive for testosterone. The average dose of the components as calculated after analyses was as follows: daidzein--14.1 mg/g sample, genistein--8.6 mg/g sample, formononetin--5 mg/g sample. These SSDs could be potentially detrimental to the growth and development of the foetus. This is likely to have implications on the health of the community. In view of the results obtained in our study, we strongly attest the importance in curbing this harmful practice by banning the supply of the drugs as well as by advocating behavioural changes in the community.
NASA Technical Reports Server (NTRS)
Danielson, Lisa; Draper, David
2016-01-01
NASA Johnson Space Center's (JSC's) Astromaterials Research and Exploration Science (ARES) Division houses a unique combination of laboratories and other assets for conducting cutting-edge planetary research. These facilities have been accessed for decades by outside scientists; over the past five years, the 16 full time contract research and technical staff members in our division have hosted a total of 223 visiting researchers, representing 35 institutions. In order to continue to provide this level of support to the planetary sciences community, and also expand our services and collaboration within the broader scientific community, we intend to submit a proposal to NASA specifically for facilities support and establishment of our laboratories as a collective, PSAMS, Planetary Sample Analyses and Mission Science. This initiative should result in substantial cost savings to PIs with NASA funding who wish to use our facilities. Another cost saving could be realized by aggregating visiting user experiments and analyses through COMPRES, which would be of particular interest to researchers in earth and material sciences. JSC is a recognized NASA center of excellence for curation, and in future will allow PIs and mission teams easy access to samples in Curation facilities that they have been approved to study. Our curation expertise could also be used for a collection of experimental run products that could be shared and distributed to COMPRES community members. These experimental run products could range from 1 bar controlled atmosphere furnace, piston cylinder, multi-anvil, CETUS (see companion abstract), to shocked products. Coordinated analyses of samples is one of the major strengths of our division, where a single sample can be prepared with minimal destruction for a variety of chemical and structural analyses, from macro to nano-scale.
Bouzas, Lorena; Hermida, Jesús
2009-01-01
Background Although high-performance liquid chromatography (HPLC) is the method of choice for blood sirolimus determination, the microparticle enzyme immunoassay (MEIA) run on the IMx® analyser is widely used in therapeutic monitoring of this immunosuppressant agent. The aim of our study was to evaluate the possible determination of sirolimus using the fluorescence polarization immunoassay (FPIA) commercialized for everolimus quantification. Methods Sirolimus concentrations were determined in whole-blood samples from liver and kidney transplant recipients using the Innofluor® Certican® FPIA (Seradyn Inc.) run on a TDx® analyser (Abbott Laboratories), Sirolimus MEIA run on an IMx® analyser (Abbott Laboratories), and HPLC (UV detection) methods. Results The Innofluor® FPIA has a similar cross-reactivity with everolimus and sirolimus, and the within- and between-run coefficients of variation obtained for sirolimus determination were 2.7%–13.3%. In analysing different blood samples from liver and kidney transplant patients the linear regressions obtained were: FPIA = 1.12 HPLC + 0.43 (n=104, r=0.874), MEIA = 1.14 HPLC (n=146, r=0.892), and FPIA = 1.00 MEIA + 0.29 (n=106, r=0.941). Better correlation coefficients were obtained between the methods in the liver transplant samples (r≥0.900) than in the kidney transplant samples (r≥0.849). No significant effect was found for sirolimus clearance or the blood hematocrit on the relationship between the results produced by both immunoassays and HPLC. Conclusion The Innofluor® FPIA is a valid alternative with an analogous performance to the MEIA for the therapeutic monitoring of sirolimus. PMID:19242874
Impact of Educational Activities in Reducing Pre-Analytical Laboratory Errors
Al-Ghaithi, Hamed; Pathare, Anil; Al-Mamari, Sahimah; Villacrucis, Rodrigo; Fawaz, Naglaa; Alkindi, Salam
2017-01-01
Objectives Pre-analytic errors during diagnostic laboratory investigations can lead to increased patient morbidity and mortality. This study aimed to ascertain the effect of educational nursing activities on the incidence of pre-analytical errors resulting in non-conforming blood samples. Methods This study was conducted between January 2008 and December 2015. All specimens received at the Haematology Laboratory of the Sultan Qaboos University Hospital, Muscat, Oman, during this period were prospectively collected and analysed. Similar data from 2007 were collected retrospectively and used as a baseline for comparison. Non-conforming samples were defined as either clotted samples, haemolysed samples, use of the wrong anticoagulant, insufficient quantities of blood collected, incorrect/lack of labelling on a sample or lack of delivery of a sample in spite of a sample request. From 2008 onwards, multiple educational training activities directed at the hospital nursing staff and nursing students primarily responsible for blood collection were implemented on a regular basis. Results After initiating corrective measures in 2008, a progressive reduction in the percentage of non-conforming samples was observed from 2009 onwards. Despite a 127.84% increase in the total number of specimens received, there was a significant reduction in non-conforming samples from 0.29% in 2007 to 0.07% in 2015, resulting in an improvement of 75.86% (P <0.050). In particular, specimen identification errors decreased by 0.056%, with a 96.55% improvement. Conclusion Targeted educational activities directed primarily towards hospital nursing staff had a positive impact on the quality of laboratory specimens by significantly reducing pre-analytical errors. PMID:29062553
Impact of Educational Activities in Reducing Pre-Analytical Laboratory Errors: A quality initiative.
Al-Ghaithi, Hamed; Pathare, Anil; Al-Mamari, Sahimah; Villacrucis, Rodrigo; Fawaz, Naglaa; Alkindi, Salam
2017-08-01
Pre-analytic errors during diagnostic laboratory investigations can lead to increased patient morbidity and mortality. This study aimed to ascertain the effect of educational nursing activities on the incidence of pre-analytical errors resulting in non-conforming blood samples. This study was conducted between January 2008 and December 2015. All specimens received at the Haematology Laboratory of the Sultan Qaboos University Hospital, Muscat, Oman, during this period were prospectively collected and analysed. Similar data from 2007 were collected retrospectively and used as a baseline for comparison. Non-conforming samples were defined as either clotted samples, haemolysed samples, use of the wrong anticoagulant, insufficient quantities of blood collected, incorrect/lack of labelling on a sample or lack of delivery of a sample in spite of a sample request. From 2008 onwards, multiple educational training activities directed at the hospital nursing staff and nursing students primarily responsible for blood collection were implemented on a regular basis. After initiating corrective measures in 2008, a progressive reduction in the percentage of non-conforming samples was observed from 2009 onwards. Despite a 127.84% increase in the total number of specimens received, there was a significant reduction in non-conforming samples from 0.29% in 2007 to 0.07% in 2015, resulting in an improvement of 75.86% ( P <0.050). In particular, specimen identification errors decreased by 0.056%, with a 96.55% improvement. Targeted educational activities directed primarily towards hospital nursing staff had a positive impact on the quality of laboratory specimens by significantly reducing pre-analytical errors.
An integrated and accessible sample data library for Mars sample return science
NASA Astrophysics Data System (ADS)
Tuite, M. L., Jr.; Williford, K. H.
2015-12-01
Over the course of the next decade or more, many thousands of geological samples will be collected and analyzed in a variety of ways by researchers at the Jet Propulsion Laboratory (California Institute of Technology) in order to facilitate discovery and contextualize observations made of Mars rocks both in situ and here on Earth if samples are eventually returned. Integration of data from multiple analyses of samples including petrography, thin section and SEM imaging, isotope and organic geochemistry, XRF, XRD, and Raman spectrometry is a challenge and a potential obstacle to discoveries that require supporting lines of evidence. We report the development of a web-accessible repository, the Sample Data Library (SDL) for the sample-based data that are generated by the laboratories and instruments that comprise JPL's Center for Analysis of Returned Samples (CARS) in order to facilitate collaborative interpretation of potential biosignatures in Mars-analog geological samples. The SDL is constructed using low-cost, open-standards-based Amazon Web Services (AWS), including web-accessible storage, relational data base services, and a virtual web server. The data structure is sample-centered with a shared registry for assigning unique identifiers to all samples including International Geo-Sample Numbers. Both raw and derived data produced by instruments and post-processing workflows are automatically uploaded to online storage and linked via the unique identifiers. Through the web interface, users are able to find all the analyses associated with a single sample or search across features shared by multiple samples, sample localities, and analysis types. Planned features include more sophisticated search and analytical interfaces as well as data discoverability through NSF's EarthCube program.
NASA Astrophysics Data System (ADS)
Caricchi, Chiara; Baldassini, Niccolò; Di Stefano, Agata; Dinarès-Turell, Jaume; Fabbrini, Alessio; Foresi, Luca Maria; Lirer, Fabrizio; Patricolo, Simona; Sagnotti, Leonardo; Winkler, Aldo
2017-04-01
In the last two decades the Neogene Period underwent a deep chronostratigraphic revision, and several GSSPs were ratified with the exception of those of Langhian and Burdigalian stages. In particular, the Burdigalian GSSP has only been temporarily placed by Lourens et al. (2004) at 20.43 Ma, in correspondence of the First Occurrence (FO) of the calcareous nannofossil species Helicosphaera ampliaperta. In this framework, we present preliminary integrated stratigraphic studies from the Contessa quarry succession (Umbria-Marche Apennines). This well-exposed section has been sampled in the Scaglia Cinerea and Bisciaro formations, and is chronostratigraphically confined within the Aquitanian-Burdigalian time interval (Montanari et al., 1997). The sampled interval is about 18 m thick, and for the first 9 m, consists of alternating calcareous and marls nut-brown layers (Scaglia Cinerea Fm) and the upper part is made up of alternating calcareous and marls gray layers, interbedded with volcanic levels. A total of 73 oriented hand samples from different stratigraphic levels has been collected for paleomagnetic analyses, whereas 78 samples were taken for biostratigraphic studies. Paleomagnetic measurements were carried out at the laboratory of the Istituto Nazionale di Geofisica e Vulcanologia (INGV). For most of the samplings levels, pairs of standard regular specimens were cut in the laboratory. One specimen from each pair was subjected to stepwise AF demagnetization and the other "sister" specimen was subjected to thermal demagnetization. Paleomagnetic analyses have provided reliable directional data that allow the identification of a consistent sequence of magnetozones. Micropaleontological analyses were performed on the calcareous plankton content. Planktonic foraminifera and calcareous nannofossils assemblages are common to abundant. The degree of conservation is moderate to good as far as nannofossils concerns and moderate for the foraminifera content. Preliminary analyses performed on a limited number of samples, confirmed and detailed the biostratigraphic attributions reported in Montanari et al. (1997). The well exposed outcrops, the lithological cyclicity, the encouraging results from magnetostratigraphic and micropaleontological analyses, make this section suitable for high-resolution stratigraphic, cyclostratigraphic and astrochronologic studies, in the perspective of the definition of the Burdigalian GSSP.
Antidoping programme and biological monitoring before and during the 2014 FIFA World Cup Brazil
Baume, Norbert; Jan, Nicolas; Emery, Caroline; Mandanis, Béatrice; Schweizer, Carine; Giraud, Sylvain; Leuenberger, Nicolas; Marclay, François; Nicoli, Raul; Perrenoud, Laurent; Robinson, Neil; Dvorak, Jiri; Saugy, Martial
2015-01-01
Background The FIFA has implemented an important antidoping programme for the 2014 FIFA World Cup. Aim To perform the analyses before and during the World Cup with biological monitoring of blood and urine samples. Methods All qualified players from the 32 teams participating in the World Cup were tested out-of-competition. During the World Cup, 2–8 players per match were tested. Over 1000 samples were collected in total and analysed in the WADA accredited Laboratory of Lausanne. Results The quality of the analyses was at the required level as described in the WADA technical documents. The urinary steroid profiles of the players were stable and consistent with previously published papers on football players. During the competition, amphetamine was detected in a sample collected on a player who had a therapeutic use exemption for attention deficit hyperactivity disorder. The blood passport data showed no significant difference in haemoglobin values between out-of-competition and postmatch samples. Conclusions Logistical issues linked to biological samples collection, and the overseas shipment during the World Cup did not impair the quality of the analyses, especially when used as the biological passport of football players. PMID:25878079
Summary and Preliminary Interpretation of Tritium and Dissolved Noble Gas Data from Site 300
DOE Office of Scientific and Technical Information (OSTI.GOV)
Visser, A.; Singleton, M.; Madrid, V.
2014-01-29
In October 2013, groundwater samples were collected from 10 wells from Site 300 and analyzed by the Environmental Radiochemistry Laboratory at Lawrence Livermore National Laboratory (LLNL). Groundwater samples were analyzed for groundwater age tracers: tritium, the helium isotope ratio of dissolved helium and the concentrations of dissolved noble gases (Helium, Neon, Argon, Krypton, and Xenon). A subset of the samples was also analyzed for excess nitrogen due to saturated zone denitrification. The age-dating data were used to evaluate the degree to which groundwater at a particular monitoring well was derived from pre-modern and/or modern sources. More specifically, the analyses canmore » be used to determine whether the recharge age of the groundwater beneath the site pre-dates anthropogenic activities at the site.« less
Pradhan, Ajay; Ivarsson, Per; Ragnvaldsson, Daniel; Berg, Håkan; Jass, Jana; Olsson, Per-Erik
2017-04-15
Metals released into the environment continue to be of concern for human health. However, risk assessment of metal exposure is often based on total metal levels and usually does not take bioavailability data, metal speciation or matrix effects into consideration. The continued development of biological endpoint analyses are therefore of high importance for improved eco-toxicological risk analyses. While there is an on-going debate concerning synergistic or additive effects of low-level mixed exposures there is little environmental data confirming the observations obtained from laboratory experiments. In the present study we utilized qRT-PCR analysis to identify key metal response genes to develop a method for biomonitoring and risk-assessment of metal pollution. The gene expression patterns were determined for juvenile zebrafish exposed to waters from sites down-stream of a closed mining operation. Genes representing different physiological processes including stress response, inflammation, apoptosis, drug metabolism, ion channels and receptors, and genotoxicity were analyzed. The gene expression patterns of zebrafish exposed to laboratory prepared metal mixes were compared to the patterns obtained with fish exposed to the environmental samples with the same metal composition and concentrations. Exposure to environmental samples resulted in fewer alterations in gene expression compared to laboratory mixes. A biotic ligand model (BLM) was used to approximate the bioavailability of the metals in the environmental setting. However, the BLM results were not in agreement with the experimental data, suggesting that the BLM may be overestimating the risk in the environment. The present study therefore supports the inclusion of site-specific biological analyses to complement the present chemical based assays used for environmental risk-assessment. Copyright © 2017 Elsevier B.V. All rights reserved.
Hill, Virginia; Cairns, Thomas; Schaffer, Michael
2008-03-21
Hair samples were contaminated by rubbing with cocaine (COC) followed by sweat application, multiple shampoo treatments and storage. The samples were then washed with isopropanol for 15min, followed by sequential aqueous washes totaling 3.5h. The amount of drug in the last wash was used to calculate a wash criterion to determine whether samples were positive due to use or contamination. Analyses of cocaine and metabolites were done by LC/MS/MS. These procedures were applied to samples produced by a U.S. government-sponsored cooperative study, in which this laboratory participated, and to samples in a parallel in-house study. All contaminated samples in both studies were correctly identified as contaminated by cutoff, benzoylecgonine (BE) presence, BE ratio, and/or the wash criterion. A method for determining hair porosity was applied to samples in both studies, and porosity characteristics of hair are discussed as they relate to experimental and real-world contamination of hair, preparation of proficiency survey samples, and analysis of unknown hair samples.
To mix or not to mix venous blood samples collected in vacuum tubes?
Parenmark, Anna; Landberg, Eva
2011-09-08
There are recommendations to mix venous blood samples by inverting the tubes immediately after venipuncture. Though mixing allows efficient anticoagulation in plasma tubes and fast initiation of coagulation in serum tubes, the effect on laboratory analyses and risk of haemolysis has not been thoroughly evaluated. Venous blood samples were collected by venipuncture in vacuum tubes from 50 patients (10 or 20 patients in each group). Four types of tubes and 18 parameters used in routine clinical chemistry were evaluated. For each patient and tube, three types of mixing strategies were used: instant mixing, no mixing and 5 min of rest followed by mixing. Most analyses did not differ significantly in samples admitted to different mixing strategies. Plasma lactate dehydrogenase and haemolysis index showed a small but significant increase in samples omitted to instant mixing compared to samples without mixing. However, in one out of twenty non-mixed samples, activated partial thromboplastin time was seriously affected. These results indicate that mixing blood samples after venipuncture is not mandatory for all types of tubes. Instant mixing may introduce interference for those analyses susceptible to haemolysis. However, tubes with liquid-based citrate buffer for coagulation testing should be mixed to avoid clotting.
Light Scattering based detection of food pathogens
USDA-ARS?s Scientific Manuscript database
The current methods for detecting foodborne pathogens are mostly destructive (i.e., samples need to be pretreated), and require time, personnel, and laboratories for analyses. Optical methods including light scattering based techniques have gained a lot of attention recently due to its their rapid a...
Tank 241-T-204, core 188 analytical results for the final report
DOE Office of Scientific and Technical Information (OSTI.GOV)
Nuzum, J.L.
TANK 241-T-204, CORE 188, ANALYTICAL RESULTS FOR THE FINAL REPORT. This document is the final laboratory report for Tank 241 -T-204. Push mode core segments were removed from Riser 3 between March 27, 1997, and April 11, 1997. Segments were received and extruded at 222-8 Laboratory. Analyses were performed in accordance with Tank 241-T-204 Push Mode Core Sampling and analysis Plan (TRAP) (Winkleman, 1997), Letter of instruction for Core Sample Analysis of Tanks 241-T-201, 241- T-202, 241-T-203, and 241-T-204 (LAY) (Bell, 1997), and Safety Screening Data Qual@ Objective (DO) ODukelow, et al., 1995). None of the subsamples submitted for totalmore » alpha activity (AT) or differential scanning calorimetry (DC) analyses exceeded the notification limits stated in DO. The statistical results of the 95% confidence interval on the mean calculations are provided by the Tank Waste Remediation Systems Technical Basis Group and are not considered in this report.« less
Vigliar, E; Malapelle, U; Bellevicine, C; de Luca, C; Troncone, G
2015-10-01
Guidelines from the College of American Pathologists (CAP), the International Association for the Study of Lung Cancer (IASLC) and the Association for Molecular Pathology (AMP) consider cytology suitable for testing epidermal growth factor receptor (EGFR) mutations in lung adenocarcinoma. The guidelines recommend that cytopathologists first discuss the possibility of testing squamous cell carcinomas (SqCC) in multidisciplinary meetings. Second, cell blocks should be analysed rather than smear preparations and, third, specimens should be sent to external molecular laboratories within three working days of receiving requests. This study monitored how these recommendations are met in practice. Our laboratory received 596 requests from cytologists from 13 different institutions. For each case, the cytological diagnosis, cytopreparation type, and time between the request and sample mailing were compared with the recommendations. Of the 596 samples, 32 (5.4%) had been reported as SqCC. Three of these (9.4%) showed EGFR mutation. Cytological slides, either ThinPrep(™) (51.2%) or direct smears (43.2%), were more frequently received than cell blocks (5.7%). The mean time between the oncologist's request and specimen dispatching was 5.8 working days. The occurrence of mutations in samples reported as SqCC was higher than expected. This questions the reliability of the original diagnosis, which reinforced the recommendation to evaluate the opportunity for testing non-adenocarcinoma cytology on a case-by-case basis. In spite of CAP/IASLC/AMP recommendations, cell blocks were underutilized for EGFR testing, but cytological slides were suitable for DNA analyses. Significant efforts are needed to avoid delays in outsourcing cytological samples for EGFR testing. © 2014 John Wiley & Sons Ltd.
Forensic validation of the SNPforID 52-plex assay.
Musgrave-Brown, Esther; Ballard, David; Balogh, Kinga; Bender, Klaus; Berger, Burkhard; Bogus, Magdalena; Børsting, Claus; Brion, María; Fondevila, Manuel; Harrison, Cheryl; Oguzturun, Ceylan; Parson, Walther; Phillips, Chris; Proff, Carsten; Ramos-Luis, Eva; Sanchez, Juan J; Sánchez Diz, Paula; Sobrino Rey, Bea; Stradmann-Bellinghausen, Beate; Thacker, Catherine; Carracedo, Angel; Morling, Niels; Scheithauer, Richard; Schneider, Peter M; Syndercombe Court, Denise
2007-06-01
The advantages of single nucleotide polymorphism (SNP) typing in forensic genetics are well known and include a wider choice of high-throughput typing platforms, lower mutation rates, and improved analysis of degraded samples. However, if SNPs are to become a realistic supplement to current short tandem repeat (STR) typing methods, they must be shown to successfully and reliably analyse the challenging samples commonly encountered in casework situations. The European SNPforID consortium, supported by the EU GROWTH programme, has developed a multiplex of 52 SNPs for forensic analysis, with the amplification of all 52 loci in a single reaction followed by two single base extension (SBE) reactions which are detected with capillary electrophoresis. In order to validate this assay, a variety of DNA extracts were chosen to represent problems such as low copy number and degradation that are commonly seen in forensic casework. A total of 40 extracts were used in the study, each of which was sent to two of the five participating laboratories for typing in duplicate or triplicate. Laboratories were instructed to carry out their analyses as if they were dealing with normal casework samples. Results were reported back to the coordinating laboratory and compared with those obtained from traditional STR typing of the same extracts using Powerplex 16 (Promega). These results indicate that, although the ability to successfully type good quality, low copy number extracts is lower, the 52-plex SNP assay performed better than STR typing on degraded samples, and also on samples that were both degraded and of limited quantity, suggesting that SNP analysis can provide advantages over STR analysis in forensically relevant circumstances. However, there were also additional problems arising from contamination and primer quality issues and these are discussed.
Performance evaluation of the Arkray Adams HA-8160 HbA1c analyser.
Thevarajah, T Malathi; Nani, Nordin; Chew, Y Y
2008-12-01
HbA1c measurement is currently routinely used to predict long term outcome of diabetes, thus playing a fundamental role in the management of diabetes. The relationship between HbA1c value and long term diabetic complications has been established by a randomised control Diabetes Control and Complications Trial (DCCT) which used high performance liquid chromatography (HPLC) as a reference method for HbA1c assay. To ensure that HbA1c results from a variety HbA1c assay methods are similar to the DCCT values, the American Diabetes Association (ADA) recommended that all laboratories should use methods certified by the National Glycohemoglobin Standardization Programme (NGSP) with interassay coefficient variation (CV) of < 5% (ideally < 3%). The International Federation of Clinical Chemistry (IFCC) working group on HbA1c standardisation has set a CV < 2.5% as a criteria for its reference laboratories. To evaluate the performance of Arkray Adams HA-8160 HbA1c analyser which uses a cation exchange HPLC method and its correlation to HbA1c assay on Cobas Integra 800 which is an immunoturbidimetric method. For the imprecision study, patient samples and control material of two levels were analysed on HA-8160 analyser 20 times in a single run (within-run imprecision) and twice a day on five consecutive days (between-run imprecision). For the recovery study, two samples each with high and low values were selected and mixed in ratios of 1:3, 1:1 and 3:1, and were analysed by HA-8160. Sixty samples were analysed by both Cobas Integra 800 and HA-8160 for method comparison study. Ten uraemic samples and ten thalassaemic samples were assayed on Cobas Integra 800 and HA 8160 for interference study. Within-run CVs were 0.6% and 0.7% for medium and high value samples respectively, 0.6% and 0.7% for low and high level controls respectively. Between-run CVs were 0.5% and 0.4% for medium and high value samples respectively, 0.5% and 0.6% for low and high level controls respectively. The mean recovery was 100.1%. A good correlation between the 2 methods (Adams = 1.00 Cobas - 0.11, r = 0.98) was observed. The Akray Adams HA-8160 HbA1c analyser performed within the target CV of < 2.5% and showed a good correlation with the Cobas Integra 800.
NASA Technical Reports Server (NTRS)
Sutter, B.; McAdam, A. C.; Rampe, E. B.; Thompson, L. M.; Ming, D. W.; Mahaffy, P. R.; Navarro-Gonzalez, R.; Stern, J. C.; Eigenbrode, J. L.; Archer, P. D.
2017-01-01
The Sample Analysis at Mars (SAM) instrument aboard the Mars Science Laboratory rover has analyzed 13 samples from Gale Crater. All SAM-evolved gas analyses have yielded a multitude of volatiles (e.g., H2O, SO2, H2S, CO2, CO, NO, O2, HCl) [1- 6]. The objectives of this work are to 1) Characterize recent evolved SO2, CO2, O2, and NO gas traces of the Murray formation mudstone, 2) Constrain sediment mineralogy/composition based on SAM evolved gas analysis (SAM-EGA), and 3) Discuss the implications of these results relative to understanding the geological history of Gale Crater.
Analysis of laboratory compaction methods of roller compacted concrete
NASA Astrophysics Data System (ADS)
Trtík, Tomáš; Chylík, Roman; Bílý, Petr; Fládr, Josef
2017-09-01
Roller-Compacted Concrete (RCC) is an ordinary concrete poured and compacted with machines typically used for laying of asphalt road layers. One of the problems connected with this technology is preparation of representative samples in the laboratory. The aim of this work was to analyse two methods of preparation of RCC laboratory samples with bulk density as the comparative parameter. The first method used dynamic compaction by pneumatic hammer. The second method of compaction had a static character. The specimens were loaded by precisely defined force in laboratory loading machine to create the same conditions as during static rolling (in the Czech Republic, only static rolling is commonly used). Bulk densities obtained by the two compaction methods were compared with core drills extracted from real RCC structure. The results have shown that the samples produced by pneumatic hammer tend to overestimate the bulk density of the material. For both compaction methods, immediate bearing index test was performed to verify the quality of compaction. A fundamental difference between static and dynamic compaction was identified. In static compaction, initial resistance to penetration of the mandrel was higher, after exceeding certain limit the resistance was constant. This means that the samples were well compacted just on the surface. Specimens made by pneumatic hammer actively resisted throughout the test, the whole volume was uniformly compacted.
Reliability of the MODS assay decentralisation process in three health regions in Peru
Mendoza, A.; Castillo, E.; Gamarra, N.; Huamán, T.; Perea, M.; Monroi, Y.; Salazar, R.; Coronel, J.; Acurio, M.; Obregón, G.; Roper, M.; Bonilla, C.; Asencios, L.; Moore, D. A. J.
2011-01-01
OBJECTIVE To deliver rapid isoniazid (INH) and rifampicin (RMP) drug susceptibility testing (DST) close to the patient, we designed a decentralisation process for the microscopic observation drug susceptibility (MODS) assay in Peru and evaluated its reliability. METHODS After 2 weeks of training, laboratory staff processed ≥120 consecutive sputum samples each in three regional laboratories. Samples were processed in parallel with MODS testing at an expert laboratory. Blinded paired results were independently analysed by the Instituto Nacional de Salud (INS) according to predetermined criteria: concordance for culture, DST against INH and RMP and diagnosis of multidrug-resistant t uberculosis (MDR-TB) ≥ 95%, McNemar's P > 0.05, kappa index (κ) ≥ 0.75 and contamination 1–4%. Sensitivity and specificity for MDR-TB were calculated. RESULTS The accreditation process for Callao (126 samples, 79.4% smear-positive), Lima Sur (n = 130, 84%) and Arequipa (n = 126, 80%) took respectively 94, 97 and 173 days. Pre-determined criteria in all regional laboratories were above expected values. The sensitivity and specificity for detecting MDR-TB in regional laboratories were >95%, except for sensitivity in Lima Sur, which was 91.7%. Contamination was 1.0–2.3%. Mean delay to positive MODS results was 9.9–12.9 days. CONCLUSION Technology transfer of MODS was reliable, effective and fast, enabling the INS to accredit regional laboratories swiftly. PMID:21219684
National audit of cerebrospinal fluid testing.
Holbrook, Ian; Beetham, Robert; Cruickshank, Anne; Egner, William; Fahie-Wilson, Mike; Keir, Geoff; Patel, Dina; Watson, Ian; White, Peter
2007-09-01
UK National External Quality Assessment Service (NEQAS) Specialist Advisory Group for EQA of CSF Proteins and Biochemistry was interested in current practice for the biochemical investigation of cerebrospinal fluid (CSF) in the UK. A questionnaire was sent to laboratories via regional audit committees and the results collated. Most laboratories were analysing CSF in a satisfactory manner. There was some variation in the reference ranges used for glucose, protein and lactate. There was concern about the rejection policies of some laboratories on these unrepeatable samples and the wavelengths used to measure bilirubin. The survey revealed the lack of spectrophotometric scanning for haem pigments and bilirubin in some hospitals. The current practice for the measurement of CSF samples in the UK is satisfactory in most laboratories responding to the questionnaire. National agreement on reference ranges for glucose, protein and lactate should be achievable. Those performing spectrophotometric scanning of the CSF were doing so in concordance with the national guidelines. Some hospitals in the UK may not have responded to the questionnaire because they did not offer spectrophotometric scanning.
DOE Office of Scientific and Technical Information (OSTI.GOV)
None
Volume II of the Site Environmental Report for 2006 is provided by Ernest Orlando Lawrence Berkeley National Laboratory as a supplemental appendix to Volume I, which contains the body of the report. Volume II contains the environmental monitoring and sampling data used to generate summary results of routine and nonroutine activities at the Laboratory (except for groundwater sampling data, which may be found in the reports referred to in Chapter 4). Volume I summarizes the results from analyses of the data. The results from sample collections are more comprehensive in Volume II than in Volume I: For completeness, all resultsmore » from sample collections that began or ended in calendar year (CY) 2006 are included in this volume. However, the samples representing CY 2005 data have not been used in the summary results that are reported in Volume I. (For example, although ambient air samples collected on January 2, 2006, are presented in Volume II, they represent December 2005 data and are not included in Table 4-2 in Volume I.)« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Wood, T.R.; Knight, J.L.; Hertzler, C.L.
1989-08-01
Sampling of the Test Reactor Area (TRA) Paint Shop Ditch at the Idaho National Engineering Laboratory was initiated in compliance with the Interim Agreement between the Department of Energy (DOE) and the Environmental Protection Agency (EPA). Sampling of the TRA Paint Shop Ditch was done as part of the Action Plan to achieve and maintain compliance with the Resource Conservation and Recovery Act (RCRA) and applicable regulations. It is the purpose of this document to provide a summary of the July 6, 1987 sampling activities that occurred in ditch west of Building TRA-662, which housed the TRA Paint Shop inmore » 1987. This report will give a narrative description of the field activities, locations of collected samples, discuss the sampling procedures and the chemical analyses. Also included in the scope of this report is to bring together data and reports on the TRA Paint Shop Ditch for archival purposes. 6 refs., 10 figs., 8 tabs.« less
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.
1988-12-01
and do not refer to monitoring zones at McClellSn AFB. b Priority poLutant metals analyses also included U.S. EPA Methods 206.2, 245.1 and 270.2. EW a...sampling protocol, and the laboratory is audited routinely. Therefore, no corrective action other than good training and supervision is necessary. The same
DOE Office of Scientific and Technical Information (OSTI.GOV)
Peters, T. B.
2013-02-26
Savannah River National Laboratory (SRNL) performed experiments on qualification material for use in the Integrated Salt Disposition Program (ISDP) Batch 6 processing. As part of this qualification work, SRNL performed an Actinide Removal Process (ARP) test. From this test, the residual monosodium titanate (MST) was analyzed for radionuclide uptake. The results of these analyses are reported and are within historical precedent.
Brumbaugh, William G.; Hammerschmidt, Chad R.; Zanella, Luciana; Rogevich, Emily; Salata, Gregory; Bolek, Radoslaw
2011-01-01
An interlaboratory comparison of acid-volatile sulfide (AVS) and simultaneously extracted nickel (SEM_Ni) measurements of sediments was conducted among five independent laboratories. Relative standard deviations for the seven test samples ranged from 5.6 to 71% (mean = 25%) for AVS and from 5.5 to 15% (mean = 10%) for SEM_Ni. These results are in stark contrast to a recently published study that indicated AVS and SEM analyses were highly variable among laboratories.
NASA Astrophysics Data System (ADS)
Bertrand, Marylène; Chabin, Annie; Colas, Cyril; Cadène, Martine; Chaput, Didier; Brack, Andre; Cottin, Herve
2015-01-01
In order to confirm the results of previous experiments concerning the chemical behaviour of organic molecules in the space environment, organic molecules (amino acids and a dipeptide) in pure form and embedded in meteorite powder were exposed in the AMINO experiment in the EXPOSE-R facility onboard the International Space Station. After exposure to space conditions for 24 months (2843 h of irradiation), the samples were returned to the Earth and analysed in the laboratory for reactions caused by solar ultraviolet (UV) and other electromagnetic radiation. Laboratory UV exposure was carried out in parallel in the Cologne DLR Center (Deutsches Zentrum für Luft und Raumfahrt). The molecules were extracted from the sample holder and then (1) derivatized by silylation and analysed by gas chromatography coupled to a mass spectrometer (GC-MS) in order to quantify the rate of degradation of the compounds and (2) analysed by high-resolution mass spectrometry (HRMS) in order to understand the chemical reactions that occurred. The GC-MS results confirm that resistance to irradiation is a function of the chemical nature of the exposed molecules and of the wavelengths of the UV light. They also confirm the protective effect of a coating of meteorite powder. The most altered compounds were the dipeptides and aspartic acid while the most robust were compounds with a hydrocarbon chain. The MS analyses document the products of reactions, such as decarboxylation and decarbonylation of aspartic acid, taking place after UV exposure. Given the universality of chemistry in space, our results have a broader implication for the fate of organic molecules that seeded the planets as soon as they became habitable as well as for the effects of UV radiation on exposed molecules at the surface of Mars, for example.
Parés-Pollán, L; Gonzalez-Quintana, A; Docampo-Cordeiro, J; Vargas-Gallego, C; García-Álvarez, G; Ramos-Rodríguez, V; Diaz Rubio-García, M P
2014-01-01
Owing to the decrease in values of biochemical glucose parameter in some samples from external extraction centres, and the risk this implies to patient safety; it was decided to apply an adaptation of the «Health Services Failure Mode and Effects Analysis» (HFMEA) to manage risk during the pre-analytical phase of sample transportation from external centres to clinical laboratories. A retrospective study of glucose parameter was conducted during two consecutive months. The analysis was performed in its different phases: to define the HFMEA topic, assemble the team, graphically describe the process, conduct a hazard analysis, design the intervention and indicators, and identify a person to be responsible for ensuring completion of each action. The results of glucose parameter in one of the transport routes, were significantly lower (P=.006). The errors and potential causes of this problem were analysed, and criteria of criticality and detectability were applied (score≥8) in the decision tree. It was decided to: develop a document management system; reorganise extractions and transport routes in some centres; quality control of the sample container ice-packs, and the time and temperature during transportation. This work proposes quality indicators for controlling time and temperature of transported samples in the pre-analytical phase. Periodic review of certain laboratory parameters can help to detect problems in transporting samples. The HFMEA technique is useful for the clinical laboratory. Copyright © 2013 SECA. Published by Elsevier Espana. All rights reserved.
USDA-ARS?s Scientific Manuscript database
Quantification of soil physical properties through soil sampling and laboratory analyses is time-, cost-, and labor-consuming, making it difficult to obtain the spatially-dense data required for precision agriculture. Proximal soil sensing is an attractive alternative, but many currently available s...
Shelton, Larry R.
1994-01-01
The U.S. Geological Survey's National Water-Quality Assessment program includes extensive data- collection efforts to assess the quality of the Nations's streams. These studies require analyses of stream samples for major ions, nutrients, sediments, and organic contaminants. For the information to be comparable among studies in different parts of the Nation, consistent procedures specifically designed to produce uncontaminated samples for trace analysis in the laboratory are critical. This field guide describes the standard procedures for collecting and processing samples for major ions, nutrients, organic contaminants, sediment, and field analyses of conductivity, pH, alkalinity, and dissolved oxygen. Samples are collected and processed using modified and newly designed equipment made of Teflon to avoid contamination, including nonmetallic samplers (D-77 and DH-81) and a Teflon sample splitter. Field solid-phase extraction procedures developed to process samples for organic constituent analyses produce an extracted sample with stabilized compounds for more accurate results. Improvements to standard operational procedures include the use of processing chambers and capsule filtering systems. A modified collecting and processing procedure for organic carbon is designed to avoid contamination from equipment cleaned with methanol. Quality assurance is maintained by strict collecting and processing procedures, replicate sampling, equipment blank samples, and a rigid cleaning procedure using detergent, hydrochloric acid, and methanol.
A computer program for geochemical analysis of acid-rain and other low-ionic-strength, acidic waters
Johnsson, P.A.; Lord, D.G.
1987-01-01
ARCHEM, a computer program written in FORTRAN 77, is designed primarily for use in the routine geochemical interpretation of low-ionic-strength, acidic waters. On the basis of chemical analyses of the water, and either laboratory or field determinations of pH, temperature, and dissolved oxygen, the program calculates the equilibrium distribution of major inorganic aqueous species and of inorganic aluminum complexes. The concentration of the organic anion is estimated from the dissolved organic concentration. Ionic ferrous iron is calculated from the dissolved oxygen concentration. Ionic balances and comparisons of computed with measured specific conductances are performed as checks on the analytical accuracy of chemical analyses. ARCHEM may be tailored easily to fit different sampling protocols, and may be run on multiple sample analyses. (Author 's abstract)
NASA Astrophysics Data System (ADS)
Danielson, L. R.; Draper, D. S.
2016-12-01
NASA Johnson Space Center's (JSC) Astromaterials Research and Exploration Science Division houses a unique combination of laboratories and other assets for conducting cutting-edge planetary research. These facilities have been accessed for decades by outside scientists; over the past five years, the 16 full time contract research and technical staff members in our division have hosted a total of 223 visiting researchers, representing 35 institutions. We intend to submit a proposal to NASA specifically for facilities support and establishment of our laboratories as a collective, PSAMS, Planetary Sample Analyses and Mission Science, which should result in substantial cost savings to PIs who wish to use our facilities. JSC is a recognized NASA center of excellence for curation, and in future will allow PIs easy access to samples in Curation facilities that they have been approved to study. Our curation expertise could also be used for a collection of experimental run products and standards that could be shared and distributed to community members, products that could range from 1 bar controlled atmosphere furnace, piston cylinder, multi-anvil, to shocked products. Coordinated analyses of samples is one of the major strengths of our division, where a single sample can be prepared with minimal destruction for a variety of chemical and structural analyses, from macro to nano-scale. A CT scanner will be delivered August 2016 and installed in the same building as all the other division experimental and analytical facilities, allowing users to construct a 3 dimensional model of their run product and/or starting material before any destruction of their sample for follow up analyses. The 3D printer may also be utilized to construct containers for diamond anvil cell experiments. Our staff scientists will work with PIs to maximize science return and serve the needs of the community. We welcome student visitors, and a graduate semester internship is available through Jacobs.
NASA Astrophysics Data System (ADS)
Egartner, Isabel; Sass, Oliver
2016-04-01
The presented investigation is part of a longer-term project which deals with the influence of salt and moisture on weathering of historic stonework. The main investigation object in the field is a part of the 300 hundred year old boundary wall of the Worchester College in Oxford, UK. A range of non-destructive techniques were applied in course of field campaigns, e.g. mapping of weathering phenomena; handheld moisture sensors; and salt sampling by paper pulp poultices. In a second step we investigated the behaviour and distribution of water and salt solution in a porous material, similar to the limestone of the College wall, under laboratory condititions. Limestone cube samples (5x5x5 cm) were soaked first with ultrapure H2O and second with different concentration of saline solutions of NaCl and Na2SO4. During the dehydration process of the stone cubes a multi-method approach including sampling by drilling, paper pulp poultices, handheld moisture sensor, conductivity sensor and Ion Chromatography (IC) were applied to investigate the moisture and salt content and distribution within the samples. The laboratory analyses were carried out at the department of applied geoscience of the Technical University of Graz, Austria. The main aim was to investigate the effectivity of the paper pulp poultices in soaking up salts from the stone samples and to use the results of the laboratory analysis to interpret and calibrate the field work results from the College wall in Oxford. Keywords: Salt weathering, paper pulp poultices, cultural heritage, field work and laboratory investigation
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.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Hertzler, C.L.; Poloski, J.P.; Bates, R.A.
1988-01-01
The Compliance Program Data Management System (DMS) developed at the Idaho National Engineering Laboratory (INEL) validates and maintains the integrity of data collected to support the Consent Order and Compliance Agreement (COCA) between the INEL and the Environmental Protection Agency (EPA). The system uses dBase III Plus programs and dBase III Plus in an interactive mode to enter, store, validate, manage, and retrieve analytical information provided on EPA Contract Laboratory Program (CLP) forms and CLP forms modified to accommodate 40 CFR 264 Appendix IX constituent analyses. Data analysis and presentation is performed utilizing SAS, a statistical analysis software program. Archivingmore » of data and results is performed at appropriate stages of data management. The DMS is useful for sampling and analysis programs where adherence to EPA CLP protocol, along with maintenance and retrieval of waste site investigation sampling results is desired or requested. 3 refs.« less
Grimmett, Paul E; Munch, Jean W
2009-01-01
1,4-Dioxane has been identified as a probable human carcinogen and an emerging contaminant in drinking water. The United States Environmental Protection Agency's (U.S. EPA) National Exposure Research Laboratory (NERL) has developed a method for the analysis of 1,4-dioxane in drinking water at ng/L concentrations. The method consists of an activated carbon solid-phase extraction of 500-mL or 100-mL water samples using dichloromethane as the elution solvent. The extracts are analyzed by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. In the NERL laboratory, recovery of 1,4-dioxane ranged from 94-110% in fortified laboratory reagent water and recoveries of 96-102% were demonstrated for fortified drinking water samples. The relative standard deviations for replicate analyses were less than 6% at concentrations exceeding the minimum reporting level.
Gemas: issues from the comparison of aqua regia and X-ray fluorescence results
NASA Astrophysics Data System (ADS)
Dinelli, Enrico; Birke, Manfred; Reimann, Clemens; Demetriades, Alecos; DeVivo, Benedetto; Flight, Dee; Ladenberger, Anna; Albanese, Stefano; Cicchella, Domenico; Lima, Annamaria
2014-05-01
The comparison of analytical results from aqua regia (AR) and X-ray fluorescence spectroscopy (XRF) can provide information on soil processes controlling the element distribution. The GEMAS (GEochemical Mapping of Agricultural and grazing land Soils) agricultural soil database is used for this comparison. Analyses for the same suite of elements and parameters were carried out in the same laboratory under strict quality control procedures. Sample preparation has been conducted at the laboratory of the The comparison of analytical results from aqua regia (AR) and X-ray fluorescence spectroscopy (XRF) can provide information on soil processes controlling the element distribution in soil. The GEMAS (GEochemical Mapping of Agricultural and grazing land Soils) agricultural soil database, consisting of 2 x ca. 2100 samples spread evenly over 33 European countries, is used for this comparison. Analyses for the same suite of elements and parameters were carried out in the same laboratory under strict quality control procedures. Sample preparation has been conducted at the laboratory of the Geological Survey of the Slovak Republic, AR analyses were carried out at ACME Labs, and XRF analyses at the Federal Institute for Geosciences and Natural Resources, Germany Element recovery by AR is very different, ranging from <1% (e.g. Na, Zr) to > 80% (e.g. Mn, P, Co). Recovery is controlled by mineralogy of the parent material, but geographic and climatic factors and the weathering history of the soils are also important. Nonetheless, even the very low recovery elements show wide ranges of variation and spatial patterns that are affected by other factors than soil parent material. For many elements soil pH have a clear influence on AR extractability: under acidic soil conditions almost all elements tend to be leached and their extractability is generally low. It progressively increases with increasing pH and is highest in the pH range 7-8. Critical is the clay content of the soil that almost for all elements correspond to higher extractability with increasing clay abundance. Also other factors such as organic matter content of soil, Fe and Mn occurrence are important for certain elements or in selected areas. This work illustrates that there are significant differences in the extractability of elements from soils and addresses important influencing factors related to soil properties, geology, climate.
Gostic, T; Klemenc, S
2007-07-04
An abandoned clandestine laboratory was seized in Slovenia. All confiscated exhibits were analysed in a forensic laboratory, where the following analytical methods were applied: capillary gas chromatography coupled with mass spectrometry (GC-MS) combined also by solid-phase micro extraction (SPME) and pyrolysis (Py) technique, Fourier transform infrared spectrometry (FTIR) and scanning electron microscopy with energy dispersive X-ray detector (SEM-EDX). The most interesting analytical findings can be summarised as follows: at the crime scene some plastic pieces, which contained cocaine dissolved (as solid solution) in polymethyl methacrylate-plexiglass (PMMA), were found. The highest cocaine concentration measured in the plastic sample was about 15% by weight. Two larger lumps of material (12 and 3 kg) were composed mainly of PMMA and CaCO3 and contained only 0.4 and 0.5% of cocaine, respectively. As for the low cocaine concentration, we assume that those two lumps of material represent discarded waste product--residue after the isolation of cocaine from plastic. Higher quantities of pure solvents (41 l) and solvent mixtures (87 l) were seized. We identified three types of pure solvents (acetone, gasoline and benzine) and two different types of solvent mixtures (benzine/acetone and gasoline/acetone). The total seized volume (87 l) of solvent mixtures holds approximately 395 g of solid residue formed mainly of PMMA and cocaine. Obviously solvent mixtures were used for isolation of cocaine from the plastic. Small quantities of relatively pure cocaine base were identified on different objects. There were two cotton sheets, most probably used for filtration. One sheet had traces of cocaine base (76% purity) on the surface, while cocaine in hydrochloride form (96%) was identified on the other sheet. GC-MS analyses of micro traces isolated from analytical balances showed the presence of cocaine and some common adulterants: phenacetine, lidocaine and procaine. A cocaine sample compressed in the shape of block was also seized. The above analytical findings inferred us to the conclusion that the illicit laboratory was used for the isolation of cocaine from PMMA resin. Further more, analyses confirm that not only isolation but also further manipulation of cocaine, i.e. adulteration/dilution, as well as the formation of cocaine blocks took place in the house. The information obtained through analyses also allowed us to make some hypotheses about possible multistage isolation procedure.
Mahajan, Prashant; Kuppermann, Nathan; Suarez, Nicolas; Mejias, Asuncion; Casper, Charlie; Dean, J Michael; Ramilo, Octavio
2015-01-01
To develop the infrastructure and demonstrate the feasibility of conducting microarray-based RNA transcriptional profile analyses for the diagnosis of serious bacterial infections in febrile infants 60 days and younger in a multicenter pediatric emergency research network. We designed a prospective multicenter cohort study with the aim of enrolling more than 4000 febrile infants 60 days and younger. To ensure success of conducting complex genomic studies in emergency department (ED) settings, we established an infrastructure within the Pediatric Emergency Care Applied Research Network, including 21 sites, to evaluate RNA transcriptional profiles in young febrile infants. We developed a comprehensive manual of operations and trained site investigators to obtain and process blood samples for RNA extraction and genomic analyses. We created standard operating procedures for blood sample collection, processing, storage, shipping, and analyses. We planned to prospectively identify, enroll, and collect 1 mL blood samples for genomic analyses from eligible patients to identify logistical issues with study procedures. Finally, we planned to batch blood samples and determined RNA quantity and quality at the central microarray laboratory and organized data analysis with the Pediatric Emergency Care Applied Research Network data coordinating center. Below we report on establishment of the infrastructure and the feasibility success in the first year based on the enrollment of a limited number of patients. We successfully established the infrastructure at 21 EDs. Over the first 5 months we enrolled 79% (74 of 94) of eligible febrile infants. We were able to obtain and ship 1 mL of blood from 74% (55 of 74) of enrolled participants, with at least 1 sample per participating ED. The 55 samples were shipped and evaluated at the microarray laboratory, and 95% (52 of 55) of blood samples were of adequate quality and contained sufficient RNA for expression analysis. It is possible to create a robust infrastructure to conduct genomic studies in young febrile infants in the context of a multicenter pediatric ED research setting. The sufficient quantity and high quality of RNA obtained suggests that whole blood transcriptional profile analysis for the diagnostic evaluation of young febrile infants can be successfully performed in this setting.
Lermen, Dominik; Schmitt, Daniel; Bartel-Steinbach, Martina; Schröter-Kermani, Christa; Kolossa-Gehring, Marike; von Briesen, Hagen; Zimmermann, Heiko
2014-01-01
Technical progress has simplified tasks in lab diagnosis and improved quality of test results. Errors occurring during the pre-analytical phase have more negative impact on the quality of test results than errors encountered during the total analytical process. Different infrastructures of sampling sites can highly influence the quality of samples and therewith of analytical results. Annually the German Environmental Specimen Bank (ESB) collects, characterizes, and stores blood, plasma, and urine samples of 120–150 volunteers each on four different sampling sites in Germany. Overarching goal is to investigate the exposure to environmental pollutants of non-occupational exposed young adults combining human biomonitoring with questionnaire data. We investigated the requirements of the study and the possibility to realize a highly standardized sampling procedure on a mobile platform in order to increase the required quality of the pre-analytical phase. The results lead to the development of a mobile epidemiologic laboratory (epiLab) in the project “Labor der Zukunft” (future’s lab technology). This laboratory includes a 14.7 m2 reception area to record medical history and exposure-relevant behavior, a 21.1 m2 examination room to record dental fillings and for blood withdrawal, a 15.5 m2 biological safety level 2 laboratory to process and analyze samples on site including a 2.8 m2 personnel lock and a 3.6 m2 cryofacility to immediately freeze samples. Frozen samples can be transferred to their final destination within the vehicle without breaking the cold chain. To our knowledge, we herewith describe for the first time the implementation of a biological safety laboratory (BSL) 2 lab and an epidemiologic unit on a single mobile platform. Since 2013 we have been collecting up to 15.000 individual human samples annually under highly standardized conditions using the mobile laboratory. Characterized and free of alterations they are kept ready for retrospective analyses in their final archive, the German ESB. PMID:25141120
Lermen, Dominik; Schmitt, Daniel; Bartel-Steinbach, Martina; Schröter-Kermani, Christa; Kolossa-Gehring, Marike; von Briesen, Hagen; Zimmermann, Heiko
2014-01-01
Technical progress has simplified tasks in lab diagnosis and improved quality of test results. Errors occurring during the pre-analytical phase have more negative impact on the quality of test results than errors encountered during the total analytical process. Different infrastructures of sampling sites can highly influence the quality of samples and therewith of analytical results. Annually the German Environmental Specimen Bank (ESB) collects, characterizes, and stores blood, plasma, and urine samples of 120-150 volunteers each on four different sampling sites in Germany. Overarching goal is to investigate the exposure to environmental pollutants of non-occupational exposed young adults combining human biomonitoring with questionnaire data. We investigated the requirements of the study and the possibility to realize a highly standardized sampling procedure on a mobile platform in order to increase the required quality of the pre-analytical phase. The results lead to the development of a mobile epidemiologic laboratory (epiLab) in the project "Labor der Zukunft" (future's lab technology). This laboratory includes a 14.7 m(2) reception area to record medical history and exposure-relevant behavior, a 21.1 m(2) examination room to record dental fillings and for blood withdrawal, a 15.5 m(2) biological safety level 2 laboratory to process and analyze samples on site including a 2.8 m(2) personnel lock and a 3.6 m2 cryofacility to immediately freeze samples. Frozen samples can be transferred to their final destination within the vehicle without breaking the cold chain. To our knowledge, we herewith describe for the first time the implementation of a biological safety laboratory (BSL) 2 lab and an epidemiologic unit on a single mobile platform. Since 2013 we have been collecting up to 15.000 individual human samples annually under highly standardized conditions using the mobile laboratory. Characterized and free of alterations they are kept ready for retrospective analyses in their final archive, the German ESB.
Algae viability over time in a ballast water sample
NASA Astrophysics Data System (ADS)
Gollasch, Stephan; David, Matej
2018-03-01
The biology of vessels' ballast water needs to be analysed for several reasons, one of these being performance tests of ballast water management systems. This analysis includes a viability assessment of phytoplankton. To overcome logistical problems to get algae sample processing gear on board of a vessel to document algae viability, samples may be transported to land-based laboratories. Concerns were raised how the storage conditions of the sample may impact algae viability over time and what the most appropriate storage conditions were. Here we answer these questions with a long-term algae viability study with daily sample analysis using Pulse-Amplitude Modulated (PAM) fluorometry. The sample was analysed over 79 days. We tested different storage conditions: fridge and room temperature with and without light. It seems that during the first two weeks of the experiment the viability remains almost unchanged with a slight downwards trend. In the continuing period, before the sample was split, a slightly stronger downwards viability trend was observed, which occurred at a similar rate towards the end of the experiment. After the sample was split, the strongest viability reduction was measured for the sample stored without light at room temperature. We concluded that the storage conditions, especially regarding temperature and light exposure, have a stronger impact on algae viability compared to the storage duration and that inappropriate storage conditions reduce algal viability. A sample storage time of up to two weeks in a dark and cool environment has little influence on the organism viability. This indicates that a two week time duration between sample taking on board a vessel and the viability measurement in a land-based laboratory may not be very critical.
Standardized protocols for quality control of MRM-based plasma proteomic workflows.
Percy, Andrew J; Chambers, Andrew G; Smith, Derek S; Borchers, Christoph H
2013-01-04
Mass spectrometry (MS)-based proteomics is rapidly emerging as a viable technology for the identification and quantitation of biological samples, such as human plasma--the most complex yet commonly employed biofluid in clinical analyses. The transition from a qualitative to quantitative science is required if proteomics is going to successfully make the transition to a clinically useful technique. MS, however, has been criticized for a lack of reproducibility and interlaboratory transferability. Currently, the MS and plasma proteomics communities lack standardized protocols and reagents to ensure that high-quality quantitative data can be accurately and precisely reproduced by laboratories across the world using different MS technologies. Toward addressing this issue, we have developed standard protocols for multiple reaction monitoring (MRM)-based assays with customized isotopically labeled internal standards for quality control of the sample preparation workflow and the MS platform in quantitative plasma proteomic analyses. The development of reference standards and their application to a single MS platform is discussed herein, along with the results from intralaboratory tests. The tests highlighted the importance of the reference standards in assessing the efficiency and reproducibility of the entire bottom-up proteomic workflow and revealed errors related to the sample preparation and performance quality and deficits of the MS and LC systems. Such evaluations are necessary if MRM-based quantitative plasma proteomics is to be used in verifying and validating putative disease biomarkers across different research laboratories and eventually in clinical laboratories.
Santos, C; Fondevila, M; Ballard, D; Banemann, R; Bento, A M; Børsting, C; Branicki, W; Brisighelli, F; Burrington, M; Capal, T; Chaitanya, L; Daniel, R; Decroyer, V; England, R; Gettings, K B; Gross, T E; Haas, C; Harteveld, J; Hoff-Olsen, P; Hoffmann, A; Kayser, M; Kohler, P; Linacre, A; Mayr-Eduardoff, M; McGovern, C; Morling, N; O'Donnell, G; Parson, W; Pascali, V L; Porto, M J; Roseth, A; Schneider, P M; Sijen, T; Stenzl, V; Court, D Syndercombe; Templeton, J E; Turanska, M; Vallone, P M; Oorschot, R A H van; Zatkalikova, L; Carracedo, Á; Phillips, C
2015-11-01
There is increasing interest in forensic ancestry tests, which are part of a growing number of DNA analyses that can enhance routine profiling by obtaining additional genetic information about unidentified DNA donors. Nearly all ancestry tests use single nucleotide polymorphisms (SNPs), but these currently rely on SNaPshot single base extension chemistry that can fail to detect mixed DNA. Insertion-deletion polymorphism (Indel) tests have been developed using dye-labeled primers that allow direct capillary electrophoresis detection of PCR products (PCR-to-CE). PCR-to-CE maintains the direct relationship between input DNA and signal strength as each marker is detected with a single dye, so mixed DNA is more reliably detected. We report the results of a collaborative inter-laboratory exercise of 19 participants (15 from the EDNAP European DNA Profiling group) that assessed a 34-plex SNP test using SNaPshot and a 46-plex Indel test using PCR-to-CE. Laboratories were asked to type five samples with different ancestries and detect an additional mixed DNA sample. Statistical inference of ancestry was made by participants using the Snipper online Bayes analysis portal plus an optional PCA module that analyzes the genotype data alongside calculation of Bayes likelihood ratios. Exercise results indicated consistent genotyping performance from both tests, reaching a particularly high level of reliability for the Indel test. SNP genotyping gave 93.5% concordance (compared to the organizing laboratory's data) that rose to 97.3% excluding one laboratory with a large number of miscalled genotypes. Indel genotyping gave a higher concordance rate of 99.8% and a reduced no-call rate compared to SNP analysis. All participants detected the mixture from their Indel peak height data and successfully assigned the correct ancestry to the other samples using Snipper, with the exception of one laboratory with SNP miscalls that incorrectly assigned ancestry of two samples and did not obtain informative likelihood ratios for a third. Therefore, successful ancestry assignments were achieved by participants in 92 of 95 Snipper analyses. This exercise demonstrates that ancestry inference tests based on binary marker sets can be readily adopted by laboratories that already have well-established CE regimes in place. The Indel test proved to be easy to use and allowed all exercise participants to detect the DNA mixture as well as achieving complete and concordant profiles in nearly all cases. Lastly, two participants successfully ran parallel next-generation sequencing analyses (each using different systems) and achieved high levels of genotyping concordance using the exercise PCR primer mixes unmodified. Copyright © 2015 Elsevier Ireland Ltd. All rights reserved.
Rothkamm, Kai; Barnard, Stephen; Ainsbury, Elizabeth A; Al-Hafidh, Jenna; Barquinero, Joan-Francesc; Lindholm, Carita; Moquet, Jayne; Perälä, Marjo; Roch-Lefèvre, Sandrine; Scherthan, Harry; Thierens, Hubert; Vral, Anne; Vandersickel, Veerle
2013-08-30
The identification of severely exposed individuals and reassurance of the 'worried well' are of prime importance for initial triage following a large scale radiation accident. We aim to develop the γ-H2AX foci assay into a rapid biomarker tool for use in accidents. Here, five laboratories established a standard operating procedure and analysed 100 ex vivo γ-irradiated, 4 or 24h incubated and overnight-shipped lymphocyte samples from four donors to generate γ-H2AX reference data, using manual and/or automated foci scoring strategies. In addition to acute, homogeneous exposures to 0, 1, 2 and 4Gy, acute simulated partial body (4Gy to 50% of cells) and protracted exposures (4Gy over 24h) were analysed. Data from all laboratories could be satisfactorily fitted with linear dose response functions. Average yields observed at 4h post exposure were 2-4 times higher than at 24h and varied considerably between laboratories. Automated scoring caused larger uncertainties than manual scoring and was unable to identify partial exposures, which were detectable in manually scored samples due to their overdispersed foci distributions. Protracted exposures were detectable but doses could not be accurately estimated with the γ-H2AX assay. We conclude that the γ-H2AX assay may be useful for rapid triage following a recent acute radiation exposure. The potentially higher speed and convenience of automated relative to manual foci scoring needs to be balanced against its compromised accuracy and inability to detect partial body exposures. Regular re-calibration or inclusion of reference samples may be necessary to ensure consistent results between laboratories or over long time periods. Crown Copyright © 2013. Published by Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Metfies, Katja; Schroeder, Friedhelm; Hessel, Johanna; Wollschläger, Jochen; Micheller, Sebastian; Wolf, Christian; Kilias, Estelle; Sprong, Pim; Neuhaus, Stefan; Frickenhaus, Stephan; Petersen, Wilhelm
2016-11-01
Information on recent biomass distribution and biogeography of photosynthetic marine protists with adequate temporal and spatial resolution is urgently needed to better understand the consequences of environmental change for marine ecosystems. Here we introduce and review a molecular-based observation strategy for high-resolution assessment of these protists in space and time. It is the result of extensive technology developments, adaptations and evaluations which are documented in a number of different publications, and the results of the recently completed field testing which are introduced in this paper. The observation strategy is organized at four different levels. At level 1, samples are collected at high spatiotemporal resolution using the remotely controlled automated filtration system AUTOFIM. Resulting samples can either be preserved for later laboratory analyses, or directly subjected to molecular surveillance of key species aboard the ship via an automated biosensor system or quantitative polymerase chain reaction (level 2). Preserved samples are analyzed at the next observational levels in the laboratory (levels 3 and 4). At level 3 this involves molecular fingerprinting methods for a quick and reliable overview of differences in protist community composition. Finally, selected samples can be used to generate a detailed analysis of taxonomic protist composition via the latest next generation sequencing technology (NGS) at level 4. An overall integrated dataset of the results based on the different analyses provides comprehensive information on the diversity and biogeography of protists, including all related size classes. At the same time the cost of the observation is optimized with respect to analysis effort and time.
Sigmund, Gerd; Koch, Anja; Orlovius, Anne-Katrin; Guddat, Sven; Thomas, Andreas; Schänzer, Wilhelm; Thevis, Mario
2014-01-01
Since January 2014, the anti-anginal drug trimetazidine [1-(2,3,4-trimethoxybenzyl)-piperazine] has been classified as prohibited substance by the World Anti-Doping Agency (WADA), necessitating specific and robust detection methods in sports drug testing laboratories. In the present study, the implementation of the intact therapeutic agent into two different initial testing procedures based on gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) is reported, along with the characterization of urinary metabolites by electrospray ionization-high resolution/high accuracy (tandem) mass spectrometry. For GC-MS analyses, urine samples were subjected to liquid-liquid extraction sample preparation, while LC-MS/MS analyses were conducted by established 'dilute-and-inject' approaches. Both screening methods were validated for trimetazidine concerning specificity, limits of detection (0.5-50 ng/mL), intra-day and inter-day imprecision (<20%), and recovery (41%) in case of the GC-MS-based method. In addition, major metabolites such as the desmethylated trimetazidine and the corresponding sulfoconjugate, oxo-trimetazidine, and trimetazidine-N-oxide as identified in doping control samples were used to complement the LC-MS/MS-based assay, although intact trimetazidine was found at highest abundance of the relevant trimetazidine-related analytes in all tested sports drug testing samples. Retrospective data mining regarding doping control analyses conducted between 1999 and 2013 at the Cologne Doping Control Laboratory concerning trimetazidine revealed a considerable prevalence of the drug particularly in endurance and strength sports accounting for up to 39 findings per year. Copyright © 2014 John Wiley & Sons, Ltd.
Managadze, G G; Safronova, A A; Luchnikov, K A; Vorobyova, E A; Duxbury, N S; Wurz, P; Managadze, N G; Chumikov, A E; Khamizov, R Kh
2017-05-01
We propose a new technique for the detection of microorganisms by elemental composition analyses of a sample extracted from regolith, permafrost, and ice of extraterrestrial bodies. We also describe the design of the ABIMAS instrument, which consists of the onboard time-of-flight laser mass-reflectron (TOF LMR) and the sample preparation unit (SPU) for biomass extraction. This instrument was initially approved to fly on board the ExoMars 2020 lander mission. The instrument can be used to analyze the elemental composition of possible extraterrestrial microbial communities and compare it to that of terrestrial microorganisms. We have conducted numerous laboratory studies to confirm the possibility of biomass identification via the following biomarkers: P/S and Ca/K ratios, and C and N abundances. We underline that only the combination of these factors will allow one to discriminate microbial samples from geological ones. Our technique has been tested experimentally in numerous laboratory trials on cultures of microorganisms and polar permafrost samples as terrestrial analogues for martian polar soils. We discuss various methods of extracting microorganisms and sample preparation. The developed technique can be used to search for and identify microorganisms in different martian samples and in the subsurface of other planets, satellites, comets, and asteroids-in particular, Europa, Ganymede, and Enceladus. Key Words: Mass spectrometry-Life-detection instruments-Biomarkers-Earth Mars-Biomass spectra. Astrobiology 17, 448-458.
Schot, Marjolein J C; van Delft, Sanne; Kooijman-Buiting, Antoinette M J; de Wit, Niek J; Hopstaken, Rogier M
2015-05-18
Various point-of-care testing (POCT) urine analysers are commercially available for routine urine analysis in general practice. The present study compares analytical performance, agreement and user-friendliness of six different POCT urine analysers for diagnosing urinary tract infection in general practice. All testing procedures were performed at a diagnostic centre for primary care in the Netherlands. Urine samples were collected at four general practices. Analytical performance and agreement of the POCT analysers regarding nitrite, leucocytes and erythrocytes, with the laboratory reference standard, was the primary outcome measure, and analysed by calculating sensitivity, specificity, positive and negative predictive value, and Cohen's κ coefficient for agreement. Secondary outcome measures were the user-friendliness of the POCT analysers, in addition to other characteristics of the analysers. The following six POCT analysers were evaluated: Uryxxon Relax (Macherey Nagel), Urisys 1100 (Roche), Clinitek Status (Siemens), Aution 11 (Menarini), Aution Micro (Menarini) and Urilyzer (Analyticon). Analytical performance was good for all analysers. Compared with laboratory reference standards, overall agreement was good, but differed per parameter and per analyser. Concerning the nitrite test, the most important test for clinical practice, all but one showed perfect agreement with the laboratory standard. For leucocytes and erythrocytes specificity was high, but sensitivity was considerably lower. Agreement for leucocytes varied between good to very good, and for the erythrocyte test between fair and good. First-time users indicated that the analysers were easy to use. They expected higher productivity and accuracy when using these analysers in daily practice. The overall performance and user-friendliness of all six commercially available POCT urine analysers was sufficient to justify routine use in suspected urinary tract infections in general practice. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted under a licence) please go to http://group.bmj.com/group/rights-licensing/permissions.
Performance evaluation of the Abbott CELL-DYN Ruby and the Sysmex XT-2000i haematology analysers.
Leers, M P G; Goertz, H; Feller, A; Hoffmann, J J M L
2011-02-01
Two mid-range haematology analysers (Abbott CELL-DYN Ruby and Sysmex XT-2000i) were evaluated to determine their analytical performance and workflow efficiency in the haematology laboratory. In total 418 samples were processed for determining equivalence of complete blood count (CBC) measurements, and 100 for reticulocyte comparison. Blood smears served for assessing the agreement of the differential counts. Inter-instrument agreement for most parameters was good although small numbers of discrepancies were observed. Systematic biases were found for mean cell volume, reticulocytes, platelets and mean platelet volume. CELL-DYN Ruby WBC differentials were obtained with all samples while the XT-2000i suppressed differentials partially or completely in 13 samples (3.1%). WBC subpopulation counts were otherwise in good agreement with no major outliers. Following first-pass CBC/differential analysis, 88 (21%) of XT-2000i samples required further analyser processing compared to 18 (4.3%) for the CELL-DYN Ruby. Smear referrals for suspected WBC/nucleated red blood cells and platelet abnormalities were indicated for 106 (25.4%) and 95 (22.7%) of the XT-2000i and CELL-DYN Ruby samples respectively. Flagging efficiencies for both analysers were found to be similar. The Sysmex XT-2000i and Abbott CELL-DYN Ruby analysers have broadly comparable analytical performance, but the CELL-DYN Ruby showed superior first-pass efficiency. © 2010 Blackwell Publishing Ltd.
NASA Technical Reports Server (NTRS)
Sutter, B.; McAdam, A. C.; Rampe, E. B.; Ming, D. W.; Mahaffy, P. R.; Navarro-Gonzalez, R.; Stern, J. C.; Eigenbrode, J. L.; Archer, P. D.
2016-01-01
The Sample Analysis at Mars (SAM) instrument aboard the Mars Science Laboratory rover has analyzed 10 samples from Gale Crater. All SAM evolved gas analyses have yielded a multitude of volatiles (e.g, H2O, SO2, H2S, CO2, CO, NO, O2, HC1). The objectives of this work are to 1) Characterize the evolved H2O, SO2, CO2, and O2 gas traces of sediments analyzed by SAM through sol 1178, 2) Constrain sediment mineralogy/composition based on SAM evolved gas analysis (SAM-EGA), and 3) Discuss the implications of these results releative to understanding the geochemical history of Gale Crater.
DATA QUALITY OBJECTIVES FOR SELECTING WASTE SAMPLES FOR BENCH-SCALE REFORMER TREATABILITY STUDIES
DOE Office of Scientific and Technical Information (OSTI.GOV)
BANNING DL
2011-02-11
This document describes the data quality objectives to select archived samples located at the 222-S Laboratory for Bench-Scale Reforming testing. The type, quantity, and quality of the data required to select the samples for Fluid Bed Steam Reformer testing are discussed. In order to maximize the efficiency and minimize the time to treat Hanford tank waste in the Waste Treatment and Immobilization Plant, additional treatment processes may be required. One of the potential treatment processes is the fluidized bed steam reformer. A determination of the adequacy of the fluidized bed steam reformer process to treat Hanford tank waste is required.more » The initial step in determining the adequacy of the fluidized bed steam reformer process is to select archived waste samples from the 222-S Laboratory that will be used in a bench scale tests. Analyses of the selected samples will be required to confirm the samples meet the shipping requirements and for comparison to the bench scale reformer (BSR) test sample selection requirements.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Peters, T.; Washington, A; . Fondeur, F.
2011-09-29
Savannah River National Laboratory (SRNL) periodically analyses solvent samples from Modular Caustic-Side Solvent Extraction Unit (MCU) in support of continuing operations. A quarterly analysis of the solvent is required to maintain solvent composition within specifications. Analytical results of the analyses of Solvent Hold Tank (SHT) samples MCU-11-314, MCU-11-315, MCU-11-316, MCU-11-317, MCU-11-318 and MCU-11-319 have been previously reported. MCU has experienced a modest decline in cesium removal efficiency while processing the current feed, 'Macrobatch 3'. While the target decontamination factor (DF) is 200, the fiscal year 2011 DF average is 161. The results of the prior solvent analysis report did notmore » identify a specific factor that would correlate with the poor cesium decontamination beyond a low concentration of the suppressor, trioctylamine. New analyses of the quarterly sample are reported in this document, as well as a cross-check of {sup 137}Cs measurements for SRNL and F/H lab. Furthermore, in an attempt to discover the reason for the decline in DF at MCU, SRNL was tasked with analyzing numerous Caustic Wash Tank (CWT) and chemical feed samples.« less
2012-01-01
Background Ovine footrot is a contagious disease with worldwide occurrence in sheep. The main causative agent is the fastidious bacterium Dichelobacter nodosus. In Scandinavia, footrot was first diagnosed in Sweden in 2004 and later also in Norway and Denmark. Clinical examination of sheep feet is fundamental to diagnosis of footrot, but D. nodosus should also be detected to confirm the diagnosis. PCR-based detection using conventional PCR has been used at our institutes, but the method was laborious and there was a need for a faster, easier-to-interpret method. The aim of this study was to develop a TaqMan-based real-time PCR assay for detection of D. nodosus and to compare its performance with culturing and conventional PCR. Methods A D. nodosus-specific TaqMan based real-time PCR assay targeting the 16S rRNA gene was designed. The inclusivity and exclusivity (specificity) of the assay was tested using 55 bacterial and two fungal strains. To evaluate the sensitivity and harmonisation of results between different laboratories, aliquots of a single DNA preparation were analysed at three Scandinavian laboratories. The developed real-time PCR assay was compared to culturing by analysing 126 samples, and to a conventional PCR method by analysing 224 samples. A selection of PCR-products was cloned and sequenced in order to verify that they had been identified correctly. Results The developed assay had a detection limit of 3.9 fg of D. nodosus genomic DNA. This result was obtained at all three laboratories and corresponds to approximately three copies of the D. nodosus genome per reaction. The assay showed 100% inclusivity and 100% exclusivity for the strains tested. The real-time PCR assay found 54.8% more positive samples than by culturing and 8% more than conventional PCR. Conclusions The developed real-time PCR assay has good specificity and sensitivity for detection of D. nodosus, and the results are easy to interpret. The method is less time-consuming than either culturing or conventional PCR. PMID:22293440
Granitto, Matthew; DeWitt, Ed H.; Klein, Terry L.
2010-01-01
This database was initiated, designed, and populated to collect and integrate geochemical data from central Colorado in order to facilitate geologic mapping, petrologic studies, mineral resource assessment, definition of geochemical baseline values and statistics, environmental impact assessment, and medical geology. The Microsoft Access database serves as a geochemical data warehouse in support of the Central Colorado Assessment Project (CCAP) and contains data tables describing historical and new quantitative and qualitative geochemical analyses determined by 70 analytical laboratory and field methods for 47,478 rock, sediment, soil, and heavy-mineral concentrate samples. Most samples were collected by U.S. Geological Survey (USGS) personnel and analyzed either in the analytical laboratories of the USGS or by contract with commercial analytical laboratories. These data represent analyses of samples collected as part of various USGS programs and projects. In addition, geochemical data from 7,470 sediment and soil samples collected and analyzed under the Atomic Energy Commission National Uranium Resource Evaluation (NURE) Hydrogeochemical and Stream Sediment Reconnaissance (HSSR) program (henceforth called NURE) have been included in this database. In addition to data from 2,377 samples collected and analyzed under CCAP, this dataset includes archived geochemical data originally entered into the in-house Rock Analysis Storage System (RASS) database (used by the USGS from the mid-1960s through the late 1980s) and the in-house PLUTO database (used by the USGS from the mid-1970s through the mid-1990s). All of these data are maintained in the Oracle-based National Geochemical Database (NGDB). Retrievals from the NGDB and from the NURE database were used to generate most of this dataset. In addition, USGS data that have been excluded previously from the NGDB because the data predate earliest USGS geochemical databases, or were once excluded for programmatic reasons, have been included in the CCAP Geochemical Database and are planned to be added to the NGDB.
Gören, Ahmet C; Bilsel, Gökhan; Şimşek, Adnan; Bilsel, Mine; Akçadağ, Fatma; Topal, Kevser; Ozgen, Hasan
2015-05-15
High Performance Liquid Chromatography LC-UV and LC-MS/MS methods were developed and validated for quantitative analyses of sodium benzoate and potassium sorbate in foods and beverages. HPLC-UV and LC-MS/MS methods were compared for quantitative analyses of sodium benzoate and potassium sorbate in a representative ketchup sample. Optimisation of the methods enabled the chromatographic separation of the analytes in less than 4 min. A correlation coefficient of 0.999 was achieved over the measured calibration range for both compounds and methods (HPLC and LC-MS/MS). The uncertainty values of sodium benzoate and potassium sorbate were found as 0.199 and 0.150 mg/L by HPLC and 0.072 and 0.044 mg/L by LC-MS/MS, respectively. Proficiency testing performance of Turkish accredited laboratories between the years 2005 and 2013 was evaluated and reported herein. The aim of the proficiency testing scheme was to evaluate the performance of the laboratories, analysing benzoate and sorbate in tomato ketchup. Copyright © 2014 Elsevier Ltd. All rights reserved.
McNamara, P J; Sharief, N
2001-09-01
Near-patient blood glucose monitoring is an essential component of neonatal intensive care but the analysers currently used are unreliable and inaccurate. The aim of this study was to compare a new glucose electrode-based analyser (EML 105) and a non-wipe reflectance photometry method (Advantage) as opposed to a recognized laboratory reference method (Hexokinase). We also investigated the effect of sample route and haematocrit on the accuracy of the glucose readings obtained by each method of analysis. Whole blood glucose concentrations ranging from 0 to 3.5 mmol/l were carefully prepared in a laboratory setting and blood samples from each respective solution were then measured by EML 105 and Advantage analysers. The results obtained were then compared with the corresponding plasma glucose reading obtained by the Hexokinase method, using linear regression analysis. An in vivo study was subsequently performed on 103 neonates, over a 1-y period, using capillary and venous whole blood samples. Whole blood glucose concentration was estimated from each sample using both analysers and compared with the corresponding plasma glucose concentration estimated by the Hexokinase method. Venous blood was centrifuged and haematocrit was estimated using standardized curves. The effect of haematocrit on the agreement between whole blood and plasma glucose was investigated, estimating the degree of correlation on a scatterplot of the results and linear regression analysis. Both the EML 105 and Hexokinase methods were highly accurate, in vitro, with small proportional biases of 2% and 5%, respectively. However, in vivo, both study analysers overestimated neonatal plasma glucose, ranging from at best 0.45 mmol/l (EML 105 venous) to 0.69 mmol/l (EML capillary). There was no significant difference in the agreement of capillary (GD = 0.12, 95% CI, [-0.32,0.08], p = 0.2) or venous samples (GD = 0.05, 95% CI. [0.09, 0.19], p = 0.49) with plasma glucose when analysed by either study method (GD = glucose difference between study analyser and reference method) However, the venous samples analysed by EML 105 estimated plasma glucose significantly better than capillary samples using the same method of analysis (GD = 0.24, 95% CI. [0.09,0.38], p < 0.01). The relationship between haematocrit and the resultant glucose differences was non-linear with correlation coefficients of r = -0.057 (EML 105 capillary), r = 0.145 (EML 105 venous), r = -0.127 (Advantage capillary) and r = -0.275 (Advantage venous). There was no significant difference in the effect of haematocrit on the performance of EML 105 versus Advantage, regardless of the sample route. Both EML 105 and Advantage overestimated plasma glucose, with no significant difference in the performance of either analyser, regardless of the route of analysis. Agreement with plasma glucose was better for venous samples but this was only statistically significant when EML 105 capillary and venous results were compared. Haematocrit is not a significant confounding factor towards the performance of either EML 105 or Advantage in neonates, regardless of the route of sampling. The margin of overestimation of blood glucose prohibits the recommendation of both EML 105 and Advantage for routine neonatal glucose screening. The consequences include failure accurately to diagnose hypoglycaemia and delays in the instigation of therapeutic measures, both of which may potentially result in an adverse, long-term, neurodevelopmental outcome.
Development of Gold Standard Ion-Selective Electrode-Based Methods for Fluoride Analysis
Martínez-Mier, E.A.; Cury, J.A.; Heilman, J.R.; Katz, B.P.; Levy, S.M.; Li, Y.; Maguire, A.; Margineda, J.; O’Mullane, D.; Phantumvanit, P.; Soto-Rojas, A.E.; Stookey, G.K.; Villa, A.; Wefel, J.S.; Whelton, H.; Whitford, G.M.; Zero, D.T.; Zhang, W.; Zohouri, V.
2011-01-01
Background/Aims: Currently available techniques for fluoride analysis are not standardized. Therefore, this study was designed to develop standardized methods for analyzing fluoride in biological and nonbiological samples used for dental research. Methods A group of nine laboratories analyzed a set of standardized samples for fluoride concentration using their own methods. The group then reviewed existing analytical techniques for fluoride analysis, identified inconsistencies in the use of these techniques and conducted testing to resolve differences. Based on the results of the testing undertaken to define the best approaches for the analysis, the group developed recommendations for direct and microdiffusion methods using the fluoride ion-selective electrode. Results Initial results demonstrated that there was no consensus regarding the choice of analytical techniques for different types of samples. Although for several types of samples, the results of the fluoride analyses were similar among some laboratories, greater differences were observed for saliva, food and beverage samples. In spite of these initial differences, precise and true values of fluoride concentration, as well as smaller differences between laboratories, were obtained once the standardized methodologies were used. Intraclass correlation coefficients ranged from 0.90 to 0.93, for the analysis of a certified reference material, using the standardized methodologies. Conclusion The results of this study demonstrate that the development and use of standardized protocols for F analysis significantly decreased differences among laboratories and resulted in more precise and true values. PMID:21160184
Gaudin, Valerie; Juhel-Gaugain, Murielle; Morétain, Jean-Pierre; Sanders, Pascal
2008-12-01
Premi Test contains viable spores of a strain of Bacillus stearothermophilus which is sensitive to antimicrobial residues, such as beta-lactams, tetracyclines, macrolides and sulphonamides. The growth of the strain is inhibited by the presence of antimicrobial residues in muscle tissue samples. Premi Test was validated according to AFNOR rules (French Association for Normalisation). The AFNOR validation was based on the comparison of reference methods (French Official method, i.e. four plate test (FPT) and the STAR protocol (five plate test)) with the alternative method (Premi Test). A preliminary study was conducted in an expert laboratory (Community Reference Laboratory, CRL) on both spiked and incurred samples (field samples). Several method performance criteria (sensitivity, specificity, relative accuracy) were estimated and are discussed, in addition to detection capabilities. Adequate agreement was found between the alternative method and the reference methods. However, Premi Test was more sensitive to beta-lactams and sulphonamides than the FPT. Subsequently, a collaborative study with 11 laboratories was organised by the CRL. Blank and spiked meat juice samples were sent to participants. The expert laboratory (CRL) statistically analysed the results. It was concluded that Premi Test could be used for the routine determination of antimicrobial residues in muscle of different animal origin with acceptable analytical performance. The detection capabilities of Premi Test for beta-lactams (amoxicillin, ceftiofur), one macrolide (tylosin) and tetracycline were at the level of the respective maximum residue limits (MRL) in muscle samples or even lower.
Stratigraphic sections of the Phosphoria formation in Wyoming, 1947-48
McKelvey, Vincent Ellis; Smith, L.E.; Hoppin, R.A.; Armstrong, F.C.
1952-01-01
As part of a comprehensive investigation of the phosphate deposits of the western field begun in 1947, the U. S. Geological Survey has measured and sampled the Permian Phosphoria formation at many localities in Wyoming and adjacent states. Because these data will not be fully synthesized for many years, segments of the data, accompanied by little or no interpretation, will be published as preliminary reports as they are assembled. This report, which contains abstracts of some of the sections measured in western Wyoming (pl. 1), is one of this series. The field and laboratory procedures adopted in these investigations are described rather fully in a companion report (McKelvey and others, 1952a). Many people have taken part in this investigation. R. M. Campbell, R. A. Gulbrandsen, R. A. Harris, D. M. Larrabee, F. W. O'Malley, O. A. Payne, R. S. Sears, R. P. Sheldon, and R. A. Smart participated in the description of the strata and the collection of the samples referred to in this report. D. B. Dimick, H. A. Larsen, and T. K. Rigby assisted in the preparation of exposures and the crushing and splitting of samples in the field. The laboratory preparation of samples for chemical analysis was done in Denver, Colo., under the direction of W. P. Huleatt. Most of the P2O5 and acid-insoluble analyses were made for the Survey by the U. S. Bureau of Mines at the Northwest Electrodevelopment Laboratory, Albany, Oreg., under the direction of S. M. Shelton and M. L. Wright. Most of the Al2O3, Fe2O3, and loss-on-ignition analyses were made by the Trace Elements Section laboratory of the Survey in Washington, D. C., under the direction of J. C. Rabbitt by chemists I. Barlow, A. Caemmerer, J. Greene, F. S. Grimadli, N. Guttag, H. Levine, H. Mela, Jr., and R. G. Milkey, and most of the spectrographic reports were prepared in this laboratory by C. L. Waring. The samples from one locality (Coal Canyon) were analyzed for P2O5, Al2O3, Fe2O3, V2O5, F, loss on ignition, and acid insoluble in the Chemical Laboratory of the Tennessee Valley Authority at Wilson Dam, Alabama, and spectrographically by D. M. Mortimer, of the Bureau of Mines at Albany. Compilation of the data has been largely by R. P. Sheldon and F. D. Frieske under the supervision of R. W. Swanson. Organization of the tabular data has been largely by Anita Cozzetto.
NASA Technical Reports Server (NTRS)
Stern, J. C.; Steele, A.; Brunner, A.; Coll, P.; Eigenbrode, J.; Franz, H. B.; Freissinet, C.; Glavin, D.; Jones, J. H.; Navarro-Gonzalez, R.;
2013-01-01
The Sample Analysis at Mars (SAM) instrument suite on the Mars Science Laboratory (MSL) Curiosity Rover detected nitrogen-bearing compounds during the pyrolysis of Rocknest material at Gale Crater. Hydrogen cyanide and acetonitrile were identified by the quadrupole mass spectrometer (QMS) both in direct evolved gas analysis (EGA). SAM carried out four separate analyses from Rocknest Scoop 5. A significant low temperature release was present in Rocknest runs 1-4, while a smaller high temperature release was also seen in Rocknest runs 1-3. Here we evaluate whether these compounds are indigenous to Mars or a pyrolysis product resulting from known terrestrial materials that are part of the SAM derivatization.
NASA Astrophysics Data System (ADS)
Galipo, Randolph C.; Canhoto, Alfredo J.; Walla, Michael D.; Morgan, Stephen L.
1999-02-01
A senior-level undergraduate laboratory experiment that demonstrates the use of solid-phase microextraction (SPME) and capillary gas chromatography-mass spectrometry (GC-MS) was developed for the identification of volatile compounds in consumer products. SPME minimizes sample preparation and concentrates volatile analytes in a solvent-free manner. Volatile flavor and fragrance compounds were extracted by SPME from the headspace of vials containing shampoos, chewing gums, and perfumes and analyzed by GC-MS. Headspace SPME was shown to be more sensitive than conventional headspace analysis of similar samples performed with an airtight syringe. Analysis times were less than 30 min, allowing multiple analyses to be performed in a typical laboratory class period.
NASA Astrophysics Data System (ADS)
Ferus, Martin; Koukal, Jakub; Lenža, Libor; Srba, Jiří; Kubelík, Petr; Laitl, Vojtěch; Zanozina, Ekaterina M.; Váňa, Pavel; Kaiserová, Tereza; Knížek, Antonín; Rimmer, Paul; Chatzitheodoridis, Elias; Civiš, Svatopluk
2018-03-01
Aims: We aim to analyse real-time Perseid and Leonid meteor spectra using a novel calibration-free (CF) method, which is usually applied in the laboratory for laser-induced breakdown spectroscopic (LIBS) chemical analysis. Methods: Reference laser ablation spectra of specimens of chondritic meteorites were measured in situ simultaneously with a high-resolution laboratory echelle spectrograph and a spectral camera for meteor observation. Laboratory data were subsequently evaluated via the CF method and compared with real meteor emission spectra. Additionally, spectral features related to airglow plasma were compared with the spectra of laser-induced breakdown and electric discharge in the air. Results: We show that this method can be applied in the evaluation of meteor spectral data observed in real time. Specifically, CF analysis can be used to determine the chemical composition of meteor plasma, which, in the case of the Perseid and Leonid meteors analysed in this study, corresponds to that of the C-group of chondrites.
NASA Astrophysics Data System (ADS)
López-Sánchez, M.; Mansilla-Plaza, L.; Sánchez-de-laOrden, M.
2017-10-01
Prior to field scale research, soil samples are analysed on a laboratory scale for electrical resistivity calibrations. Currently, there are a variety of field instruments to estimate the water content in soils using different physical phenomena. These instruments can be used to develop moisture-resistivity relationships on the same soil samples. This assures that measurements are performed on the same material and under the same conditions (e.g., humidity and temperature). A geometric factor is applied to the location of electrodes, in order to calculate the apparent electrical resistivity of the laboratory test cells. This geometric factor can be determined in three different ways: by means of the use of an analytical approximation, laboratory trials (experimental approximation), or by the analysis of a numerical model. The first case, the analytical approximation, is not appropriate for complex cells or arrays. And both, the experimental and numerical approximation can lead to inaccurate results. Therefore, we propose a novel approach to obtain a compromise solution between both techniques, providing a more precise determination of the geometrical factor.
Thiros, Susan A.; Bender, David A.; Mueller, David K.; Rose, Donna L.; Olsen, Lisa D.; Martin, Jeffrey D.; Bernard, Bruce; Zogorski, John S.
2011-01-01
The Field Contamination Study (FCS) was designed to determine the field processes that tend to result in clean field blanks and to identify potential sources of contamination to blanks collected in the field from selected volatile organic compounds (VOCs) and wastewater-indicator compounds (WICs). The VOCs and WICs analyzed in the FCS were detected in blanks collected by the U.S. Geological Survey (USGS) National Water-Quality Assessment (NAWQA) Program during 1996–2008 and 2002–08, respectively. To minimize the number of variables, the study required ordering of supplies just before sampling, storage of supplies and equipment in clean areas, and use of adequate amounts of purge-and-trap volatile-grade methanol and volatile pesticide-grade blank water (VPBW) to clean sampling equipment and to collect field blanks.Blanks and groundwater samples were collected during 2008–09 at 16 sites, which were a mix of water-supply and monitoring wells, located in 9 States. Five different sample types were collected for the FCS at each site: (1) a source-solution blank collected at the USGS National Water Quality Laboratory (NWQL) using laboratory-purged VPBW, (2) source-solution blanks collected in the field using laboratory-purged VPBW, (3) source-solution blanks collected in the field using field-purged VPBW, (4) a field blank collected using field-purged VPBW, and (5) a groundwater sample collected from a well. The source-solution blank and field-blank analyses were used to identify, quantify, and document extrinsic contamination and to help determine the sources and causes of data-quality problems that can affect groundwater samples.Concentrations of compounds detected in FCS analyses were quantified and results were stored in the USGS National Water Information System database after meeting rigorous identification and quantification criteria. The study also utilized information provided by laboratory analysts about evidence indicating the presence of selected compounds, using less rigorous identification criteria than is required for reporting data to the National Water Information System database. For the FCS, these data are considered adequate to indicate "evidence of presence," and were used only for diagnostic purposes. Evidence of VOCs and WICs at low concentrations near or less than the long-term method detection level can indicate a contamination problem that could affect future datasets if method detection levels were ever to be lowered.
Experiments on planetary ices at UCL
NASA Astrophysics Data System (ADS)
Grindrod, P. M.; Fortes, A. D.; Wood, I. G.; Dobson, D.; Sammonds, P. R.; Stone-Drake, L.; Vocadlo, L.
2007-08-01
Using a suite of techniques and equipment, we conduct several different types of experiments on planetary ices at UCL. Samples are prepared in the Ice Physics Laboratory, which consists of a 5 chamber complex of inter-connected cold rooms, controllable from +30 to -30 deg C. Within this laboratory we have a functioning triaxial deformation cell operating at low temperature (down to -90 deg C) and high pressures (300 MPa), an Automatic Ice Fabric Analyser (AIFA) and a low-temperature microscope with CCD output. Polycrystalline samples, 40mm diameter by 100mm long, are compressed in the triaxial rig with a confining pressure; single crystal specimens are compressed in a separate uniaxial creep rig which operates at zero confining pressure for surface studies. A cold stage is also available for study of ice microstructural studies on our new Jeol JSM-6480LV SEM, which also allows tensile, compression and/or bending tests, with load ranges from less than 2N to 5000N. Finally, we also use a cold stage on a new PANalytical, X'pert PRO MPD, high resolution powder diffractometer to study the structure and phase behaviour of icy materials. Recent highlights of our work include: (1) derivation of a manufacturing process for methane clathrate at low temperatures, analysed in the X-Ray Diffraction Laboratory, for future rheological experiments, (2) analysed the growth behaviour of MS11, (3) refurbished and commenced calibration tests on the triaxial deformation cell using ice Ih, and (4) performed creep tests on gypsum and epsomite using the single crystal deformation cell. Further experiments will build on these preliminary results.
NASA Technical Reports Server (NTRS)
Weaver, W. L.; Norton, H. N.; Darnell, W. L.
1975-01-01
Mission concepts were investigated for automated return to Earth of a Mars surface sample adequate for detailed analyses in scientific laboratories. The minimum sample mass sufficient to meet scientific requirements was determined. Types of materials and supporting measurements for essential analyses are reported. A baseline trajectory profile was selected for its low energy requirements and relatively simple implementation, and trajectory profile design data were developed for 1979 and 1981 launch opportunities. Efficient spacecraft systems were conceived by utilizing existing technology where possible. Systems concepts emphasized the 1979 launch opportunity, and the applicability of results to other opportunities was assessed. It was shown that the baseline missions (return through Mars parking orbit) and some comparison missions (return after sample transfer in Mars orbit) can be accomplished by using a single Titan III E/Centaur as the launch vehicle. All missions investigated can be accomplished by use of Space Shuttle/Centaur vehicles.
Potential sources of analytical bias and error in selected trace element data-quality analyses
Paul, Angela P.; Garbarino, John R.; Olsen, Lisa D.; Rosen, Michael R.; Mebane, Christopher A.; Struzeski, Tedmund M.
2016-09-28
Potential sources of analytical bias and error associated with laboratory analyses for selected trace elements where concentrations were greater in filtered samples than in paired unfiltered samples were evaluated by U.S. Geological Survey (USGS) Water Quality Specialists in collaboration with the USGS National Water Quality Laboratory (NWQL) and the Branch of Quality Systems (BQS).Causes for trace-element concentrations in filtered samples to exceed those in associated unfiltered samples have been attributed to variability in analytical measurements, analytical bias, sample contamination either in the field or laboratory, and (or) sample-matrix chemistry. These issues have not only been attributed to data generated by the USGS NWQL but have been observed in data generated by other laboratories. This study continues the evaluation of potential analytical bias and error resulting from matrix chemistry and instrument variability by evaluating the performance of seven selected trace elements in paired filtered and unfiltered surface-water and groundwater samples collected from 23 sampling sites of varying chemistries from six States, matrix spike recoveries, and standard reference materials.Filtered and unfiltered samples have been routinely analyzed on separate inductively coupled plasma-mass spectrometry instruments. Unfiltered samples are treated with hydrochloric acid (HCl) during an in-bottle digestion procedure; filtered samples are not routinely treated with HCl as part of the laboratory analytical procedure. To evaluate the influence of HCl on different sample matrices, an aliquot of the filtered samples was treated with HCl. The addition of HCl did little to differentiate the analytical results between filtered samples treated with HCl from those samples left untreated; however, there was a small, but noticeable, decrease in the number of instances where a particular trace-element concentration was greater in a filtered sample than in the associated unfiltered sample for all trace elements except selenium. Accounting for the small dilution effect (2 percent) from the addition of HCl, as required for the in-bottle digestion procedure for unfiltered samples, may be one step toward decreasing the number of instances where trace-element concentrations are greater in filtered samples than in paired unfiltered samples.The laboratory analyses of arsenic, cadmium, lead, and zinc did not appear to be influenced by instrument biases. These trace elements showed similar results on both instruments used to analyze filtered and unfiltered samples. The results for aluminum and molybdenum tended to be higher on the instrument designated to analyze unfiltered samples; the results for selenium tended to be lower. The matrices used to prepare calibration standards were different for the two instruments. The instrument designated for the analysis of unfiltered samples was calibrated using standards prepared in a nitric:hydrochloric acid (HNO3:HCl) matrix. The instrument designated for the analysis of filtered samples was calibrated using standards prepared in a matrix acidified only with HNO3. Matrix chemistry may have influenced the responses of aluminum, molybdenum, and selenium on the two instruments. The best analytical practice is to calibrate instruments using calibration standards prepared in matrices that reasonably match those of the samples being analyzed.Filtered and unfiltered samples were spiked over a range of trace-element concentrations from less than 1 to 58 times ambient concentrations. The greater the magnitude of the trace-element spike concentration relative to the ambient concentration, the greater the likelihood spike recoveries will be within data control guidelines (80–120 percent). Greater variability in spike recoveries occurred when trace elements were spiked at concentrations less than 10 times the ambient concentration. Spike recoveries that were considerably lower than 90 percent often were associated with spiked concentrations substantially lower than what was present in the ambient sample. Because the main purpose of spiking natural water samples with known quantities of a particular analyte is to assess possible matrix effects on analytical results, the results of this study stress the importance of spiking samples at concentrations that are reasonably close to what is expected but sufficiently high to exceed analytical variability. Generally, differences in spike recovery results between paired filtered and unfiltered samples were minimal when samples were analyzed on the same instrument.Analytical results for trace-element concentrations in ambient filtered and unfiltered samples greater than 10 and 40 μg/L, respectively, were within the data-quality objective for precision of ±25 percent. Ambient trace-element concentrations in filtered samples greater than the long-term method detection limits but less than 10 μg/L failed to meet the data-quality objective for precision for at least one trace element in about 54 percent of the samples. Similarly, trace-element concentrations in unfiltered samples greater than the long-term method detection limits but less than 40 μg/L failed to meet this data-quality objective for at least one trace-element analysis in about 58 percent of the samples. Although, aluminum and zinc were particularly problematic, limited re-analyses of filtered and unfiltered samples appeared to improve otherwise failed analytical precision.The evaluation of analytical bias using standard reference materials indicate a slight low bias for results for arsenic, cadmium, selenium, and zinc. Aluminum and molybdenum show signs of high bias. There was no observed bias, as determined using the standard reference materials, during the analysis of lead.
Burnett, Andrew D; Fan, Wenhui; Upadhya, Prashanth C; Cunningham, John E; Hargreaves, Michael D; Munshi, Tasnim; Edwards, Howell G M; Linfield, Edmund H; Davies, A Giles
2009-08-01
Terahertz frequency time-domain spectroscopy has been used to analyse a wide range of samples containing cocaine hydrochloride, heroin and ecstasy--common drugs-of-abuse. We investigated real-world samples seized by law enforcement agencies, together with pure drugs-of-abuse, and pure drugs-of-abuse systematically adulterated in the laboratory to emulate real-world samples. In order to investigate the feasibility of automatic spectral recognition of such illicit materials by terahertz spectroscopy, principal component analysis was employed to cluster spectra of similar compounds.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Oji, L. N.; Reboul, S. H.
The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) Engineering (SRR-E) to provide sample characterization and analyses of Tank 51 sludge samples in support of Sludge Batch (SB) 10. The six Tank 51 sludge samples were sampled and delivered to SRNL in August of 2017. These six Tank 51 sludge samples, after undergoing physical characterizations which included rheology, weight percent total solid, dissolved solids and density measurements, were combined into one composite Tank 51 sample and analyzed for corrosion controls analytes, select radionuclides, chemical elements, density and weight percent total solids.
Clandestine laboratory scene investigation and processing using portable GC/MS
NASA Astrophysics Data System (ADS)
Matejczyk, Raymond J.
1997-02-01
This presentation describes the use of portable gas chromatography/mass spectrometry for on-scene investigation and processing of clandestine laboratories. Clandestine laboratory investigations present special problems to forensic investigators. These crime scenes contain many chemical hazards that must be detected, identified and collected as evidence. Gas chromatography/mass spectrometry performed on-scene with a rugged, portable unit is capable of analyzing a variety of matrices for drugs and chemicals used in the manufacture of illicit drugs, such as methamphetamine. Technologies used to detect various materials at a scene have particular applications but do not address the wide range of samples, chemicals, matrices and mixtures that exist in clan labs. Typical analyses performed by GC/MS are for the purpose of positively establishing the identity of starting materials, chemicals and end-product collected from clandestine laboratories. Concerns for the public and investigator safety and the environment are also important factors for rapid on-scene data generation. Here is described the implementation of a portable multiple-inlet GC/MS system designed for rapid deployment to a scene to perform forensic investigations of clandestine drug manufacturing laboratories. GC/MS has long been held as the 'gold standard' in performing forensic chemical analyses. With the capability of GC/MS to separate and produce a 'chemical fingerprint' of compounds, it is utilized as an essential technique for detecting and positively identifying chemical evidence. Rapid and conclusive on-scene analysis of evidence will assist the forensic investigators in collecting only pertinent evidence thereby reducing the amount of evidence to be transported, reducing chain of custody concerns, reducing costs and hazards, maintaining sample integrity and speeding the completion of the investigative process.
Study of activation of metal samples from LDEF-1 and Spacelab-2
NASA Technical Reports Server (NTRS)
Laird, C. E.
1991-01-01
The activation of metal samples and other material orbited onboard the Long Duration Exposure Facility (LDEF) and Spacelab-2 were studied. Measurements of the radioactivities of spacecraft materials were made, and corrections for self-absorption and efficiency were calculated. Activation cross sections for specific metal samples were updated while cross sections for other materials were tabulated from the scientific literature. Activation cross sections for 200 MeV neutrons were experimentally determined. Linear absorption coefficients, half lives, branching ratios and other pertinent technical data needed for LDEF sample analyses were tabulated. The status of the sample counting at low background facilities at national laboratories is reported.
Beam tracking phase tomography with laboratory sources
NASA Astrophysics Data System (ADS)
Vittoria, F. A.; Endrizzi, M.; Kallon, G. K. N.; Hagen, C. K.; Diemoz, P. C.; Zamir, A.; Olivo, A.
2018-04-01
An X-ray phase-contrast laboratory system is presented, based on the beam-tracking method. Beam-tracking relies on creating micro-beamlets of radiation by placing a structured mask before the sample, and analysing them by using a detector with sufficient resolution. The system is used in tomographic configuration to measure the three dimensional distribution of the linear attenuation coefficient, difference from unity of the real part of the refractive index, and of the local scattering power of specimens. The complementarity of the three signals is investigated, together with their potential use for material discrimination.
Tempestilli, Massimo; Pucci, Luigia; Notari, Stefania; Di Caro, Antonino; Castilletti, Concetta; Rivelli, Maria Rosaria; Agrati, Chiara; Pucillo, Leopoldo Paolo
2015-11-01
Ebola virus, an enveloped virus, is the cause of the largest and most complex Ebola virus disease (EVD) outbreak in West Africa. Blood or body fluids of an infected person may represent a biohazard to laboratory workers. Laboratory tests of virus containing specimens should be conducted in referral centres at biosafety level 4, but based on the severity of clinical symptoms, basic laboratories might be required to execute urgent tests for patients suspected of EVD. The aim of this work was to compare the analytical performances of laboratory tests when Triton X-100, a chemical agent able to inactivate other enveloped viruses, was added to specimens. Results of clinical chemistry, coagulation and haematology parameters on samples before and after the addition of 0.1% (final concentration) of Triton X-100 and 1 h of incubation at room temperature were compared. Overall, results showed very good agreement by all statistical analyses. Triton X-100 at 0.1% did not significantly affect the results for the majority of the analytes tested. Triton X-100 at 0.1% can be used to reduce the biohazard in performing laboratory tests on samples from patients with EVD without affecting clinical decisions.
An inter-laboratory comparison study on transfer, persistence and recovery of DNA from cable ties.
Steensma, Kristy; Ansell, Ricky; Clarisse, Lindy; Connolly, Edward; Kloosterman, Ate D; McKenna, Louise G; van Oorschot, Roland A H; Szkuta, Bianca; Kokshoorn, Bas
2017-11-01
To address questions on the activity that led to the deposition of biological traces in a particular case, general information on the probabilities of transfer, persistence and recovery of cellular material in relevant scenarios is necessary. These figures may be derived from experimental data described in forensic literature when conditions relevant to the case were included. The experimental methodology regarding sampling, DNA extraction, DNA typing and profile interpretation that were used to generate these published data may differ from those applied in the case and thus the applicability of the literature data may be questioned. To assess the level of variability that different laboratories obtain when similar exhibits are analysed, we performed an inter-laboratory study between four partner laboratories. Five sets of 20 cable ties bound by different volunteers were distributed to the participating laboratories and sampled and processed according to the in-house protocols. Differences were found for the amount of retrieved DNA, as well as for the reportability and composition of the DNA profiles. These differences also resulted in different probabilities of transfer, persistence and recovery for each laboratory. Nevertheless, when applied to a case example, these differences resulted in similar assignments of weight of evidence given activity-level propositions. Copyright © 2017 Elsevier B.V. All rights reserved.
Kubachka, Kevin; Heitkemper, Douglas T; Conklin, Sean
2017-07-01
Before being designated AOAC First Action Official MethodSM 2016.04, the U.S. Food and Drug Administration's method, EAM 4.10 High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometric Determination of Four Arsenic Species in Fruit Juice, underwent both a single-laboratory validation and a multilaboratory validation (MLV) study. Three federal and five state regulatory laboratories participated in the MLV study, which is the primary focus of this manuscript. The method was validated for inorganic arsenic (iAs) measured as the sum of the two iAs species arsenite [As(III)] and arsenate [As(V)], dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) by analyses of 13 juice samples, including three apple juice, three apple juice concentrate, four grape juice, and three pear juice samples. In addition, two water Standard Reference Materials (SRMs) were analyzed. The method LODs and LOQs obtained among the eight laboratories were approximately 0.3 and 2 ng/g, respectively, for each of the analytes and were adequate for the intended purpose of the method. Each laboratory analyzed method blanks, fortified method blanks, reference materials, triplicate portions of each juice sample, and duplicate fortified juice samples (one for each matrix type) at three fortification levels. In general, repeatability and reproducibility of the method was ≤15% RSD for each species present at a concentration >LOQ. The average recovery of fortified analytes for all laboratories ranged from 98 to 104% iAs, DMA, and MMA for all four juice sample matrixes. The average iAs results for SRMs 1640a and 1643e agreed within the range of 96-98% of certified values for total arsenic.
Federal Register 2010, 2011, 2012, 2013, 2014
2010-08-30
... enhance the lab capabilities to handle human pathogenic bacteria in animal feed. DATES: Important dates... supplemental grant funds will enable analyses of human pathogenic bacteria found in animal feed, for samples... bacteria in animal feed. This additional program will be compatible with other FERN Cooperative Agreement...
Lee, Hye-Seung; Burkhardt, Brant R; McLeod, Wendy; Smith, Susan; Eberhard, Chris; Lynch, Kristian; Hadley, David; Rewers, Marian; Simell, Olli; She, Jin-Xiong; Hagopian, Bill; Lernmark, Ake; Akolkar, Beena; Ziegler, Anette G; Krischer, Jeffrey P
2014-07-01
The Environmental Determinants of Diabetes in the Young planned biomarker discovery studies on longitudinal samples for persistent confirmed islet cell autoantibodies and type 1 diabetes using dietary biomarkers, metabolomics, microbiome/viral metagenomics and gene expression. This article describes the details of planning The Environmental Determinants of Diabetes in the Young biomarker discovery studies using a nested case-control design that was chosen as an alternative to the full cohort analysis. In the frame of a nested case-control design, it guides the choice of matching factors, selection of controls, preparation of external quality control samples and reduction of batch effects along with proper sample allocation. Our design is to reduce potential bias and retain study power while reducing the costs by limiting the numbers of samples requiring laboratory analyses. It also covers two primary end points (the occurrence of diabetes-related autoantibodies and the diagnosis of type 1 diabetes). The resulting list of case-control matched samples for each laboratory was augmented with external quality control samples. Copyright © 2013 John Wiley & Sons, Ltd.
The present and future of microplastic pollution in the marine environment.
Ivar do Sul, Juliana A; Costa, Monica F
2014-02-01
Recently, research examining the occurrence of microplastics in the marine environment has substantially increased. Field and laboratory work regularly provide new evidence on the fate of microplastic debris. This debris has been observed within every marine habitat. In this study, at least 101 peer-reviewed papers investigating microplastic pollution were critically analysed (Supplementary material). Microplastics are commonly studied in relation to (1) plankton samples, (2) sandy and muddy sediments, (3) vertebrate and invertebrate ingestion, and (4) chemical pollutant interactions. All of the marine organism groups are at an eminent risk of interacting with microplastics according to the available literature. Dozens of works on other relevant issues (i.e., polymer decay at sea, new sampling and laboratory methods, emerging sources, externalities) were also analysed and discussed. This paper provides the first in-depth exploration of the effects of microplastics on the marine environment and biota. The number of scientific publications will increase in response to present and projected plastic uses and discard patterns. Therefore, new themes and important approaches for future work are proposed. Copyright © 2013 Elsevier Ltd. All rights reserved.
Blood analyses of wolf pups and their ecological and metabolic interpretation
Seal, U.S.; Mech, L.D.; Van Ballenberghe, V.
1975-01-01
Blood samples were obtained from 32 wolf (Canis lupus) pups live-trapped over a three-year period in northern Minnesota. The results of 21 laboratory analyses of hematology and blood chemistry are tabulated and analyzed in terms of study area, age, sex, and year of co11ection. Mean values are compared to those reported for dogs in the same age group. The numerous differences between dog and wolf pups are interpreted in terms of nutritional levels and dietary composition with the suggestion that the wolves are not achieving their full growth potential. Individual abnormal test results are tabulated and possible interpretations are suggested. Abnormal results were observed in 13 animals including 10 of 11 animals sampled in 1972. The results in the 1972 animals indicated a poorer nutrition. This preponderance of abnormal test results in pups from 1972 is correlated with ecological studies on this wolf population indicating decreased survival. The potential value of such long-term integrated field and laboratory studies for providing a more complete understanding of changes in the dynamics of natural populations in terms of the responses of individual animals is demonstrated.
2014-09-30
axis and physiological processes driven by the GCs are essential for an individual’s ability to respond and adapt to stress, prolonged elevation of...health assessments. Stress and reproductive hormones (cortisol, aldosterone , thyroid, testosterone, progesterone) have been routinely measured in blood...in South Carolina. Laboratory Analyses Hormone concentrations (cortisol, aldosterone , reproductive and thyroid hormones) in serum samples have
NASA Technical Reports Server (NTRS)
Allen, Carlton; Sellar, Glenn; Nunez, Jorge; Mosie, Andrea; Schwarz, Carol; Parker, Terry; Winterhalter, Daniel; Farmer, Jack
2009-01-01
Astronauts on long-duration lunar missions will need the capability to high-grade their samples to select the highest value samples for transport to Earth and to leave others on the Moon. We are supporting studies to define the necessary and sufficient measurements and techniques for high-grading samples at a lunar outpost. A glovebox, dedicated to testing instruments and techniques for high-grading samples, is in operation at the JSC Lunar Experiment Laboratory. A reference suite of lunar rocks and soils, spanning the full compositional range found in the Apollo collection, is available for testing in this laboratory. Thin sections of these samples are available for direct comparison. The Lunar Sample Compendium, on-line at http://www-curator.jsc.nasa.gov/lunar/compendium.cfm, summarizes previous analyses of these samples. The laboratory, sample suite, and Compendium are available to the lunar research and exploration community. In the first test of possible instruments for lunar sample high-grading, we imaged 18 lunar rocks and four soils from the reference suite using the Multispectral Microscopic Imager (MMI) developed by Arizona State University and JPL (see Farmer et. al. abstract). The MMI is a fixed-focus digital imaging system with a resolution of 62.5 microns/pixel, a field size of 40 x 32 mm, and a depth-of-field of approximately 5 mm. Samples are illuminated sequentially by 21 light emitting diodes in discrete wavelengths spanning the visible to shortwave infrared. Measurements of reflectance standards and background allow calibration to absolute reflectance. ENVI-based software is used to produce spectra for specific minerals as well as multi-spectral images of rock textures.
Human exploration of Mars - The role of a Mars outpost laboratory
NASA Technical Reports Server (NTRS)
Duke, Michael B.
1992-01-01
Consideration is given to a Martian exploration strategy which includes intensive robotic reconnaissance to characterize features of Mars' geology that are important to the solution of major problems of Mars history, including the possible past presence of life. A human reconnaissance phase may follow the robotic reconnaissance phase, guided to the most productive sites by the results of the robotic missions. The strategy also involves an intensive human phase of investigation, with interactive field geology/laboratory investigation at the Mars outpost. The laboratory investigations, as well as the field work, should be highly interactive with a broad scientific community on earth. The most detailed analyses would be performed on samples returned to earth.
Examination Of Sulfur Measurements In DWPF Sludge Slurry And SRAT Product Materials
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bannochie, C. J.; Wiedenman, B. J.
2012-11-29
Savannah River National Laboratory (SRNL) was asked to re-sample the received SB7b WAPS material for wt. % solids, perform an aqua regia digestion and analyze the digested material by inductively coupled plasma - atomic emission spectroscopy (ICP-AES), as well as re-examine the supernate by ICP-AES. The new analyses were requested in order to provide confidence that the initial analytical subsample was representative of the Tank 40 sample received and to replicate the S results obtained on the initial subsample collected. The ICP-AES analyses for S were examined with both axial and radial detection of the sulfur ICP-AES spectroscopic emission linesmore » to ascertain if there was any significant difference in the reported results. The outcome of this second subsample of the Tank 40 WAPS material is the first subject of this report. After examination of the data from the new subsample of the SB7b WAPS material, a team of DWPF and SRNL staff looked for ways to address the question of whether there was in fact insoluble S that was not being accounted for by ion chromatography (IC) analysis. The question of how much S is reaching the melter was thought best addressed by examining a DWPF Slurry Mix Evaporator (SME) Product sample, but the significant dilution of sludge material, containing the S species in question, that results from frit addition was believed to add additional uncertainty to the S analysis of SME Product material. At the time of these discussions it was believed that all S present in a Sludge Receipt and Adjustment Tank (SRAT) Receipt sample would be converted to sulfate during the course of the SRAT cycle. A SRAT Product sample would not have the S dilution effect resulting from frit addition, and hence, it was decided that a DWPF SRAT Product sample would be obtained and submitted to SRNL for digestion and sample preparation followed by a round-robin analysis of the prepared samples by the DWPF Laboratory, F/H Laboratories, and SRNL for S and sulfate. The results of this round-robin analytical study are the second subject of this report.« less
40 CFR 270.63 - Permits for land treatment demonstrations using field test or laboratory analyses.
Code of Federal Regulations, 2011 CFR
2011-07-01
... demonstrations using field test or laboratory analyses. 270.63 Section 270.63 Protection of Environment... using field test or laboratory analyses. (a) For the purpose of allowing an owner or operator to meet... the field test or laboratory analyses, or as a two-phase facility permit covering the field tests, or...
40 CFR 270.63 - Permits for land treatment demonstrations using field test or laboratory analyses.
Code of Federal Regulations, 2010 CFR
2010-07-01
... demonstrations using field test or laboratory analyses. 270.63 Section 270.63 Protection of Environment... using field test or laboratory analyses. (a) For the purpose of allowing an owner or operator to meet... the field test or laboratory analyses, or as a two-phase facility permit covering the field tests, or...
40 CFR 270.63 - Permits for land treatment demonstrations using field test or laboratory analyses.
Code of Federal Regulations, 2014 CFR
2014-07-01
... demonstrations using field test or laboratory analyses. 270.63 Section 270.63 Protection of Environment... using field test or laboratory analyses. (a) For the purpose of allowing an owner or operator to meet... the field test or laboratory analyses, or as a two-phase facility permit covering the field tests, or...
40 CFR 270.63 - Permits for land treatment demonstrations using field test or laboratory analyses.
Code of Federal Regulations, 2013 CFR
2013-07-01
... demonstrations using field test or laboratory analyses. 270.63 Section 270.63 Protection of Environment... using field test or laboratory analyses. (a) For the purpose of allowing an owner or operator to meet... the field test or laboratory analyses, or as a two-phase facility permit covering the field tests, or...
40 CFR 270.63 - Permits for land treatment demonstrations using field test or laboratory analyses.
Code of Federal Regulations, 2012 CFR
2012-07-01
... demonstrations using field test or laboratory analyses. 270.63 Section 270.63 Protection of Environment... using field test or laboratory analyses. (a) For the purpose of allowing an owner or operator to meet... the field test or laboratory analyses, or as a two-phase facility permit covering the field tests, or...
DOE Office of Scientific and Technical Information (OSTI.GOV)
McDonald, Benjamin S.; Zalavadia, Mital A.; Miller, Brian W.
Environmental sampling and sample analyses by the International Atomic Energy Agency’s (IAEA) Network of Analytical Laboratories (NWAL) is a critical technical tool used to detect facility misuse under a Comprehensive Safeguards Agreement and to verify the absence of undeclared nuclear material activities under an Additional Protocol. Currently all environmental swipe samples (ESS) are screened using gamma spectrometry and x-ray fluorescence to estimate the amount of U and/or Pu in the ESS, to guide further analysis, and to assist in the shipment of ESS to the NWAL. Quantitative Digital Autoradiography for Environmental Samples (QDARES) is being developed to complement existing techniquesmore » through the use of a portable, real-time, high-spatial-resolution camera called the Ionizing-radiation Quantum Imaging Detector (iQID). The iQID constructs a spatial map of radionuclides within a sample or surface in real-time as charged particles (betas) and photons (gamma/x-rays) are detected and localized on an event-by-event basis. Knowledge of the location and nature of radioactive hot spots on the ESS could provide information for subsequent laboratory analysis. As a nondestructive technique, QDARES does not compromise the ESS chain of custody or subsequent laboratory analysis. In this paper we will present the system design and construction, characterization measurements with calibration sources, and initial measurements of ESS.« less
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 2003 through June 2005. Results for the quality-control samples for 20 analytical procedures were evaluated for bias and precision. Control charts indicate that data for five 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, pH, silicon, and sodium. Seven of the analytical procedures were biased throughout the analysis period for the high-concentration sample, but were within control limits; these procedures were: dissolved organic carbon, chloride, nitrate (ion chromatograph), nitrite, silicon, sodium, and sulfate. The calcium and magnesium procedures were biased throughout the analysis period for the low-concentration sample, but were within control limits. The total aluminum 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 indicate that the procedures for 17 of 18 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 22 analytes. At least 85 percent of the samples met data-quality objectives for all analytes except total monomeric aluminum (82 percent of samples met objectives), total aluminum (77 percent of samples met objectives), chloride (80 percent of samples met objectives), fluoride (76 percent of samples met objectives), and nitrate (ion chromatograph) (79 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 indicated good data quality over the time period, with ratings for each sample in the satisfactory, good, and excellent ranges or less than 10 percent error. The P-sample (low-ionic-strength constituents) analysis had one marginal and two unsatisfactory ratings for the chloride procedure. The T-sample (trace constituents)analysis had two unsatisfactory ratings and one high range percent error for the aluminum procedure. The N-sample (nutrient constituents) analysis had one marginal rating for the nitrate procedure. Results of Environment Canada's National Water Research Institute (NWRI) program indicated that at least 84 percent of the samples met data-quality objectives for 11 of the 14 analytes; the exceptions were ammonium, total aluminum, and acid-neutralizing capacity. The ammonium procedure did not meet data quality objectives in all studies. Data-quality objectives were not met in 23 percent of samples analyzed for total aluminum and 45 percent of samples analyzed acid-neutralizing capacity. Results from blind reference-sample analyses indicated that data-quality objectives were met by at least 86 percent of the samples analyzed for calcium, chloride, fluoride, magnesium, pH, potassium, sodium, and sulfate. Data-quality objectives were not met by samples analyzed for fluoride.
Horowitz, A.J.; Smith, J.J.; Elrick, K.A.
2001-01-01
A prototype 14-L Teflon? churn splitter was evaluated for whole-water sample-splitting capabilities over a range of sediment concentratons and grain sizes as well as for potential chemical contamination from both organic and inorganic constituents. These evaluations represent a 'best-case' scenario because they were performed in the controlled environment of a laboratory, and used monomineralic silica sand slurries of known concentration made up in deionized water. Further, all splitting was performed by a single operator, and all the requisite concentration analyses were performed by a single laboratory. The prototype Teflon? churn splitter did not appear to supply significant concentrations of either organic or inorganic contaminants at current U.S. Geological Survey (USGS) National Water Quality Laboratory detection and reporting limits when test samples were prepared using current USGS protocols. As with the polyethylene equivalent of the prototype Teflon? churn, the maximum usable whole-water suspended sediment concentration for the prototype churn appears to lie between 1,000 and 10,000 milligrams per liter (mg/L). Further, the maximum grain-size limit appears to lie between 125- and 250-microns (m). Tests to determine the efficacy of the valve baffle indicate that it must be retained to facilitate representative whole-water subsampling.
NASA Technical Reports Server (NTRS)
Greenbauer-Seng, L. A.
1983-01-01
The accurate determination of trace metals and fuels is an important requirement in much of the research into and development of alternative fuels for aerospace applications. Recognizing the detrimental effects of certain metals on fuel performance and fuel systems at the part per million and in some cases part per billion levels requires improved accuracy in determining these low concentration elements. Accurate analyses are also required to ensure interchangeability of analysis results between vendor, researcher, and end use for purposes of quality control. Previous interlaboratory studies have demonstrated the inability of different laboratories to agree on the results of metal analysis, particularly at low concentration levels, yet typically good precisions are reported within a laboratory. An interlaboratory study was designed to gain statistical information about the sources of variation in the reported concentrations. Five participant laboratories were used on a fee basis and were not informed of the purpose of the analyses. The effects of laboratory, analytical technique, concentration level, and ashing additive were studied in four fuel types for 20 elements of interest. The prescribed sample preparation schemes (variations of dry ashing) were used by all of the laboratories. The analytical data were statistically evaluated using a computer program for the analysis of variance technique.
Loper, Connie A.; Crawford, J. Kent; Otto, Kim L.; Manning, Rhonda L.; Meyer, Michael T.; Furlong, Edward T.
2007-01-01
This report presents environmental and quality-control data from analyses of 15 pharmaceutical and 31 antibiotic compounds in water samples from streams and wells in south-central Pennsylvania. The analyses are part of a study by the U.S. Geological Survey (USGS) in cooperation with the Pennsylvania Department of Environmental Protection (PADEP) to define concentrations of selected emerging contaminants in streams and well water in Pennsylvania. Sampling was conducted at 11 stream sites and at 6 wells in 9 counties of south-central Pennsylvania. Five of the streams received municipal wastewater and 6 of the streams received runoff from agricultural areas dominated by animal-feeding operations. For all 11 streams, samples were collected at locations upstream and downstream of the municipal effluents or animal-feeding operations. All six wells were in agricultural settings. A total of 120 environmental samples and 21 quality-control samples were analyzed for the study. Samples were collected at each site in March/April, May, July, and September 2006 to obtain information on changes in concentration that could be related to seasonal use of compounds.For streams, 13 pharmaceuticals and 11 antibiotics were detected at least 1 time. Detections included analytical results that were estimated or above the minimum reporting limits. Seventy-eight percent of all detections were analyzed in samples collected downstream from municipal-wastewater effluents. For streams receiving wastewater effluents, the pharmaceuticals caffeine and para-xanthine (a degradation product of caffeine) had the greatest concentrations, 4.75 μg/L (micrograms per liter) and 0.853 μg/L, respectively. Other pharmaceuticals and their respective maximum concentrations were carbamazepine (0.516 μg/L) and ibuprofen (0.277 μg/L). For streams receiving wastewater effluents, the antibiotic azithromycin had the greatest concentration (1.65 μg/L), followed by sulfamethoxazole (1.34 μg/L), ofloxacin (0.329 μg/L), and trimethoprim (0.256 μg/L).For streams receiving runoff from animal-feeding operations, the only pharmaceuticals detected were acetaminophen, caffeine, cotinine, diphenhydramine, and carbamazepine. The maximum concentration for pharmaceuticals was 0.053 μg/L. Three streams receiving runoff from animal-feeding operations had detections of one or more antibiotic compound--oxytetracycline, sulfadimethoxine, sulfamethoxazole, and tylosin. The maximum concentration for antibiotics was 0.157 μg/L. The average number of compounds (pharmaceuticals and antibiotics) detected in sites downstream from animal-feeding operations was three. The average number of compounds detected downstream from municipal-wastewater effluents was 13.For wells used to supply livestock, four compounds were detected--two pharmaceuticals (cotinine and diphenhydramine) and two antibiotics (tylosin and sulfamethoxazole). There were five detections in all the well samples. The maximum concentration detected in well water was for cotinine, estimated to be 0.024 μg/L.Seasonal occurrence of pharmaceutical and antibiotic compounds in stream water varied by compound and site type. At four stream sites, the same compounds were detected in all four seasonal samples. At other sites, pharmaceutical or antibiotic compounds were detected only one time in seasonal samples. Winter samples collected in streams receiving municipalwastewater effluent had the greatest number of compounds detected (21). Research analytical methods were used to determine concentrations for pharmaceuticals and antibiotics. To assist in evaluating the quality of the analyses, detailed information is presented on laboratory methodology and results from qualitycontrol samples. Quality-control data include results for nine blanks, nine duplicate environmental sample pairs, and three laboratory-spiked environmental samples as well as the recoveries of compounds in laboratory surrogates and laboratory reagent spikes.
Tobe, Shanan S; Bailey, Stuart; Govan, James; Welch, Lindsey A
2013-03-01
Although poaching is a common wildlife crime, the high and prohibitive cost of specialised animal testing means that many cases are left un-investigated. We previously described a novel approach to wildlife crime investigation that looked at the identification of human DNA on poached animal remains (Tobe, Govan and Welch, 2011). Human DNA was successfully isolated and amplified from simulated poaching incidents, however a low template protocol was required which made this method unsuitable for use in many laboratories. We now report on an optimised recovery and amplification protocol which removes the need for low template analysis. Samples from 10 deer (40 samples total - one from each leg) analysed in the original study were re-analysed in the current study with an additional 11 deer samples. Four samples analysed using Chelex did not show any results and a new method was devised whereby the available DNA was concentrated. By combining the DNA extracts from all tapings of the same deer remains followed by concentration, the recovered quantity of human DNA was found to be 29.5pg±43.2pg, 31× greater than the previous study. The use of the Investigator Decaplex SE (QIAGEN) STR kit provided better results in the form of more complete profiles than did the AmpFℓSTR® SGM Plus® kit at 30cycles (Applied Biosystems). Re-analysis of the samples from the initial study using the new, optimised protocol resulted in an average increase of 18% of recovered alleles. Over 17 samples, 71% of the samples analysed using the optimised protocol showed sufficient amplification for comparison to a reference profile and gave match probabilities ranging from 7.7690×10(-05) to 2.2706×10(-14). The removal of low template analysis means this optimised method provides evidence of high probative value and is suitable for immediate use in forensic laboratories. All methods and techniques used are standard and are compatible with current SOPs. As no high cost non-human DNA analysis is required the overall process is no more expensive than the investigation of other volume crime samples. The technique is suitable for immediate use in poaching incidents. Copyright © 2012 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.
Evaluation of dredged material proposed for ocean disposal from Hudson River, New York
DOE Office of Scientific and Technical Information (OSTI.GOV)
Gardiner, W.W.; Barrows, E.S.; Antrim, L.D.
1996-09-01
The Hudson River (Federal Project No. 41) was one of seven waterways that the U.S. Army Corps of Engineers-New York District (USACE-NYD) requested the Battelle Marine Sciences Laboratory (MSL) to sample and evaluate for dredging and disposal in March 1994. Sediment samples were collected from the Hudson River. Tests and analyses were conducted on Hudson River sediment core samples. The evaluation of proposed dredged material from the Hudson River 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 collected from Hudson River were analyzedmore » for grain size, moisture content, and total organic carbon (TOC). A composite sediment sample, representing the entire area proposed for dredging, was analyzed for bulk density, specific gravity, metals, chlorinated pesticides, polychlorinated biphenyl (PCB) congeners, polynuclear aromatic hydrocarbons (PAH), and 1,4-dichlorobenzene. Site water and elutriate water, prepared from the suspended-particulate phase (SPP) of Hudson River sediment, were analyzed for metals, pesticides, and PCBS. Water-column or SPP toxicity tests were performed with three species. Benthic acute toxicity tests were performed. Bioaccumulation tests were also conducted.« less
Discrepancies in reporting the CAG repeat lengths for Huntington's disease
Quarrell, Oliver W; Handley, Olivia; O'Donovan, Kirsty; Dumoulin, Christine; Ramos-Arroyo, Maria; Biunno, Ida; Bauer, Peter; Kline, Margaret; Landwehrmeyer, G Bernhard
2012-01-01
Huntington's disease results from a CAG repeat expansion within the Huntingtin gene; this is measured routinely in diagnostic laboratories. The European Huntington's Disease Network REGISTRY project centrally measures CAG repeat lengths on fresh samples; these were compared with the original results from 121 laboratories across 15 countries. We report on 1326 duplicate results; a discrepancy in reporting the upper allele occurred in 51% of cases, this reduced to 13.3% and 9.7% when we applied acceptable measurement errors proposed by the American College of Medical Genetics and the Draft European Best Practice Guidelines, respectively. Duplicate results were available for 1250 lower alleles; discrepancies occurred in 40% of cases. Clinically significant discrepancies occurred in 4.0% of cases with a potential unexplained misdiagnosis rate of 0.3%. There was considerable variation in the discrepancy rate among 10 of the countries participating in this study. Out of 1326 samples, 348 were re-analysed by an accredited diagnostic laboratory, based in Germany, with concordance rates of 93% and 94% for the upper and lower alleles, respectively. This became 100% if the acceptable measurement errors were applied. The central laboratory correctly reported allele sizes for six standard reference samples, blind to the known result. Our study differs from external quality assessment (EQA) schemes in that these are duplicate results obtained from a large sample of patients across the whole diagnostic range. We strongly recommend that laboratories state an error rate for their measurement on the report, participate in EQA schemes and use reference materials regularly to adjust their own internal standards. PMID:21811303
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 2001 through June 2003. Results for the quality-control samples for 19 analytical procedures were evaluated for bias and precision. Control charts indicate that data for six 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, chloride, magnesium, nitrate (ion chromatography), potassium, and sodium. The calcium procedure was biased throughout the analysis period for the high-concentration sample, but was within control limits. The total monomeric aluminum and fluoride procedures were biased throughout the analysis period for the low-concentration sample, but were within control limits. The total aluminum, pH, specific conductance, and sulfate 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 indicate that the procedures for 16 of 18 analytes were within control limits, although the concentrations for blanks were occasionally outside the control limits. The data-quality objective was not met for the dissolved organic carbon or specific conductance procedures. 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 90 percent of the samples met data-quality objectives for all procedures except total monomeric aluminum (83 percent of samples met objectives), total aluminum (76 percent of samples met objectives), ammonium (73 percent of samples met objectives), dissolved organic carbon (86 percent of samples met objectives), and nitrate (81 percent of samples met objectives). The data-quality objective was not met for the nitrite procedure. Results of the USGS interlaboratory Standard Reference Sample (SRS) Project indicated satisfactory or above data quality over the time period, with most performance ratings for each sample in the good-to-excellent range. The N-sample (nutrient constituents) analysis had one unsatisfactory rating for the ammonium procedure in one study. The T-sample (trace constituents) analysis had one unsatisfactory rating for the magnesium procedure and one marginal rating for the potassium procedure in one study and one unsatisfactory rating for the sodium procedure in another. Results of Environment Canada's National Water Research Institute (NWRI) program indicated that at least 90 percent of the samples met data-quality objectives for 10 of the 14 analytes; the exceptions were acid-neutralizing capacity, ammonium, dissolved organic carbon, and sodium. Data-quality objectives were not met in 37 percent of samples analyzed for acid-neutralizing capacity, 28 percent of samples analyzed for dissolved organic carbon, and 30 percent of samples analyzed for sodium. Results indicate a positive bias for the ammonium procedure in one study and a negative bias in another. Results from blind reference-sample analyses indicated that data-quality objectives were met by at least 90 percent of the samples analyzed for calcium, chloride, magnesium, pH, potassium, and sodium. Data-quality objectives were met by 78 percent of
Gray, James L.; Kanagy, Leslie K.; Furlong, Edward T.; McCoy, Jeff W.; Kanagy, Chris J.
2011-01-01
On April 22, 2010, the explosion on and subsequent sinking of the Deepwater Horizon oil drilling platform resulted in the release of crude oil into the Gulf of Mexico. At least 4.4 million barrels had been released into the Gulf of Mexico through July 15, 2010, 10 to 29 percent of which was chemically dispersed, primarily using two dispersant formulations. Initially, the dispersant Corexit 9527 was used, and when existing stocks of that formulation were exhausted, Corexit 9500 was used. Over 1.8 million gallons of the two dispersants were applied in the first 3 months after the spill. This report presents the development of an analytical method to analyze one of the primary surfactant components of both Corexit formulations, di(ethylhexyl) sodium sulfosuccinate (DOSS), the preliminary results, and the associated quality assurance/quality control (QA/QC) from samples collected from various points on the Gulf Coast between Texas and Florida. Seventy water samples and 8 field QC samples were collected before the predicted landfall of oil (pre-landfall) on the Gulf Coast, and 51 water samples and 10 field QC samples after the oil made landfall (post-landfall). Samples were collected in Teflon(Registered) bottles and stored at -20(degrees)C until analysis. Extraction of whole-water samples used sorption onto a polytetrafluoroethylene (PTFE) filter to isolate DOSS, with subsequent 50 percent methanol/water elution of the combined dissolved and particulate DOSS fractions. High-performance liquid chromatography/tandem mass spectrometry (LC/MS/MS) was used to identify and quantify DOSS by the isotope dilution method, using a custom-synthesized 13C4-DOSS labeled standard. Because of the ubiquitous presence of DOSS in laboratory reagent water, a chromatographic column was installed in the LC/MS/MS between the system pumps and the sample injector that separated this ambient background DOSS contamination from the sample DOSS, minimizing one source of blank contamination. Laboratory and field QA/QC for pre-landfall samples included laboratory reagent spike and blank samples, a total of 34 replicate analyses for the 78 environmental and field blank samples, and 11 randomly chosen laboratory matrix spike samples. Laboratory and field QA/QC for post-landfall samples included laboratory reagent spike and blank samples, a laboratory 'in-bottle' duplicate for each sample, and analysis of 24 randomly chosen laboratory matrix spike samples. Average DOSS recovery of 89(+/-)9.5 percent in all native (non-13C4-DOSS ) spikes was observed, with a mean relative percent difference between sample duplicates of 36 percent. The reporting limit for this analysis was 0.25 micrograms per liter due to blank limitations; DOSS was not detected in any samples collected in October (after oil landfall at certain study sites) above that concentration. It was detected prior to oil landfall above 0.25 micrograms per liter in 3 samples, but none exceeded the Environmental Protection Agency aquatic life criteria of 40 micrograms per liter.
Anderson, Kim A.; Seck, Dogo; Hobbie, Kevin A.; Traore, Anna Ndiaye; McCartney, Melissa A.; Ndaye, Adama; Forsberg, Norman D.; Haigh, Theodore A.; Sower, Gregory J.
2014-01-01
It is difficult to assess pollution in remote areas of less-developed regions owing to the limited availability of energy, equipment, technology, trained personnel and other key resources. Passive sampling devices (PSDs) are technologically simple analytical tools that sequester and concentrate bioavailable organic contaminants from the environment. Scientists from Oregon State University and the Centre Régional de Recherches en Ecotoxicologie et de Sécurité Environnementale (CERES) in Senegal developed a partnership to build capacity at CERES and to develop a pesticide-monitoring project using PSDs. This engagement resulted in the development of a dynamic training process applicable to capacity-building programmes. The project culminated in a field and laboratory study where paired PSD samples were simultaneously analysed in African and US laboratories with quality control evaluation and traceability. The joint study included sampling from 63 sites across six western African countries, generating a 9000 data point pesticide database with virtual access to all study participants. PMID:24535398
Anderson, Kim A; Seck, Dogo; Hobbie, Kevin A; Traore, Anna Ndiaye; McCartney, Melissa A; Ndaye, Adama; Forsberg, Norman D; Haigh, Theodore A; Sower, Gregory J
2014-04-05
It is difficult to assess pollution in remote areas of less-developed regions owing to the limited availability of energy, equipment, technology, trained personnel and other key resources. Passive sampling devices (PSDs) are technologically simple analytical tools that sequester and concentrate bioavailable organic contaminants from the environment. Scientists from Oregon State University and the Centre Régional de Recherches en Ecotoxicologie et de Sécurité Environnementale (CERES) in Senegal developed a partnership to build capacity at CERES and to develop a pesticide-monitoring project using PSDs. This engagement resulted in the development of a dynamic training process applicable to capacity-building programmes. The project culminated in a field and laboratory study where paired PSD samples were simultaneously analysed in African and US laboratories with quality control evaluation and traceability. The joint study included sampling from 63 sites across six western African countries, generating a 9000 data point pesticide database with virtual access to all study participants.
Boscarino, Brent T.; Halpin, Kathleen E.; Rudstam, Lars G.; Walsh, Maureen G.; Lantry, Brian F.
2012-01-01
We use a combination of spectral sensitivity analyses, laboratory behavioral observations and field distributions of a vertically migrating invertebrate, Hemimysis anomala (a recent invasive species to the Laurentian Great Lakes of North America), to determine if light preference and timing of emergence has an ontogenetic component. Juvenile Hemimysis (−3.4 and 10−2.4 mylux— a Hemimysis-specific unit of brightness derived from visual pigment analyses (wavelength of maximum absorbance = 500 nm; 1 mylux ~ 159 lx). These preferred light levels are equivalent to those present during nautical twilight on the Earth's surface and were several orders of magnitude brighter than those most preferred by adults (> 4.5 mm) in the laboratory (10−6.4 to 10−7.4 mylux). Both size classes completely avoided light levels of 10−0.4 mylux and greater, which are representative of daytime light levels at the Earth's surface. Net hauls taken at ~ 20-min intervals from sunset to the end of nautical twilight on two sampling occasions on Seneca Lake, New York (sampling depth = 2 m) revealed that juveniles emerged into the water column during civil twilight. Adult Hemimysis emerged later during nautical twilight when juveniles had already reached their maximum abundance in the water column. Laboratory-derived light preferences successfully predicted the timing of emergence and time of maximal abundance of both size classes on both sampling occasions. This study is one of the first to demonstrate that Hemimysis diel vertical migration has an ontogenetic component and to report the specific light levels likely to initiate and limit vertical movements.
Ehler, Edvard; Vanek, Daniel
2017-05-01
Isolated populations present a constant threat to the correctness of forensic genetic casework. In this review article we present several examples of how analyzing samples from isolated populations can bias the results of the forensic statistics and analyses. We select our examples from isolated populations from central and southeastern Europe, namely the Valachs and the European Roma. We also provide the reader with general strategies and principles to improve the laboratory practice (best practice) and reporting of samples from supposedly isolated populations. These include reporting the precise population data used for computing the forensic statistics, using the appropriate θ correction factor for calculating allele frequencies, typing ancestry informative markers in samples of unknown or uncertain ethnicity and establishing ethnic-specific forensic databases. Copyright © 2017 Elsevier Ltd and Faculty of Forensic and Legal Medicine. All rights reserved.
The NOSAMS sample preparation laboratory in the next millenium: Progress after the WOCE program
NASA Astrophysics Data System (ADS)
Gagnon, Alan R.; McNichol, Ann P.; Donoghue, Joanne C.; Stuart, Dana R.; von Reden, Karl; Nosams
2000-10-01
Since 1991, the primary charge of the National Ocean Sciences AMS (NOSAMS) facility at the Woods Hole Oceanographic Institution has been to supply high throughput, high precision AMS 14C analyses for seawater samples collected as part of the World Ocean Circulation Experiment (WOCE). Approximately 13,000 samples taken as part of WOCE should be fully analyzed by the end of Y2K. Additional sample sources and techniques must be identified and incorporated if NOSAMS is to continue in its present operation mode. A trend in AMS today is the ability to routinely process and analyze radiocarbon samples that contain tiny amounts (<100 μg) of carbon. The capability to mass-produce small samples for 14C analysis has been recognized as a major facility goal. The installation of a new 134-position MC-SNICS ion source, which utilizes a smaller graphite target cartridge than presently used, is one step towards realizing this goal. New preparation systems constructed in the sample preparation laboratory (SPL) include an automated bank of 10 small-volume graphite reactors, an automated system to process organic carbon samples, and a multi-dimensional preparative capillary gas chromatograph (PCGC).
Flow cytometric analyses of CD34+ cells with inclusion of internal positive controls.
Gutensohn, Kai; Jessen, Maria; Ketels, Andrea; Gramatzki, Martin; Humpe, Andreas
2012-02-01
Flow cytometric measurement of CD34+ events is used to ensure the quality of human progenitor cell grafts. This study was conducted to evaluate whether the spiking of routine samples from peripheral blood and apheresis products with CD34+ positive controls is feasible. A total of 42 samples from 32 patients and one healthy donor were stained in duplicate for CD34+ cells. Before flow cytometric analysis, one tube was spiked with stabilized CD34+ cells at a defined concentration. Median numbers of viable CD34+ cells/µL did not differ between unspiked and spiked tubes (median 37, range 0-714; and median 34, range 0-719, respectively). The 95% confidence interval (CI) of the mean showed a broad overlap between these samples (41.9-119.1 and 41.4-119.3, respectively). In addition, the 95% CI of the mean for CD45+ cells/µL overlapped broadly and median numbers did not differ. Median viability of all CD45+ cells was significantly lower in the spiked tubes (96.75, range 64-98.8 vs. 99.25, range 97.5-99.8) with no overlap of the 95% CI of the mean viability. The results of this study show that spiking of routine samples with internal positive controls does not affect CD34+ cell analyses, but does support the reliability of important clinical data. The inclusion of positive controls is expedient for laboratories that perform analyses with low CD34+ numbers and laboratories that use different flow cytometric analyzers and may also become a requirement to meet statutory regulations. © 2012 American Association of Blood Banks.
A degassing instrument for analysing CO2 dissolved in natural water
NASA Astrophysics Data System (ADS)
Durham, Brian; Pfrang, Christian
2017-04-01
Arising from our EGU 2017 presentation (http://meetingorganizer.copernicus.org/EGU2016/posters/20564, X2 352), interest has been expressed in its application to the analysis of the hydrocarbonate ion [HCO3-] in atmospheric water. Arising from the historic difficulty in analysing the aqueous [HCO3-] ion ('it is in all our reagents', pers. comm. UK laboratory) the classic determination has been to measure a suite of other anions and cations including [H+] via pH, and to treat the balance of negative charge as a measure of [HCO3-]. From this balance, dissolved CO2 can be inferred via the dissociation constant as published for pure water. CO2 + H2O ⇓♢[HCO3-] + [H+] K1 = 4.2 x 10-7 Our EGU 2016 presentation sought to determine how the ionic environment in 263 UK rain samples can influence the above equilibrium, which is work in progress. In the mean time we have received the following expression of interest from an atmospheric science advisory group. …….. is very interested in the role of H-carbonate in the ion balance of precipitation. They have had some discussions recently about the best approach to infer H-carbonate currently discussing the possibility of sending you samples from other locations for analysis. We have duly offered to use our degassing instrument to corroborate current analyses in a batch of 'blind' samples, and to provide a design for a basic degasser that water quality laboratories could evaluate in house. This paper therefore presents a circuit for degassing CO2 from water samples irrespective of whether in atmospheric equilibrium or supersaturated, including a prototype 4-way distribution and collection valve which it is hoped will make the analysis intuitive and therefore open to automation.
DiFrancesco, Robin; Rosenkranz, Susan L.; Taylor, Charlene R.; Pande, Poonam G.; Siminski, Suzanne M.; Jenny, Richard W.; Morse, Gene D.
2013-01-01
Among National Institutes of Health (NIH) HIV Research Networks conducting multicenter trials, samples from protocols that span several years are analyzed at multiple clinical pharmacology laboratories (CPLs) for multiple antiretrovirals (ARV). Drug assay data are, in turn, entered into study-specific datasets that are used for pharmacokinetic analyses, merged to conduct cross-protocol pharmacokinetic analysis and integrated with pharmacogenomics research to investigate pharmacokinetic-pharmacogenetic associations. The CPLs participate in a semi-annual proficiency testing (PT) program implemented by the Clinical Pharmacology Quality Assurance (CPQA) program. Using results from multiple PT rounds, longitudinal analyses of recovery are reflective of accuracy and precision within/across laboratories. The objectives of this longitudinal analysis of PT across multiple CPLs were to develop and test statistical models that longitudinally: (1)assess the precision and accuracy of concentrations reported by individual CPLs; (2)determine factors associated with round-specific and long-term assay accuracy, precision and bias using a new regression model. A measure of absolute recovery is explored as a simultaneous measure of accuracy and precision. Overall, the analysis outcomes assured 97% accuracy (±20% of the final target concentration of all (21)drug concentration results reported for clinical trial samples by multiple CPLs).Using the CLIA acceptance of meeting criteria for ≥2/3 consecutive rounds, all ten laboratories that participated in three or more rounds per analyte maintained CLIA proficiency. Significant associations were present between magnitude of error and CPL (Kruskal Wallis [KW]p<0.001), and ARV (KW p<0.001). PMID:24052065
McCleskey, R. Blaine; Nordstrom, D. Kirk; Steiger, Judy I.; Kimball, Briant A.; Verplanck, Philip L.
2003-01-01
Water analyses are reported for 259 samples collected from the Red River, New Mexico, and its tributaries during low-flow(2001) and spring snowmelt (2002) tracer studies. Water samples were collected along a 20-kilometer reach of the Red River beginning just east of the town of Red River and ending at the U.S. Geological Survey streamflow-gaging station located east of Questa, New Mexico. The study area was divided into three sections where separate injections and synoptic sampling events were performed during the low-flow tracer study. During the spring snowmelt tracer study, three tracer injections and synoptic sampling events were performed bracketing the areas with the greatest metal loading into the Red River as determined from the low-flow tracer study. The lowflow tracer synoptic sampling events were August 17, 20, and 24, 2001. The synoptic sampling events for the spring snowmelt tracer were March 30, 31, and April 1, 2002. Stream and large inflow water samples were sampled using equal-width and depth-integrated sampling methods and composited into half-gallon bottles. Grab water samples were collected from smaller inflows. Stream temperatures were measured at the time of sample collection. Samples were transported to a nearby central processing location where pH and specific conductance were measured and the samples processed for chemical analyses. Cations, trace metals, iron redox species, and fluoride were analyzed at the U.S. Geological Survey laboratory in Boulder, Colorado. Cations and trace metal concentrations were determined using inductively coupled plasma-optical emission spectrometry and graphite furnace atomic absorption spectrometry. Arsenic concentrations were determined using hydride generation atomic absorption spectrometry, iron redox species were measured using ultraviolet-visible spectrometry, and fluoride concentrations were determined using an ion-selective electrode. Alkalinity was measured by automated titration, and sulfate, chloride, and bromide were analyzed by ion chromatography at the U.S. Geological Survey laboratory in Salt Lake City, Utah.
Leaching of organic contaminants from storage of reclaimed asphalt pavement.
Norin, Malin; Strömvall, A M
2004-03-01
Recycling of asphalt has been promoted by rapid increases in both the use and price of petroleum-based bitumen. Semi-volatile organic compounds in leachates from reclaimed asphalt pavement, measured in field samples and in laboratory column test, were analysed through a GC/MS screen-test methodology. Sixteen PAH (polyaromatic hydrocarbons) were also analysed in leachates from the column study. The highest concentrations of semi-volatile compounds, approximately 400 microg l(-1), were measured in field samples from the scarified stockpile. Naphthalene, butylated hydroxytoluene (BHT) and dibutyl phthalate (DBP) were the most dominant of the identified semi-volatiles. The occurrence of these compounds in urban groundwater, also indicate high emission rates and persistent structures of the compounds, making them potentially hazardous. Car exhausts, rubber tires and the asphalt material itself are all probable emission sources, determined from the organic contaminants released from the stockpiles. The major leaching mechanism indicated was dissolution of organic contaminants from the surface of the asphalt gravels. In the laboratory column test, the release of high-molecular weight and more toxic PAH was higher in the leachates after two years than at the commencement of storage. The concentrations of semi-volatiles in leachates, were also several times lower than those from the field stockpile. These results demonstrate the need to follow up laboratory column test with real field measurements.
Law enforcement tools available at the Savannah River Site
DOE Office of Scientific and Technical Information (OSTI.GOV)
Hofstetter, K.J.
A number of nuclear technologies developed and applied at the Savannah River Site in support of nuclear weapons material production and environmental remediation can be applied to problems in law enforcement. Techniques and equipment for high-sensitivity analyses of samples are available to identify and quantify trace elements and establish origins and histories of forensic evidence removed from crime scenes. While some of theses capabilities are available at local crime laboratories, state-of-the-art equipment and breakthroughs in analytical techniques are continually being developed at DOE laboratories. Extensive experience with the handling of radioactive samples at the DOE labs minimizes the chances ofmore » cross-contamination of evidence received from law enforcement. In addition to high-sensitivity analyses, many of the field techniques developed for use in a nuclear facility can assist law enforcement personnel in detecting illicit materials and operations, in retrieving of pertinent evidence and in surveying crime scenes. Some of these tools include chemical sniffers, hand-held detectors, thermal imaging, etc. In addition, mobile laboratories can be deployed to a crime scene to provide field screening of potential evidence. A variety of portable sensors can be deployed on vehicle, aerial, surface or submersible platforms to assist in the location of pertinent evidence or illicit operations. Several specific nuclear technologies available to law enforcement and their potential uses are discussed.« less
Gałuszka, Agnieszka; Migaszewski, Zdzisław M; Namieśnik, Jacek
2015-07-01
The recent rapid progress in technology of field portable instruments has increased their applications in environmental sample analysis. These instruments offer a possibility of cost-effective, non-destructive, real-time, direct, on-site measurements of a wide range of both inorganic and organic analytes in gaseous, liquid and solid samples. Some of them do not require the use of reagents and do not produce any analytical waste. All these features contribute to the greenness of field portable techniques. Several stationary analytical instruments have their portable versions. The most popular ones include: gas chromatographs with different detectors (mass spectrometer (MS), flame ionization detector, photoionization detector), ultraviolet-visible and near-infrared spectrophotometers, X-ray fluorescence spectrometers, ion mobility spectrometers, electronic noses and electronic tongues. The use of portable instruments in environmental sample analysis gives a possibility of on-site screening and a subsequent selection of samples for routine laboratory analyses. They are also very useful in situations that require an emergency response and for process monitoring applications. However, quantification of results is still problematic in many cases. The other disadvantages include: higher detection limits and lower sensitivity than these obtained in laboratory conditions, a strong influence of environmental factors on the instrument performance and a high possibility of sample contamination in the field. This paper reviews recent applications of field portable instruments in environmental sample analysis and discusses their analytical capabilities. Copyright © 2015 Elsevier Inc. All rights reserved.
Aarsand, Aasne K; Villanger, Jørild H; Støle, Egil; Deybach, Jean-Charles; Marsden, Joanne; To-Figueras, Jordi; Badminton, Mike; Elder, George H; Sandberg, Sverre
2011-11-01
The porphyrias are a group of rare metabolic disorders whose diagnosis depends on identification of specific patterns of porphyrin precursor and porphyrin accumulation in urine, blood, and feces. Diagnostic tests for porphyria are performed by specialized laboratories in many countries. Data regarding the analytical and diagnostic performance of these laboratories are scarce. We distributed 5 sets of multispecimen samples from different porphyria patients accompanied by clinical case histories to 18-21 European specialist porphyria laboratories/centers as part of a European Porphyria Network organized external analytical and postanalytical quality assessment (EQA) program. The laboratories stated which analyses they would normally have performed given the case histories and reported results of all porphyria-related analyses available, interpretative comments, and diagnoses. Reported diagnostic strategies initially showed considerable diversity, but the number of laboratories applying adequate diagnostic strategies increased during the study period. We found an average interlaboratory CV of 50% (range 12%-152%) for analytes in absolute concentrations. Result normalization by forming ratios to the upper reference limits did not reduce this variation. Sixty-five percent of reported results were within biological variation-based analytical quality specifications. Clinical interpretation of the obtained analytical results was accurate, and most laboratories established the correct diagnosis in all distributions. Based on a case-based EQA scheme, variations were apparent in analytical and diagnostic performance between European specialist porphyria laboratories. Our findings reinforce the use of EQA schemes as an essential tool to assess both analytical and diagnostic processes and thereby to improve patient care in rare diseases.
Virdis, Salvatore; Scarano, Christian; Spanu, Vincenzo; Murittu, Gavino; Spanu, Carlo; Ibba, Ignazio; De Santis, Enrico Pietro Luigi
2014-12-09
In the present work the results of a survey conducted in Sardinia Region on Aflatoxin M 1 (AFM 1 ) contamination in milk of small ruminants from 2005 to 2013 are reported. A total of 517 sheep and 88 goat milk samples from bulk tank, tank trucks and silo tank milk were collected. Analyses were performed by the Regional Farmers Association laboratory using high-performance liquid chromatography following the ISO 14501:1998 standard. None of the sheep milk samples analysed during 2005-2012 showed AFM 1 contamination. In sheep milk samples collected in 2013, 8 out of 172 (4.6%) were contaminated by AFM 1 with a concentration (mean±SD) of 12.59±14.05 ng/L. In one bulk tank milk sample 58.82 ng/L AFM 1 was detected, exceeding the EU limit. In none of goat milk samples analysed from 2010 to 2012 AFM 1 was detected. In 2013, 9 out of 66 goat milk samples (13.6%) showed an AFM 1 concentration of 47.21±19.58 ng/L. Two of these samples exceeded the EU limit, with concentrations of 62.09 and 138.6 ng/L. Higher contamination frequency and concentration rates were detected in bulk tank milk samples collected at farm than in bulk milk truck or silo samples, showing a dilution effect on AFM 1 milk content along small ruminants supply chain. The rate and levels of AFM 1 contamination in sheep and goat milk samples were lower than other countries. However, the small number of milk samples analysed for AFM 1 in Sardinia Region in 2005-2013 give evidence that food business operators check programmes should be improved to ensure an adequate monitoring of AFM 1 contamination in small ruminant dairy chain.
Yin, Xuejun; Neal, Bruce; Tian, Maoyi; Li, Zhifang; Petersen, Kristina; Komatsu, Yuichiro; Feng, Xiangxian; Wu, Yangfeng
2018-04-01
Measurement of mean population Na and K intakes typically uses laboratory-based assays, which can add significant logistical burden and costs. A valid field-based measurement method would be a significant advance. In the current study, we used 24 h urine samples to compare estimates of Na, K and Na:K ratio based upon assays done using the field-based Horiba twin meter v. laboratory-based methods. The performance of the Horiba twin meter was determined by comparing field-based estimates of mean Na and K against those obtained using laboratory-based methods. The reported 95 % limits of agreement of Bland-Altman plots were calculated based on a regression approach for non-uniform differences. The 24 h urine samples were collected as part of an ongoing study being done in rural China. One hundred and sixty-six complete 24 h urine samples were qualified for estimating 24 h urinary Na and K excretion. Mean Na and K excretion were estimated as 170·4 and 37·4 mmol/d, respectively, using the meter-based assays; and 193·4 and 43·8 mmol/d, respectively, using the laboratory-based assays. There was excellent relative reliability (intraclass correlation coefficient) for both Na (0·986) and K (0·986). Bland-Altman plots showed moderate-to-good agreement between the two methods. Na and K intake estimations were moderately underestimated using assays based upon the Horiba twin meter. Compared with standard laboratory-based methods, the portable device was more practical and convenient.
Utzinger, J; Botero-Kleiven, S; Castelli, F; Chiodini, P L; Edwards, H; Köhler, N; Gulletta, M; Lebbad, M; Manser, M; Matthys, B; N'Goran, E K; Tannich, E; Vounatsou, P; Marti, H
2010-03-01
The present study aimed to compare the diagnostic performance of different European reference laboratories in diagnosing helminths and intestinal protozoa, using an ether-concentration method applied to sodium acetate-acetic acid-formalin (SAF)-preserved faecal samples. In total, 102 stool specimens were analysed during a cross-sectional parasitological survey in urban farming communities in Côte d'Ivoire. Five SAF-preserved faecal samples were prepared from each specimen and forwarded to the participating reference laboratories, processed and examined under a microscope adhering to a standard operating procedure (SOP). Schistosoma mansoni (cumulative prevalence: 51.0%) and hookworm (cumulative prevalence: 39.2%) were the predominant helminths. There was excellent agreement (kappa > 0.8; p < 0.001) among the reference laboratories for the diagnosis of S. mansoni, hookworm, Trichuris trichiura and Ascaris lumbricoides. Moderate agreement (kappa = 0.54) was found for Hymenolepis nana, and lesser agreement was observed for other, less prevalent helminths. The predominant intestinal protozoa were Entamoeba coli (median prevalence: 67.6%), Blastocystis hominis (median prevalence: 55.9%) and Entamoeba histolytica/Entamoeba dispar (median prevalence: 47.1%). Substantial agreement among reference laboratories was found for E. coli (kappa = 0.69), but only fair or moderate agreement was found for other Entamoeba species, Giardia intestinalis and Chilomastix mesnili. There was only poor agreement for B. hominis, Isospora belli and Trichomonas intestinalis. In conclusion, although common helminths were reliably diagnosed by European reference laboratories, there was only moderate agreement between centres for pathogenic intestinal protozoa. Continued external quality assessment and the establishment of a formal network of reference laboratories is necessary to further enhance both accuracy and uniformity in parasite diagnosis.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Evans, J.C.; Thomas, B.L.; Pool, K.H.
1996-07-01
This report describes the results of vapor samples obtained to compare vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling System (ISVS) with and without particulate prefiltration. Samples were collected from the headspace of waste storage tank 241-S-102 (Tank S-102) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) was contracted by Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for water, ammonia, permanent gases, total nonmethane hydrocarbons (TNMHCs, also known as TO-12), and organic analytes in samples collected in SUMMA{trademark} canisters and on triple sorbentmore » traps (TSTs) from the tank headspace. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sampling and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was {open_quotes}Sampling and Analysis Plan for Tank Vapor Sampling Comparison Test{close_quote}, and the sample jobs were designated S6007, S6008, and S6009. Samples were collected by WHC on January 26, 1996, using the VSS, a truck-based sampling method using a heated probe; and the ISVS with and without particulate prefiltration.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Pool, K.H.; Evans, J.C.; Thomas, B.L.
1996-07-01
This report describes the results of vapor samples obtained to compare vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling System (ISVS) with and without particulate prefiltration. Samples were collected from the headspace of waste storage tank 241-BY-108 (Tank BY-108) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) was contracted by Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for water, ammonia, permanent gases, total nonmethane hydrocarbons (TNMHCs, also known as TO-12), and organic analytes in samples collected in SUMMA{trademark} canisters and on triple sorbentmore » traps (TSTs) from the tank headspace. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sampling and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was {open_quotes}Sampling and Analysis Plan for Tank Vapor Sampling Comparison Test{close_quotes}, and the sample jobs were designated S6004, S6005, and S6006. Samples were collected by WHC on January 23, 1996, using the VSS, a truck-based sampling method using a heated probe; and the ISVS with and without particulate prefiltration.« less
Capillary microextraction: A new method for sampling methamphetamine vapour.
Nair, M V; Miskelly, G M
2016-11-01
Clandestine laboratories pose a serious health risk to first responders, investigators, decontamination companies, and the public who may be inadvertently exposed to methamphetamine and other chemicals used in its manufacture. Therefore there is an urgent need for reliable methods to detect and measure methamphetamine at such sites. The most common method for determining methamphetamine contamination at former clandestine laboratory sites is selected surface wipe sampling, followed by analysis with gas chromatography-mass spectrometry (GC-MS). We are investigating the use of sampling for methamphetamine vapour to complement such wipe sampling. In this study, we report the use of capillary microextraction (CME) devices for sampling airborne methamphetamine, and compare their sampling efficiency with a previously reported dynamic SPME method. The CME devices consisted of PDMS-coated glass filter strips inside a glass tube. The devices were used to dynamically sample methamphetamine vapour in the range of 0.42-4.2μgm -3 , generated by a custom-built vapour dosing system, for 1-15min, and methamphetamine was analysed using a GC-MS fitted with a ChromatoProbe thermal desorption unit. The devices showed good reproducibility (RSD<15%), and a curvilinear pre-equilibrium relationship between sampling times and peak area, which can be utilised for calibration. Under identical sampling conditions, the CME devices were approximately 30 times more sensitive than the dynamic SPME method. The CME devices could be stored for up to 3days after sampling prior to analysis. Consecutive sampling of methamphetamine and its isotopic substitute, d-9 methamphetamine showed no competitive displacement. This suggests that CME devices, pre-loaded with an internal standard, could be a feasible method for sampling airborne methamphetamine at former clandestine laboratories. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.
Noble gas isotopes in mineral springs within the Cascadia Forearc, Wasihington and Oregon
McCrory, Patricia A.; Constantz, James E.; Hunt, Andrew G.
2014-01-01
This U.S. Geological Survey report presents laboratory analyses along with field notes for a pilot study to document the relative abundance of noble gases in mineral springs within the Cascadia forearc of Washington and Oregon. Estimates of the depth to the underlying Juan de Fuca oceanic plate beneath the sample sites are derived from the McCrory and others (2012) slab model. Some of these springs have been previously sampled for chemical analyses (Mariner and others, 2006), but none currently have publicly available noble gas data. Helium isotope values as well as the noble gas values and ratios presented below will be used to determine the sources and mixing history of these mineral waters.
Moore, C.R.
1989-01-01
This report presents physical, chemical, and biological data collected at 50 sampling sites on selected streams in Chester County, Pennsylvania from 1969 to 1980. The physical data consist of air and water temperature, stream discharge, suspended sediment, pH, specific conductance, and dissolved oxygen. The chemical data consist of laboratory determinations of total nutrients, major ions, and trace metals. The biological data consist of total coliform, fecal coliform, and fecal streptococcus bacteriological analyses, and benthicmacroinvertebrate population analyses. Brillouin's diversity index, maximum diversity, minimum diversity, and evenness for each sample, and median and mean Brilloiuin's diversity index, standard deviation, and standard error of the mean were calculated for the benthic-macroinvertebrate data for each site.
USDA-ARS?s Scientific Manuscript database
Recent metagenomic analyses of the turkey gut ribonucleic acid (RNA) virus community in our laboratory have identified novel enteric RNA viruses that may play roles in the poultry enteric diseases and in performance problems noted in the field. This has lead to new molecular diagnostic assays for ce...
Behind the scene with the fathead team: Part III. Molecular, biochemical, and in vitro analyses
As part of a research team focused on aquatic toxicity testing using fathead minnows as a model species, this presentation is the third in the three-part series, giving an overview of the types of field and laboratory studies as well as sample processing our team conducts at the ...
ERIC Educational Resources Information Center
Lightburn, Millard E.; Fraser, Barry J.
2007-01-01
The main purpose of this research was to evaluate the use of anthropometric activities among a sample of 761 high-school biology students in terms of student outcomes (achievement and attitudes) and classroom environment (assessed with the Science Laboratory Environment Inventory, SLEI). Data analyses supported the SLEI's factorial validity,…
Construction Materials Used in the Historical Roman Era Bath in Myra
Oguz, Cem; Turker, Fikret
2014-01-01
The physical, chemical, and mechanical properties of mortars and bricks used in the historical building that was erected at Myra within the boundaries of Antalya Province during the Roman time were investigated. The sample picked points were marked on the air photographs and plans of the buildings and samples were photographed. Then petrographic evaluation was made by stereo microscope on the polished surfaces of construction materials (mortar, brick) taken from such historical buildings in laboratory condition. Also, microstructural analyses (SEM/EDX, XRD), physical analyses (unit volume, water absorption by mass, water absorption by volume, specific mass, compacity, and porosity), chemical analyses (acid loss and sieve analysis, salt analyses, pH, protein, fat, pozzolanic activity, and conductivity analyses), and mechanical experiments (compressive strength, point loading test, and tensile strength at bending) were applied and the obtained results were evaluated. It was observed that good adherence was provided between the binder and the aggregate in mortars. It was also detected that bricks have preserved their originality against environmental, atmospheric, and physicochemical effects and their mechanical properties showed that they were produced by appropriate techniques. PMID:25089290
Construction materials used in the historical Roman era bath in Myra.
Oguz, Cem; Turker, Fikret; Kockal, Niyazi Ugur
2014-01-01
The physical, chemical, and mechanical properties of mortars and bricks used in the historical building that was erected at Myra within the boundaries of Antalya Province during the Roman time were investigated. The sample picked points were marked on the air photographs and plans of the buildings and samples were photographed. Then petrographic evaluation was made by stereo microscope on the polished surfaces of construction materials (mortar, brick) taken from such historical buildings in laboratory condition. Also, microstructural analyses (SEM/EDX, XRD), physical analyses (unit volume, water absorption by mass, water absorption by volume, specific mass, compacity, and porosity), chemical analyses (acid loss and sieve analysis, salt analyses, pH, protein, fat, pozzolanic activity, and conductivity analyses), and mechanical experiments (compressive strength, point loading test, and tensile strength at bending) were applied and the obtained results were evaluated. It was observed that good adherence was provided between the binder and the aggregate in mortars. It was also detected that bricks have preserved their originality against environmental, atmospheric, and physicochemical effects and their mechanical properties showed that they were produced by appropriate techniques.
Field Exploration and Life Detection Sampling Through Planetary Analogue Sampling (FELDSPAR).
NASA Technical Reports Server (NTRS)
Stockton, A.; Amador, E. S.; Cable, M. L.; Cantrell, T.; Chaudry, N.; Cullen, T.; Duca, Z.; Gentry, D. M.; Kirby, J.; Jacobsen, M.;
2017-01-01
Exploration missions to Mars rely on rovers to perform analyses over small sampling areas; however, landing sites for these missions are selected based on large-scale, low-resolution remote data. The use of Earth analogue environments to estimate the multi-scale spatial distributions of key signatures of habitability can help ensure mission science goals are met. A main goal of FELDSPAR is to conduct field operations analogous to Mars sample return in its science, operations, and technology from landing site selection, to in-field sampling location selection, remote or stand-off analysis, in situ analysis, and home laboratory analysis. Lava fields and volcanic regions are relevant analogues to Martian landscapes due to desiccation, low nutrient availability, and temperature extremes. Operationally, many Icelandic lava fields are remote enough to require that field expeditions address several sampling constraints that are experienced in robotic exploration, including in situ and sample return missions. The Fimmvruhls lava field was formed by a basaltic effusive eruption associated with the 2010 Eyjafjallajkull eruption. Mlifellssandur is a recently deglaciated plain to the north of the Myrdalsjkull glacier. Holuhraun was formed by a 2014 fissure eruptions just north of the large Vatnajkull glacier. Dyngjusandur is an alluvial plain apparently kept barren by repeated mechanical weathering. Informed by our 2013 expedition, we collected samples in nested triangular grids every decade from the 10 cm scale to the 1 km scale (as permitted by the size of the site). Satellite imagery is available for older sites, and for Mlifellssandur, Holuhraun, and Dyngjusandur we obtained overhead imagery at 1 m to 200 m elevation. PanCam-style photographs were taken in the field by sampling personnel. In-field reflectance spectroscopy was also obtained with an ASD spectrometer in Dyngjusandur. All sites chosen were 'homogeneous' in apparent color, morphology, moisture, grain size, and reflectance spectra at all scales greater than 10 cm. Field lab assays were conducted to monitor microbial habitation, including ATP quantification, qPCR for fungal, bacterial, and archaeal DNA, and direct cell imaging using fluorescence microscopy. Home laboratory analyses include Raman spectroscopy and community sequencing. ATP appeared to be significantly more sensitive to small changes in sampling location than qPCR or fluorescence microscopy. Bacterial and archaeal DNA content were more consistent at the smaller scales, but similarly variable across more distant sites. Conversely, cell counts and fungal DNA content have significant local variation but appear relatively homogeneous over scales of 1 km. ATP, bacterial DNA, and archaeal DNA content were relatively well correlated at many spatial scales. While we have observed spatial variation at various scales and are beginning to observe how that variation fluctuates over time as biodiversity recovers after an eruption, we do not yet fully understand what parameters lead to the observed spatial variation. Home laboratory analyses will help us further understand the elemental and structural composition of the basaltic matrices, but further field analyses are vital for the understanding how temperature, moisture, incident radiation, and so forth influence the habitability of a microclimate.
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)
Carlsbad Field Office
The Performance Demonstration Program (PDP) for headspace gases distributes blind audit samples in a gas matrix for analysis of volatile organic compounds (VOCs). Participating measurement facilities (i.e., fixed laboratories, mobile analysis systems, and on-line analytical systems) are located across the United States. Each sample distribution is termed a PDP cycle. These evaluation cycles provide an objective measure of the reliability of measurements performed for transuranic (TRU) waste characterization. The primary documents governing the conduct of the PDP are the Quality Assurance Program Document (QAPD) (DOE/CBFO-94-1012) and the Waste Isolation Pilot Plant (WIPP) Waste Analysis Plan (WAP) contained in the Hazardousmore » Waste Facility Permit (NM4890139088-TSDF) issued by the New Mexico Environment Department (NMED). The WAP requires participation in the PDP; the PDP must comply with the QAPD and the WAP. This plan implements the general requirements of the QAPD and the applicable requirements of the WAP for the Headspace Gas (HSG) PDP. Participating measurement facilities analyze blind audit samples of simulated TRU waste package headspace gases according to the criteria set by this PDP Plan. Blind audit samples (hereafter referred to as PDP samples) are used as an independent means to assess each measurement facility’s compliance with the WAP quality assurance objectives (QAOs). To the extent possible, the concentrations of VOC analytes in the PDP samples encompass the range of concentrations anticipated in actual TRU waste package headspace gas samples. Analyses of headspace gases are required by the WIPP to demonstrate compliance with regulatory requirements. These analyses must be performed by measurement facilities that have demonstrated acceptable performance in this PDP. These analyses are referred to as WIPP analyses and the TRU waste package headspace gas samples on which they are performed are referred to as WIPP samples in this document. Participating measurement facilities must analyze PDP samples using the same procedures used for routine waste characterization analyses of WIPP samples.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Carlsbad Field Office
The Performance Demonstration Program (PDP) for headspace gases distributes sample gases of volatile organic compounds (VOCs) for analysis. Participating measurement facilities (i.e., fixed laboratories, mobile analysis systems, and on-line analytical systems) are located across the United States. Each sample distribution is termed a PDP cycle. These evaluation cycles provide an objective measure of the reliability of measurements performed for transuranic (TRU) waste characterization. The primary documents governing the conduct of the PDP are the Quality Assurance Program Document (QAPD) (DOE/CBFO-94-1012) and the Waste Isolation Pilot Plant (WIPP) Waste Analysis Plan (WAP) contained in the Hazardous Waste Facility Permit (NM4890139088-TSDF) issuedmore » by the New Mexico Environment Department (NMED). The WAP requires participation in the PDP; the PDP must comply with the QAPD and the WAP. This plan implements the general requirements of the QAPD and the applicable requirements of the WAP for the Headspace Gas (HSG) PDP. Participating measurement facilities analyze blind audit samples of simulated TRU waste package headspace gases according to the criteria set by this PDP Plan. Blind audit samples (hereafter referred to as PDP samples) are used as an independent means to assess each measurement facility’s compliance with the WAP quality assurance objectives (QAOs). To the extent possible, the concentrations of VOC analytes in the PDP samples encompass the range of concentrations anticipated in actual TRU waste package headspace gas samples. Analyses of headspace gases are required by the WIPP to demonstrate compliance with regulatory requirements. These analyses must be performed by measurement facilities that have demonstrated acceptable performance in this PDP. These analyses are referred to as WIPP analyses and the TRU waste package headspace gas samples on which they are performed are referred to as WIPP samples in this document. Participating measurement facilities must analyze PDP samples using the same procedures used for routine waste characterization analyses of WIPP samples.« less
Information systems as a quality management tool in clinical laboratories
NASA Astrophysics Data System (ADS)
Schmitz, Vanessa; Rosecler Bez el Boukhari, Marta
2007-11-01
This article describes information systems as a quality management tool in clinical laboratories. The quality of laboratory analyses is of fundamental importance for health professionals in aiding appropriate diagnosis and treatment. Information systems allow the automation of internal quality management processes, using standard sample tests, Levey-Jennings charts and Westgard multirule analysis. This simplifies evaluation and interpretation of quality tests and reduces the possibility of human error. This study proposes the development of an information system with appropriate functions and costs for the automation of internal quality control in small and medium-sized clinical laboratories. To this end, it evaluates the functions and usability of two commercial software products designed for this purpose, identifying the positive features of each, so that these can be taken into account during the development of the proposed system.
NASA Astrophysics Data System (ADS)
Reyer, D.; Philipp, S. L.
2012-04-01
Heterogeneous rock properties in terms of layering and complex infrastructure of fault zones are typical phenomena in sedimentary basins such as the North German Basin. To be able to model reservoir stimulation in layered stratifications and to better adapt the drilling strategy to the rock mechanical conditions it is important to have knowledge about the effects of heterogeneous rock properties on fracture propagation and fault zone infrastructure for typical sedimentary reservoir rocks in the North German Basin. Therefore we aim at quantifying these properties by performing structural geological field studies in outcrop analogues combined with laboratory analyses. The field studies in Rotliegend sandstones (Lower Permian), the sandstones of the Middle Bunter (Lower Triassic) and the sandstones of the Upper Keuper (Upper Triassic) focus on 1) host rock fracture systems and 2) fault zone infrastructure. We analyse quantitatively the dimension, geometry, persistence and connectivity of fracture systems separately for host rocks and fault damage zones. The results show that in rocks with distinctive layering (sandstones and shales) natural fractures are often restricted to individual layers, that is, they are stratabound. The probability of fracture arrest seems to depend on the stiffness contrast between the two layers and on the thickness of the softer layer. The field studies are complemented by systematic sampling to obtain mechanical property variations caused by the layering. For the samples we measure the parameters Young's modulus, compressive and tensile strengths, elastic strain energy, density and porosity. The results show that the mechanical properties vary considerably and many samples are clearly anisotropic. That is, samples taken perpendicular to layering commonly have higher strengths but lower stiffnesses than those taken parallel to layering. We combine the results of laboratory analyses and field measurements to specify the mechanical heterogeneities of the sedimentary reservoir rocks of the North German Basin and of the mechanical units of fault zones therein. To estimate the in situ rock properties at different depths it is further important to understand how rocks from outcrops differ from rocks at depth (for example due to alteration and removal of the overburden load). To answer these questions we analyse samples from drill cores from depths relevant for the use as geothermal reservoirs which are stratigraphically and lithologically equivalent to those taken in outcrop analogues. The results from drill-core sample analyses are then compared with the results from the outcrop samples. Another approach is to analyse how rock mechanical properties correlate with petrographic properties (e.g., mineral content, cementation, fabric, porosity) to use this knowledge to extrapolate the data to depth. Altogether these results will be very useful to make better assumptions on natural reservoir permeabilities and to better adapt the drilling and reservoir stimulation strategy to the rock mechanical conditions.
Mineralogy and Petrology of COMET WILD2 Nucleus Samples
NASA Technical Reports Server (NTRS)
Zolensky, Michael; Bland, Phil; Bradley, John; Brearley, Adrian; Brennan, Sean; Bridges, John; Brownlee, Donald; Butterworth, Anna; Dai, Zurong; Ebel, Denton
2006-01-01
The sample return capsule of the Stardust spacecraft will be recovered in northern Utah on January 15, 2006, and under nominal conditions it will be delivered to the new Stardust Curation Laboratory at the Johnson Space Center two days later. Within the first week we plan to begin the harvesting of aerogel cells, and the comet nucleus samples they contain for detailed analysis. By the time of the LPSC meeting we will have been analyzing selected removed grains for more than one month. This presentation will present the first results from the mineralogical and petrological analyses that will have been performed.
Survey on nutrient content of different organic fertilisers.
Rajan, Jagadish; Anandhan, Shanmugaselvan Veilumuthu
2015-06-01
The knowledge of nutrient aspects of organic fertilisers is of much relevance in assessing their availability and long-term effect to the soil and crop and in formulating sound fertiliser recommendation. Around 619 organic fertiliser samples under different categories, which were received by the analytical laboratory of UPASI Tea Research Institute, Valparai, were examined for their nutrient status. The trend in the number of samples received every year for the past 5 years showed that there is a gradual, steady and linear increase in the number of samples received by the laboratory which, in turn, authenticates the increase in the production and utilisation of organic fertilisers in agricultural sector. This also reveals the awareness of organic farming among farmers in recent times. The organic fertilisers received by the laboratory were categorised into different groups based on their nomenclature. The number of samples received each year under different categories varies to a larger extent. The nutritional status was unpredictable based on the nomenclature of the sample received. In addition to this frequency distribution, the nutritional values analysed are discussed in this paper. Correlation matrix was worked out between all the parameters estimated. It is evident that if maintenance of proper carbon-to-nitrogen ratio and moisture content is ascertained in the finished product, one can guarantee the quality of the organic fertiliser in terms of nutrient content.
García-González, Elena; Aramendía, Maite; Álvarez-Ballano, Diego; Trincado, Pablo; Rello, Luis
2016-04-01
Endogenous antibodies (EA) may interfere with immunoassays, causing erroneous results for hormone analyses. As (in most cases) this interference arises from the assay format and most immunoassays, even from different manufacturers, are constructed in a similar way, it is possible for a single type of EA to interfere with different immunoassays. Here we describe the case of a patient whose serum sample contains EA that interfere several hormones tests. We also discuss the strategies deployed to detect interference. Over a period of four years, a 30-year-old man was subjected to a plethora of laboratory and imaging diagnostic procedures as a consequence of elevated hormone results, mainly of pituitary origin, which did not correlate with the overall clinical picture. Once analytical interference was suspected, the best laboratory approaches to investigate it were sample reanalysis on an alternative platform and sample incubation with antibody blocking tubes. Construction of an in-house 'nonsense' sandwich assay was also a valuable strategy to confirm interference. In contrast, serial sample dilutions were of no value in our case, while polyethylene glycol (PEG) precipitation gave inconclusive results, probably due to the use of inappropriate PEG concentrations for several of the tests assayed. Clinicians and laboratorians must be aware of the drawbacks of immunometric assays, and alert to the possibility of EA interference when results do not fit the clinical pattern.
Cureau, Felipe Vogt; Bloch, Katia Vergetti; Henz, Aline; Schaan, Camila W; Klein, Carlos Henrique; Oliveira, Cecília Lacroix de; Giannini, Denise Tavares; Leon, Elisa Brosina de; Abreu, Gabriela de Azevedo; Telo, Gabriela Heiden; Dias, Glauber Monteiro; Carvalho, Kênia Mara Baiocchi de; Barufaldi, Laura Augusta; Kuschnir, Maria Cristina Caetano; Szklo, Moyses; Montenegro, Renan; Silva, Thiago Luiz Nogueira da; Ekelund, Ulf; Schaan, Beatriz D
2017-05-18
The Study of Cardiovascular Risk in Adolescents (ERICA) is a pioneering study that aimed to assess the prevalence of cardiovascular risk factors, including metabolic syndrome components in Brazilian adolescents. This study aims to describe the methodological aspects related to blood collection as well as to report pertaining results of the preparation, transport, storage, and exams in ERICA. Exams in ERICA were performed in a single laboratory and blood samples were collected in schools in a standardized manner. Logistics involved air transportation of samples to the reference laboratory with controlled temperature since sample collection. The serum was stored in local biorepositories in four centers to be used in future analyses. During the study, 284,247 exams were performed and rate of participation in exams was 56.2%, thus involving 40,732 adolescents. From the total, 92.6% of the samples reached the reference laboratory maintaining the temperature between 0-10°C. No clinical significant changes in results due to temperature changes were identified. External quality control recorded satisfactory results in 98.7% of the evaluations. Four biorepositories with samples of 7,785 adolescents were created. Thus, we can consider that the logistics adopted in ERICA was fairly successful and description of this as well as the difficulties experienced in Brazil can inform and facilitate the planning of future studies, especially in developing countries.
Taylor, Howard E.; Spence, John R.; Antweiler, Ronald C.; Berghoff, Kevin; Plowman, Terry I.; Peart, Dale B.; Roth, David A.
2004-01-01
The U.S. Geological Survey, in cooperation with the National Park Service conducted an intensive assessment of selected springs along the Colorado River Corridor in Arches National Park, Canyonlands National Park, Glen Canyon National Recreation Area, and Grand Canyon National Park in 1997 and 1998, for the purpose of measuring and evaluating the water quality and quantity of the resource. This study was conducted to establish baseline data for the future evaluation of possible effects from recreational use and climate change. Selected springs and seeps were visited over a study period from 1997 to 1998, during which, discharge and on-site chemical measurements were made at selected springs and seeps, and samples were collected for subsequent chemical laboratory analysis. This interdisciplinary study also includes simultaneous studies of flora and fauna, measured and sampled coincidently at the same sites. Samples collected during this study were transported to U.S. Geological Survey laboratories in Boulder, Colorado, where analyses were performed using state-of-the-art laboratory technology. The location of the selected springs and seeps, elevation, geology, aspect, and onsite measurements including temperature, discharge, dissolved oxygen, pH, and specific conductance, were recorded. Laboratory analyses include determinations for alkalinity, aluminum, ammonium (nitrogen), antimony, arsenic, barium, beryllium, bismuth, boron, bromide, cadmium, calcium, cerium, cesium, chloride, chromium, cobalt, copper, dissolved inorganic carbon, dissolved organic carbon, dysprosium, erbium, europium, fluoride, gadolinium, holmium, iodine, iron, lanthanum, lead, lithium, lutetium, magnesium, manganese, mercury, molybdenum, neodymium, nickel, nitrate (nitrogen), nitrite (nitrogen), phosphate, phosphorus, potassium, praseodymium, rhenium, rubidium, samarium, selenium, silica, silver, sodium, strontium, sulfate, tellurium, terbium, thallium, thorium, thulium, tin, titanium, tungsten, uranium, vanadium, yttrium, ytterbium, zinc, and zirconium in these springs and seeps. Biological observations include physical setting, vegetation, invertebrate habitats, and invertebrate microhabitats.
Survey of bottled drinking water sold in Canada. Part 2. Selected volatile organic compounds
DOE Office of Scientific and Technical Information (OSTI.GOV)
Page, B.D.; Conacher, H.B.S.; Salminen, J.
Selected volatile organic compound (VOC) contaminants were determined in 182 samples of retail bottled waters purchased in Canada. Samples included spring water (86) packaged in containers of polyethylene or in smaller containers of transparent plastic or glass, mineral water (61) packaged only in transparent plastic or glass, and miscellaneous bottled waters (35). Analyses were performed by 3 laboratories, each using headspace sampling and capillary gas chromatography with either mass spectrometric (1 laboratory) or flame ionization detection with mass spectrometric confirmation, if required (2 laboratories). Benzene, the contaminant of primary interest, was detected in only 1 of the 182 samples atmore » 2 {mu}g/kg. Other VOC contaminants detected (number of positive samples, average, and range of positives in {mu}g/kg) included toluene (20, 6.92, 0.5-63), cyclohexane (23, 39.2, 3-108), chloroform (12, 25.8, 3.7-70), and dichloromethane (4, 59, 22-97). Cyclohexane was found in the plastic and as a migrant from the plastic in 20 samples of spring water, but it was found in only 1 of 61 mineral water samples analyzed at only 3 {mu}g/kg/. Chloroform was found almost exclusively in samples that could have been obtained from public water supplies. It was not found in mineral water samples, but it was found in 1 spring water sample at 3.7 {mu}g/kg. The source of the toluene contamination was not known. Other VOCs detected include ethanol and limonene, associated with added flavoring; pentane, as a migrant from a foamed polystyrene cap liner; and 1,1,2,2-tetra-chloroethylene in a sample of demineralized water. 10 refs., 6 tabs.« less
Performance Evaluation of the Sysmex CS-5100 Automated Coagulation Analyzer.
Chen, Liming; Chen, Yu
2015-01-01
Coagulation testing is widely applied clinically, and laboratories increasingly demand automated coagulation analyzers with short turn-around times and high-throughput. The purpose of this study was to evaluate the performance of the Sysmex CS-5100 automated coagulation analyzer for routine use in a clinical laboratory. The prothrombin time (PT), international normalized ratio (INR), activated partial thromboplastin time (APTT), fibrinogen (Fbg), and D-dimer were compared between the Sysmex CS-5100 and Sysmex CA-7000 analyzers, and the imprecision, comparison, throughput, STAT function, and performance for abnormal samples were measured in each. The within-run and between-run coefficients of variation (CV) for the PT, APTT, INR, and D-dimer analyses showed excellent results both in the normal and pathologic ranges. The correlation coefficients between the Sysmex CS-5100 and Sysmex CA-7000 were highly correlated. The throughput of the Sysmex CS-5100 was faster than that of the Sysmex CA-7000. There was no interference at all by total bilirubin concentrations and triglyceride concentrations in the Sysmex CS-5100 analyzer. We demonstrated that the Sysmex CS-5100 performs with satisfactory imprecision and is well suited for coagulation analysis in laboratories processing large sample numbers and icteric and lipemic samples.
Arsenic exposure in drinking water: an unrecognized health threat in Peru.
George, Christine Marie; Sima, Laura; Arias, M Helena Jahuira; Mihalic, Jana; Cabrera, Lilia Z; Danz, David; Checkley, William; Gilman, Robert H
2014-08-01
To assess the extent of arsenic contamination of groundwater and surface water in Peru and, to evaluate the accuracy of the Arsenic Econo-Quick(™) (EQ) kit for measuring water arsenic concentrations in the field. Water samples were collected from 151 water sources in 12 districts of Peru, and arsenic concentrations were measured in the laboratory using inductively-coupled plasma mass spectrometry. The EQ field kit was validated by comparing a subset of 139 water samples analysed by laboratory measurements and the EQ kit. In 86% (96/111) of the groundwater samples, arsenic exceeded the 10 µg/l arsenic concentration guideline given by the World Health Organization (WHO) for drinking water. In 56% (62/111) of the samples, it exceeded the Bangladeshi threshold of 50 µg/l; the mean concentration being 54.5 µg/l (range: 0.1-93.1). In the Juliaca and Caracoto districts, in 96% (27/28) of groundwater samples arsenic was above the WHO guideline; and in water samples collected from the section of the Rímac river running through Lima, all had arsenic concentrations exceeding the WHO limit. When validated against laboratory values, the EQ kit correctly identified arsenic contamination relative to the guideline in 95% (106/111) of groundwater and in 68% (19/28) of surface water samples. In several districts of Peru, drinking water shows widespread arsenic contamination, exceeding the WHO arsenic guideline. This poses a public health threat requiring further investigation and action. For groundwater samples, the EQ kit performed well relative to the WHO arsenic limit and therefore could provide a vital tool for water arsenic surveillance.
A Multicenter Study To Evaluate the Performance of High-Throughput Sequencing for Virus Detection
Ng, Siemon H. S.; Vandeputte, Olivier; Aljanahi, Aisha; Deyati, Avisek; Cassart, Jean-Pol; Charlebois, Robert L.; Taliaferro, Lanyn P.
2017-01-01
ABSTRACT The capability of high-throughput sequencing (HTS) for detection of known and unknown viruses makes it a powerful tool for broad microbial investigations, such as evaluation of novel cell substrates that may be used for the development of new biological products. However, like any new assay, regulatory applications of HTS need method standardization. Therefore, our three laboratories initiated a study to evaluate performance of HTS for potential detection of viral adventitious agents by spiking model viruses in different cellular matrices to mimic putative materials for manufacturing of biologics. Four model viruses were selected based upon different physical and biochemical properties and commercial availability: human respiratory syncytial virus (RSV), Epstein-Barr virus (EBV), feline leukemia virus (FeLV), and human reovirus (REO). Additionally, porcine circovirus (PCV) was tested by one laboratory. Independent samples were prepared for HTS by spiking intact viruses or extracted viral nucleic acids, singly or mixed, into different HeLa cell matrices (resuspended whole cells, cell lysate, or total cellular RNA). Data were obtained using different sequencing platforms (Roche 454, Illumina HiSeq1500 or HiSeq2500). Bioinformatic analyses were performed independently by each laboratory using available tools, pipelines, and databases. The results showed that comparable virus detection was obtained in the three laboratories regardless of sample processing, library preparation, sequencing platform, and bioinformatic analysis: between 0.1 and 3 viral genome copies per cell were detected for all of the model viruses used. This study highlights the potential for using HTS for sensitive detection of adventitious viruses in complex biological samples containing cellular background. IMPORTANCE Recent high-throughput sequencing (HTS) investigations have resulted in unexpected discoveries of known and novel viruses in a variety of sample types, including research materials, clinical materials, and biological products. Therefore, HTS can be a powerful tool for supplementing current methods for demonstrating the absence of adventitious or unwanted viruses in biological products, particularly when using a new cell line. However, HTS is a complex technology with different platforms, which needs standardization for evaluation of biologics. This collaborative study was undertaken to investigate detection of different virus types using two different HTS platforms. The results of the independently performed studies demonstrated a similar sensitivity of virus detection, regardless of the different sample preparation and processing procedures and bioinformatic analyses done in the three laboratories. Comparable HTS detection of different virus types supports future development of reference virus materials for standardization and validation of different HTS platforms. PMID:28932815
Johnson, Steven M.; Swanson, Robert B.
1994-01-01
Prototype stream-monitoring sites were operated during part of 1992 in the Central Nebraska Basins (CNBR) and three other study areas of the National Water-Quality Assessment (NAWQ) Program of the U.S. Geological Survey. Results from the prototype project provide information needed to operate a net- work of intensive fixed station stream-monitoring sites. This report evaluates operating procedures for two NAWQA prototype sites at Maple Creek near Nickerson and the Platte River at Louisville, eastern Nebraska. Each site was sampled intensively in the spring and late summer 1992, with less intensive sampling in midsummer. In addition, multiple samples were collected during two high- flow periods at the Maple Creek site--one early and the other late in the growing season. Water-samples analyses included determination of pesticides, nutrients, major ions, suspended sediment, and measurements of physical properties. Equipment and protocols for the water-quality sampling procedures were evaluated. Operation of the prototype stream- monitoring sites included development and comparison of onsite and laboratory sample-processing proce- dures. Onsite processing was labor intensive but allowed for immediate preservation of all sampled constituents. Laboratory processing required less field labor and decreased the risk of contamination, but allowed for no immediate preservation of the samples.
GMOseek: a user friendly tool for optimized GMO testing.
Morisset, Dany; Novak, Petra Kralj; Zupanič, Darko; Gruden, Kristina; Lavrač, Nada; Žel, Jana
2014-08-01
With the increasing pace of new Genetically Modified Organisms (GMOs) authorized or in pipeline for commercialization worldwide, the task of the laboratories in charge to test the compliance of food, feed or seed samples with their relevant regulations became difficult and costly. Many of them have already adopted the so called "matrix approach" to rationalize the resources and efforts used to increase their efficiency within a limited budget. Most of the time, the "matrix approach" is implemented using limited information and some proprietary (if any) computational tool to efficiently use the available data. The developed GMOseek software is designed to support decision making in all the phases of routine GMO laboratory testing, including the interpretation of wet-lab results. The tool makes use of a tabulated matrix of GM events and their genetic elements, of the laboratory analysis history and the available information about the sample at hand. The tool uses an optimization approach to suggest the most suited screening assays for the given sample. The practical GMOseek user interface allows the user to customize the search for a cost-efficient combination of screening assays to be employed on a given sample. It further guides the user to select appropriate analyses to determine the presence of individual GM events in the analyzed sample, and it helps taking a final decision regarding the GMO composition in the sample. GMOseek can also be used to evaluate new, previously unused GMO screening targets and to estimate the profitability of developing new GMO screening methods. The presented freely available software tool offers the GMO testing laboratories the possibility to select combinations of assays (e.g. quantitative real-time PCR tests) needed for their task, by allowing the expert to express his/her preferences in terms of multiplexing and cost. The utility of GMOseek is exemplified by analyzing selected food, feed and seed samples from a national reference laboratory for GMO testing and by comparing its performance to existing tools which use the matrix approach. GMOseek proves superior when tested on real samples in terms of GMO coverage and cost efficiency of its screening strategies, including its capacity of simple interpretation of the testing results.
Koller, Marianne; Becker, Christian; Thiermann, Horst; Worek, Franz
2010-05-15
The purpose of this study was to check the applicability of different analytical methods for the identification of unknown nerve agents in human body fluids. Plasma and urine samples were spiked with nerve agents (plasma) or with their metabolites (urine) or were left blank. Seven random samples (35% of all samples) were selected for the verification test. Plasma was worked up for unchanged nerve agents and for regenerated nerve agents after fluoride-induced reactivation of nerve agent-inhibited butyrylcholinesterase. Both extracts were analysed by GC-MS. Metabolites were extracted from plasma and urine, respectively, and were analysed by LC-MS. The urinary metabolites and two blank samples could be identified without further measurements, plasma metabolites and blanks were identified in six of seven samples. The analysis of unchanged nerve agent provided five agents/blanks and the sixth agent after further investigation. The determination of the regenerated agents also provided only five clear findings during the first screening because of a rather noisy baseline. Therefore, the sample preparation was extended by a size exclusion step performed before addition of fluoride which visibly reduced baseline noise and thus improved identification of the two missing agents. The test clearly showed that verification should be performed by analysing more than one biomarker to ensure identification of the agent(s). Copyright (c) 2010 Elsevier B.V. All rights reserved.
Kupina, Steve; Roman, Mark
2014-01-01
An international collaborative study was conducted of an HPLC-refractive index (RI) detector method for the determination of the combined amounts of sugars, glycerol, organic acids, and phenolic compounds in wines and wine-like beverages. Nine collaborating laboratories representing major winery, contract laboratories, and government laboratories tested eight different materials as blind duplicates using the proposed method. Sample materials included red and white wines, port, wine cooler, and nonalcoholic wine. One material was a negative control, and one material was a reference material. Samples were either treated with an ion-exchange resin to remove interfering organic acids prior to analysis or left untreated to include organic acids and phenolics. Red wine samples were treated with polyvinylpolypyrrolidone to remove potential interferences from phenolics prior to analysis. The HPLC analyses were performed on a Bio-Rad Fast Acid Analysis Column using RI detection. Reproducibility (RSD(R)) for untreated samples (sugars + phenolics + organic acids) ranged from 6.6% for Titrivin AA4 reference material to 11.0% for dry red wine. RSD(R) for treated samples (sugars only) ranged from 6.8% for white zinfandel to 18.9% for dry white wine. RSD(R) for treated samples (sugars only) + glycerol ranged from 6.4% for white zinfandel to 19.8% for dry red wine. Based on these results, the method was adopted as Official First Action status for determination of total carbohydrates in wine and wine-like beverages.
Cho, Min-Chul; Kim, So Young; Jeong, Tae-Dong; Lee, Woochang; Chun, Sail; Min, Won-Ki
2014-11-01
Verification of new lot reagent's suitability is necessary to ensure that results for patients' samples are consistent before and after reagent lot changes. A typical procedure is to measure results of some patients' samples along with quality control (QC) materials. In this study, the results of patients' samples and QC materials in reagent lot changes were analysed. In addition, the opinion regarding QC target range adjustment along with reagent lot changes was proposed. Patients' sample and QC material results of 360 reagent lot change events involving 61 analytes and eight instrument platforms were analysed. The between-lot differences for the patients' samples (ΔP) and the QC materials (ΔQC) were tested by Mann-Whitney U tests. The size of the between-lot differences in the QC data was calculated as multiples of standard deviation (SD). The ΔP and ΔQC values only differed significantly in 7.8% of the reagent lot change events. This frequency was not affected by the assay principle or the QC material source. One SD was proposed for the cutoff for maintaining pre-existing target range after reagent lot change. While non-commutable QC material results were infrequent in the present study, our data confirmed that QC materials have limited usefulness when assessing new reagent lots. Also a 1 SD standard for establishing a new QC target range after reagent lot change event was proposed. © The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav.
Esmaeili Rastaghi, Ahmad Reza; Spotin, Adel; Khataminezhad, Mohammad Reza; Jafarpour, Mostafa; Alaeenovin, Elnaz; Najafzadeh, Narmin; Samei, Neda; Taleshi, Neda; Mohammadi, Somayeh; Parvizi, Parviz
2017-10-01
Leishmaniasis as an emerging and reemerging disease is increasing worldwide with high prevalence and new incidence in recent years. For epidemiological investigation and accurate identification of Leishmania species, three nuclear and mitochondrial genes (ITS-rDNA, Hsp70, and Cyt b ) were employed and analyzed from clinical samples in three important Zoonotic Cutaneous Leishmaniasis (ZCL) foci of Iran. In this cross-sectional/descriptive study conducted in 2014-15, serous smears of lesions were directly prepared from suspected patients of ZCL in Turkmen in northeast, Abarkouh in center and Shush district in southwest of Iran. They were directly prepared from suspected patients and DNA was extracted. Two nuclear genes of ITS-rDNA, Hsp70 and one mitochondrial gene of Cyt b within Leishmania parasites were amplified. RFLP was performed on PCR-positive samples. PCR products were sequenced, aligned and edited with sequencher 4.1.4 and phylogenic analyses performed using MEGA 5.05 software. Overall, 203 out of 360 clinical samples from suspected patients were Leishmania positive using routine laboratory methods and 231 samples were positive by molecular techniques. L. major L. tropica , and L. turanica were firmly identified by employing different molecular genes and phylogenic analyses. By combining different molecular genes, Leishmania parasites were identified accurately. The sensitivity and specificity three genes were evaluated and had more advantages to compare routine laboratory methods. ITS-rDNA gene is more appropriate for firm identification of Leishmania species.
Applicability of two mobile analysers for mercury in urine in small-scale gold mining areas.
Baeuml, Jennifer; Bose-O'Reilly, Stephan; Lettmeier, Beate; Maydl, Alexandra; Messerer, Katalin; Roider, Gabriele; Drasch, Gustav; Siebert, Uwe
2011-12-01
Mercury is still used in developing countries to extract gold from the ore in small-scale gold mining areas. This is a major health hazard for people living in mining areas. The concentration of mercury in urine was analysed in different mining areas in Zimbabwe, Indonesia and Tanzania. First the urine samples were analysed by CV-AAS (cold vapour atomic absorption spectrometry) during the field projects with a mobile mercury analyser (Lumex(®) or Seefelder(®)) and secondly, in a laboratory with a stationary CV-AAS mercury analyser (PerkinElmer(®)). Caused by the different systems (reduction agent either SnCl(2) (Lumex(®) or Seefelder(®))) or NaBH(4) (PerkinElmer(®)), with the mobile analysers only the inorganic mercury was obtained and with the stationary system the total mercury concentration was measured. The aims of the study were whether the results obtained in field with the mobile equipments can be compared with the stationary reference method in the laboratory and allow the application of these mobile analysers in screening studies on concerned populations to select those, who are exposed to critical mercury levels. Overall, the concentrations obtained with the two mobile systems were approximately 25% lower than determined with the stationary system. Nevertheless, both mobile systems seem to be very useful for screening of volunteers in field. Moreover, regional staff may be trained on such analysers to perform screening tests by themselves. Copyright © 2011 Elsevier GmbH. All rights reserved.
Harju, Kirsi; Rapinoja, Marja-Leena; Avondet, Marc-André; Arnold, Werner; Schär, Martin; Luginbühl, Werner; Kremp, Anke; Suikkanen, Sanna; Kankaanpää, Harri; Burrell, Stephen; Söderström, Martin; Vanninen, Paula
2015-01-01
A saxitoxin (STX) proficiency test (PT) was organized as part of the Establishment of Quality Assurance for the Detection of Biological Toxins of Potential Bioterrorism Risk (EQuATox) project. The aim of this PT was to provide an evaluation of existing methods and the European laboratories’ capabilities for the analysis of STX and some of its analogues in real samples. Homogenized mussel material and algal cell materials containing paralytic shellfish poisoning (PSP) toxins were produced as reference sample matrices. The reference material was characterized using various analytical methods. Acidified algal extract samples at two concentration levels were prepared from a bulk culture of PSP toxins producing dinoflagellate Alexandrium ostenfeldii. The homogeneity and stability of the prepared PT samples were studied and found to be fit-for-purpose. Thereafter, eight STX PT samples were sent to ten participating laboratories from eight countries. The PT offered the participating laboratories the possibility to assess their performance regarding the qualitative and quantitative detection of PSP toxins. Various techniques such as official Association of Official Analytical Chemists (AOAC) methods, immunoassays, and liquid chromatography-mass spectrometry were used for sample analyses. PMID:26602927
Conclusions on measurement uncertainty in microbiology.
Forster, Lynne I
2009-01-01
Since its first issue in 1999, testing laboratories wishing to comply with all the requirements of ISO/IEC 17025 have been collecting data for estimating uncertainty of measurement for quantitative determinations. In the microbiological field of testing, some debate has arisen as to whether uncertainty needs to be estimated for each method performed in the laboratory for each type of sample matrix tested. Queries also arise concerning the estimation of uncertainty when plate/membrane filter colony counts are below recommended method counting range limits. A selection of water samples (with low to high contamination) was tested in replicate with the associated uncertainty of measurement being estimated from the analytical results obtained. The analyses performed on the water samples included total coliforms, fecal coliforms, fecal streptococci by membrane filtration, and heterotrophic plate counts by the pour plate technique. For those samples where plate/membrane filter colony counts were > or =20, uncertainty estimates at a 95% confidence level were very similar for the methods, being estimated as 0.13, 0.14, 0.14, and 0.12, respectively. For those samples where plate/membrane filter colony counts were <20, estimated uncertainty values for each sample showed close agreement with published confidence limits established using a Poisson distribution approach.
McCrory, Patricia A.; Constantz, James E.; Hunt, Andrew G.
2017-01-31
IntroductionThis U.S. Geological Survey report presents laboratory analyses along with field notes for an exploratory study to document the relative abundance of noble gases in mineral springs and water wells within the Cascadia forearc of Washington, Oregon, and California (fig. 1). This report describes 14 samples collected in 2014 and 2015 and complements a previous report that describes 9 samples collected in 2012 and 2013 (McCrory and others, 2014b). Estimates of the depth to the underlying Juan de Fuca oceanic plate beneath sample sites are derived from the McCrory and others (2012) slab model. Some of the springs have been previously sampled for chemical analyses (Mariner and others, 2006), but none of the springs or wells currently has publicly available noble gas data. The helium and neon isotope values and ratios presented below are used to determine the sources and mixing history of these mineral and well waters (for example, McCrory and others, 2016).
Ground-water quality for Grainger County, Tennessee
Weaver, J.D.; Patel, A.R.; Hickey, A.C.
1994-01-01
The residents of Grainger County depend on ground water for many of their daily needs including personal consumption and crop irrigation. To address concerns associated with ground-water quality related to domestic use, the U.S. Geological Survey collected water samples from 35 wells throughout the county during the summer 1992. The water samples were analyzed to determine if pesticides, nutrients, bacteria, and other selected constituents were present in the ground water. Wells selected for the study were between 100 and 250 feet deep and yielded 10 to 50 gallons of water per minute. Laboratory analyses of the water found no organic pesticides at concentrations exceeding the primary maximum contaminant levels established by the State of Tennessee for wells used for public supply. However, fecal coliform bacteria were detected at concentrations exceeding the State's maximum contaminant level in water from 15 of the 35 wells sampled. Analyses also indicated several inorganic compounds were present in the water samples at concentrations exceeding the secondary maximum contaminant level.
NASA Astrophysics Data System (ADS)
Wall, A. M.; Brabander, D. J.
2005-05-01
The area of Hewitt's Cove, Hingham, Massachusetts structurally represents the southern extent of the Boston Basin, and as such, provides the opportunity to identify and recognize basin-wide events. While the stratigraphy of the Boston Basin has been developed since the advent of U-Pb geochronology and formal stratigraphic facies descriptions (Socci and Smith, 2001), the stratigraphy of the Hewitt's Cove area has not been thoroughly addressed since the work of William O. Crosby in 1894 (Billings, 1976, Bailey and Bland, 2001). Hewitt's Cove consists of an andesitic basaltic flow, approximately 150 m thick, overlain by siltstone and conglomeratic sequences. Field-Portable X-Ray Fluorescence (FP-XRF) was used on fresh and weathered surfaces on the outcrop and in hand samples, and these analyses were compared with conventional laboratory XRF analyses. The in situ field-based analyses produced a reproducible chemostratigraphy that is consistent with subsequent laboratory-based analyses. These data suggest that the series of andesitic basalt flows at Hewitt's Cove are the result of compositionally different magmatic pulses. Additional analyses must be completed to determine the extent of these pulses and the extent of variation in this area before further conclusions can be made. This study particularly demonstrates the utility of using FP-XRF in igneous geologic applications.
Plant, Jon D; Neradelik, Moni B; Polissar, Nayak L; Fadok, Valerie A; Scott, Brian A
2014-01-01
Background Canine allergen-specific IgE assays in the USA are not subjected to an independent laboratory reliability monitoring programme. Hypothesis/Objectives The aim of this study was to evaluate the agreement of diagnostic results and treatment recommendations of four serum IgE assays commercially available in the USA. Methods Replicate serum samples from 10 atopic dogs were submitted to each of four laboratories for allergen-specific IgE assays (ACTT®, VARL Liquid Gold, ALLERCEPT® and Greer® Aller-g-complete®). The interlaboratory agreement of standard, regional panels and ensuing treatment recommendations were analysed with the kappa statistic (κ) to account for agreement that might occur merely by chance. Six comparisons of pairs of laboratories and overall agreement among laboratories were analysed for ungrouped allergens (as tested) and also with allergens grouped according to reported cross-reactivity and taxonomy. Results The overall chance-corrected agreement of the positive/negative test results for ungrouped and grouped allergens was slight (κ = 0.14 and 0.13, respectively). Subset analysis of the laboratory pair with the highest level of diagnostic agreement (κ = 0.36) found slight agreement (κ = 0.13) for ungrouped plants and fungi, but substantial agreement (κ = 0.71) for ungrouped mites. The overall agreement of the treatment recommendations was slight (κ = 0.11). Altogether, 85.1% of ungrouped allergen treatment recommendations were unique to one laboratory or another. Conclusions and clinical importance Our study indicated that the choice of IgE assay may have a major influence on the positive/negative results and ensuing treatment recommendations. PMID:24461034
NASA Astrophysics Data System (ADS)
Focke, Maximilian; Mark, Daniel; Stumpf, Fabian; Müller, Martina; Roth, Günter; Zengerle, Roland; von Stetten, Felix
2011-06-01
Two microfluidic cartridges intended for upgrading standard laboratory instruments with automated liquid handling capability by use of centrifugal forces are presented. The first microfluidic cartridge enables purification of DNA from human whole blood and is operated in a standard laboratory centrifuge. The second microfluidic catridge enables genotyping of pathogens by geometrically multiplexed real-time PCR. It is operated in a slightly modified off-the-shelf thermal cycler. Both solutions aim at smart and cost-efficient ways to automate work flows in laboratories. The DNA purification cartridge automates all liquid handling steps starting from a lysed blood sample to PCR ready DNA. The cartridge contains two manually crushable glass ampoules with liquid reagents. The DNA yield extracted from a 32 μl blood sample is 192 +/- 30 ng which corresponds to 53 +/- 8% of a reference extraction. The genotyping cartridge is applied to analyse isolates of the multi-resistant Staphyloccus aureus (MRSA) by real-time PCR. The wells contain pre-stored dry reagents such as primers and probes. Evaluation of the system with 44 genotyping assays showed a 100% specificity and agreement with the reference assays in standard tubes. The lower limit of detection was well below 10 copies of DNA per reaction.
Densmore, Christine L.; Blazer, V.S.; Cartwright, Deborah D.; Schill, W.B.; Schachte, J.H.; Petrie, C.J.; Batur, M.V.; Waldrop, T.B.; Mack, A.; Pooler, P.S.
2001-01-01
Three strains of rainbow trout and steelhead Oncorhynchus mykiss were evaluated for the presence of whirling disease in field and laboratory trials. In the field exposures, fingerling Salmon River steelhead and Cayuga Lake and Randolph strains of rainbow trout were placed in wire cages in an earthen, stream-fed pond in New York State that was known to harbor Myxobolus cerebralis. Control fish were held at another hatchery that was free of whirling disease. In the controlled trials at the National Fish Health Research Laboratory, fingerling steelhead and Cayuga Lake and Mount Lassen rainbow trout were exposed to triactinomyxons at low (200 triactinomyxons/fish) or high (2,000 triactinomyxons/fish) levels for 2 h. Controls of each group were sham-exposed. Following an incubation period of 154 d for laboratory trials and 180 d for field trials, cranial tissue samples were taken for spore enumeration (field and laboratory trials) and histological analyses (laboratory only). Clinical signs of disease, including whirling behavior, blacktail, and skeletal deformities, were recorded for each fish in the laboratory trial at the terminal sampling. No clinical evidence of disease was noted among fish in the field trials. Clinical signs were noted among all strains in the laboratory trials at both exposure levels, and these signs were consistently greatest for the Mount Lassen strain. Whirling and skeletal deformities were more evident in the steelhead than in the Cayuga Lake rainbow trout; blacktail was more common in the Cayuga Lake fish. In both field and laboratory trials, spore counts were significantly higher for Cayuga Lake rainbow trout than in steelhead. In laboratory trials, moderate to marked cranial tissue lesions predominated in all three strains.
A laboratory rainfall simulator to study the soil erosion and runoff water
NASA Astrophysics Data System (ADS)
Cancelo González, Javier; Rial, M. E.; Díaz-Fierros, Francisco
2010-05-01
The soil erosion and the runoff water composition in some areas affected by forest fires or submitted to intensive agriculture are an important factor to keep an account, particularly in sensitive areas like estuary and rias that have a high importance in the socioeconomic development of some regions. An understanding of runoff production indicates the processes by which pollutants reach streams and also indicates the management techniques that might be uses to minimize the discharge of these materials into surface waters. One of the most methodology implemented in the soil erosion studies is a rainfall simulation. This method can reproduce the natural soil degradation processes in field or laboratory experiences. With the aim of improve the rainfall-runoff generation, a laboratory rainfall simulator which incorporates a fan-like intermittent water jet system for rainfall generation were modified. The major change made to the rainfall simulator consist in a system to coupling stainless steel boxes, whose dimensions are 12 x 20 x 45 centimeters, and it allows to place soil samples under the rainfall simulator. Previously these boxes were used to take soil samples in field with more of 20 centimeters of depth, causing the minimum disturbance in their properties and structure. These new implementations in the rainfall simulator also allow collect water samples of runoff in two ways: firstly, the rain water that constituted the overland flow or direct runoff and besides the rain water seeps into the soil by the process of infiltration and contributed to the subsurface runoff. Among main the variables controlled in the rainfall simulations were the soil slope and the intensity and duration of rainfall. With the aim of test the prototype, six soil samples were collected in the same sampling point and subjected to rainfall simulations in laboratory with the same intensity and duration. Two samples will constitute the control test, and they were fully undisturbed, and four samples were subjected to controlled burnings with different fire severity: two samples burnt to 250°C and the other two samples burnt to 450°C. Preliminary laboratory data of soil erosion and surface and subsurface runoff were obtained. The water parameters analysed were: pH, electrical conductivity, temperature (in the moment of sampling) and suspended sediments, ammonium, nitrates, total nitrogen (Kjeldahl method), within 24 hours after sampling.
Segmental hair analysis in order to evaluate driving performance.
Stramesi, C; Polla, M; Vignali, C; Zucchella, A; Groppi, A
2008-03-21
On the 31st of July 2002 the Lombardy local government issued a memorandum, C.R. 35/SAN, providing "guidelines to investigate drugs of abuse addiction in order to judge driving performance". About hair samples, this memorandum advises that the proximal lock of 6 cm-length would be analysed for opiates, cocaine, cannabinoids, amphetamine and derivatives, divided into two segments of 3 cm each. The Local Medical Driving Licence Commissions (CML) can decide whether or not to enforce these instructions; from our survey it resulted that most CMLs do not abide by the memorandum, not requiring segmental analysis. The purpose of our study was to verify whether this procedural discordance could affect analytical results and, consequently, the evaluation of the subject's driving performance. We analysed hair samples taken from subjects who were requesting the renewal of their driving licence in our Laboratory during the period from 1 August 2002 to 31 December 2006. We divided samples into two groups: (1) samples previously analysed in one single segment which resulted positive for at least one analyte, but under the cut-off (0.5 ng/mg), were re-analysed in accordance with the guidelines; (2) samples previously processed following guidelines which resulted positive in one of the segments were newly analysed in a single segment. Comparing the new results with the original ones, an increase of positive results emerged in the first group. The second set of results fully supported the first ones. These results underscore the importance of the 35/SAN memorandum, so if the guidelines had been followed there would have been a larger amount of driving licence renewal denied.
Assessment the impact of samplers change on the uncertainty related to geothermalwater sampling
NASA Astrophysics Data System (ADS)
Wątor, Katarzyna; Mika, Anna; Sekuła, Klaudia; Kmiecik, Ewa
2018-02-01
The aim of this study is to assess the impact of samplers change on the uncertainty associated with the process of the geothermal water sampling. The study was carried out on geothermal water exploited in Podhale region, southern Poland (Małopolska province). To estimate the uncertainty associated with sampling the results of determinations of metasilicic acid (H2SiO3) in normal and duplicate samples collected in two series were used (in each series the samples were collected by qualified sampler). Chemical analyses were performed using ICP-OES method in the certified Hydrogeochemical Laboratory of the Hydrogeology and Engineering Geology Department at the AGH University of Science and Technology in Krakow (Certificate of Polish Centre for Accreditation No. AB 1050). To evaluate the uncertainty arising from sampling the empirical approach was implemented, based on double analysis of normal and duplicate samples taken from the same well in the series of testing. The analyses of the results were done using ROBAN software based on technique of robust statistics analysis of variance (rANOVA). Conducted research proved that in the case of qualified and experienced samplers uncertainty connected with the sampling can be reduced what results in small measurement uncertainty.
Cosgun, Yasemin; Guldemir, Dilek; Coskun, Aslihan; Yolbakan, Sultan; Kalaycioglu, Atila Taner; Korukluoglu, Gulay; Durmaz, Riza
2018-04-01
Measles is an important childhood infection targeted to be eliminated by the World Health Organization (WHO). Virus circulation has not been interrupted in the European Region because high vaccination rates could not be achieved among some countries of the WHO European Region including Turkey. The purpose of this study was to evaluate the laboratory findings of measles cases confirmed in the last nine years, to assess the epidemiological data of the cases, to determine the molecular genotyping studies and to emphasise the importance of laboratory-based surveillance in measles. From 2007 to 2010, only 18 imported cases were detected in Turkey. However, this number increased with a local outbreak of 111 cases in 2011, followed by another outbreak in 2012 in Istanbul that spread countrywide in the following two years; a total of 8661 laboratory-confirmed measles cases were reported from 2012 to 2015. After ELISA detection of a measles IgM-positive result in serum samples of potential measles cases, RT-PCR was performed with urine or nasopharyngeal swab samples of patients, and amplicons were subjected to sequencing. In the samples of 2010 and 2011, D4 and D9 genotypes were mainly detected; as of 2012, the D8 genotype has gained importance. Although D8 was also identified in 2014, in the same year genotype H1 viruses were detected in Turkey for the first time. Therefore, it is important to perform a genotypic analysis of the virus causing the outbreak, analyse epidemiological connections of the contact, determine the source of the outbreak and plan measures based on this information.
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
Vanhoof, Chris; Corthouts, Valère; Tirez, Kristof
2004-04-01
To determine the heavy metal content in soil samples at contaminated locations, a static and time consuming procedure is used in most cases. Soil samples are collected and analyzed in the laboratory at high quality and high analytical costs. The demand by government and consultants for a more dynamic approach and by customers requiring performances in which analyses are performed in the field with immediate feedback of the analytical results, is growing. Especially during the follow-up of remediation projects or during the determination of the sampling strategy, field analyses are advisable. For this purpose four types of ED-XRF systems, ranging from portable up to high performance laboratory systems, have been evaluated. The evaluation criteria are based on the performance characteristics for all the ED-XRF systems such as limit of detection, accuracy and the measurement uncertainty on one hand, and also the influence of the sample pretreatment on the obtained results on the other hand. The study proved that the field portable system and the bench top system, placed in a mobile van, can be applied as field techniques, resulting in semi-quantitative analytical results. A limited homogenization of the analyzed sample significantly increases the representativeness of the soil sample. The ED-XRF systems can be differentiated by their limits of detection which are a factor of 10 to 20 higher for the portable system. The accuracy of the results and the measurement uncertainty also improved using the bench top system. Therefore, the selection criteria for applicability of both field systems are based on the required detection level and also the required accuracy of the results.
Variable temperature sensitivity of soil organic carbon in North American forests
Cinzia Fissore; Christian P. Giardina; Christopher W. Swanston; Gary M. King; Randall K. Kolka
2009-01-01
We investigated mean residence time (MRT) for soil organic carbon (SOC) sampled from paired hardwood and pine forests located along a 22 °C mean annual temperature (MAT) gradient in North America. We used acid hydrolysis fractionation, radiocarbon analyses, long-term laboratory incubations (525-d), and a three-pool model to describe the size and kinetics of...
Ball, James W.; Nordstrom, D. Kirk; Cunningham, Kirk M.; Schoonen, Martin A.; Xu, Yong; DeMonge, Jennifer M.
1998-01-01
Forty-two water analyses are reported for samples collected at 8 hot springs and their overflow drainages, two geysers, and two ambient-temperature acid streams in Yellowstone National Park during 1994-95. These water samples were collected and analyzed as part of the initial research investigations on sulfur redox speciation in the hot springs of Yellowstone and to document chemical changes in overflows that affect major ions, redox species, and trace elements. The sulfur redox speciation research is a collaboration between the State University of New York (SUNY) at Stony Brook and the U.S. Geological Survey (USGS). Four hot springs, Ojo Caliente, Azure, Frying Pan, and Angel Terrace, were studied in detail. Analyses were performed adjacent to the sampling site or in an on-site mobile lab truck constructed by the USGS, or later in a USGS laboratory. Water temperature, specific conductance, pH, Eh, D.O., and dissolved H2S were determined adjacent to the sample source at the time of sampling. Alkalinity and F- were determined on-site on the day of sample collection. Thiosulfate and polythionates were determined as soon as possible (minutes to hours later) by ion chromatography (IC). Other major anions (Cl-, SO4 2-, Br-) also were determined on-site by IC within two days of sample collection. Ammonium, Fe(II), and Fe(total) were determined on-site by ultraviolet/visible spectrophotometry within two days of sample collection. Later in the USGS laboratory, densities were determined. Concentrations of Ca, Mg, Li, Na, and K were determined by flame atomic absorption and emission (Na, K) spectrometry. Concentrations of Al, As, B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe(total), K, Mg, Mn, Na, Ni, Pb, Si, Sr, V, and Zn were determined by inductively-coupled plasma optical emission spectrometry. Trace concentrations of Al and Mg were determined by Zeeman-corrected graphite furnace atomic absorption spectrometry. Three important conclusions from the sampling and analyses are: (1) variability in H2S concentrations can be caused as much by sampling and preservation artifacts as by actual variations in water composition over time, (2) historical determinations of S2O3 2- were subject to overestimation, most likely because of inadequate preservation leading to H2S oxidation, and (3) S2O3 2- is a common constituent of hot spring waters.
Basic data from five core holes in the Raft River geothermal area, Cassia County, Idaho
Crosthwaite, E. G.
1976-01-01
meters) were completed in the area (Crosthwaite, 1974), and the Aerojet Nuclear Company, under the auspices of the U.S. Energy Research and Development Administration, was planning some deep drilling 4,000 to 6,000 feet (1,200 to 1,800 meters) (fig. 1). The purpose of the core drilling was to provide information to test geophysical interpretations of the subsurface structure and lithology and to provide hydrologic and geologic data on the shallow part of the geothermal system. Samples of the core were made available to several divisions and branches of the Geological Survey and to people and agencies outside the Survey. This report presents the basic data from the core holes that had been collected to September 1, 1975, and includes lithologic and geophysical well logs, chemical analyses of water (table 1), and laboratory analyses of cores (table 2) that were completed as of the above date. The data were collected by the Idaho District office, Hydrologic Laboratory, Borehole Geophysics Research Project, and Drilling, Sampling, and Testing Section, all of the Water Resources Division, and the Branch of Central Environmental Geology of the Geologic Divison.
279 - Xanes Studies on UV-Irradiated Interstellar Ice Analogs: A Comparison to STARDUST Samples
NASA Technical Reports Server (NTRS)
Milam, Stefanie N.; Cody, George D.; Kilcoyne, A. L. David; Nuevo, Michel; Sandford, Scott A.; Stroud, Rhonda M.; DeGregorio, Bradley T.
2010-01-01
We present C-, N-, and O-XANES (X-ray Absorption Near-Edge Spectroscopy) results of organic residues produced in the laboratory from the UV irradiation of astrophysical ice analogs containing H20, CO, CH30H, NH31 in order to mimic processes that may occur in cold icy bodies of the outer Solar System, particularly in comets, Such analyses showed that laboratory-formed organic residues mainly consist of a solid phase and an oily phase. C-XANES analysis of the solid phase suggests a rich distribution of organic functionalities, among which carbonyl groups, C=C bonds, and alcohols are present. Results from N-XANES indicate the possible presence of amide, amine, and nitrile groups, The O-XANES spectra confirmed the a-bearing groups, These results are compared with the XANES spectra obtained from STARDUST cometary samples,
NASA Astrophysics Data System (ADS)
Scarciglia, Fabio; Morrone, Fabio; Pelle, Teresa; Buttafuoco, Gabriele; Conforti, Massimo; Muto, Francesco; Critelli, Salvatore; Fabbricatore, Davide; Filomena, Luciana; Rago, Valeria; Robustelli, Gaetano; Tripodi, Vincenzo; Versace, Pasquale
2015-04-01
Effects of chemical and physical weathering processes on different rock types as predisposing factors of a number of landslides are often investigated in detail. Conversely, very few research studies on triggering mechanisms of shallow landslides and related risk assessment are focused on evaluation of morphological and physical discontinuities caused by pedogenetic processes affecting parent materials. Also sampling strategies for geotechnical or hydrological laboratory analyses can be biased by the lack of detailed information about the soil spatial variability and of a consequent horizon-wise selection of samples from soil profiles. In this work we summarize the main results on the assessment of shallow landslide susceptibility along the A3 highway section between Cosenza Sud and Altilia in northern Calabria (southern Italy). This research is part of a wider project (PON01-01503: "Integrated systems for hydrogeological risk monitoring, early warning and mitigation along the main lifelines"), aimed at hydro-geological risk mitigation and early warning along three highway sections of southern Italy. Based on a detailed geological and geomorphological survey, the main lithological, structural and relief features of the landscape were mapped, with a special emphasis on active, dormant and inactive landslides and their geo-lithological control factors. A soil survey was also carried out in the field, showing a dominance of Entisols and Inceptisols on steep slopes, and Mollisols and Alfisols on gentle landforms. Soil observations were focused on the identification of pedological discontinuities as potential factors that might trigger shallow landslides. A number of soil profiles, often close to landslide scarps, evidenced significant morphological changes of the parent materials, such as texture, pedogenic structure, dry consistence and moisture, or hydromorphic features caused by transient water-logging conditions, and clay-illuviated horizons. Buried soils were recognized, often truncated by erosion, and overlain by younger soils developed on colluvia, debris flows and detrital slope deposits. Five representative soil profiles were selected and sampled for pedological, geotechnical and hydrological laboratory analyses. Bulk and undisturbed samples were collected for chemical and physical soil analyses (particle size distribution, organic and inorganic carbon, pH, electrical conductivity, soluble salts), for determining bulk density, Atterberg limits, cohesive strength, angle of internal friction, water retention and for thin sections to be observed under an optical polarizing microscope, respectively. Preliminary results of laboratory analyses showed irregular patterns of pedological (particle size distribution, organic matter content, bulk density), geotechnical (Atterberg limits) and hydrological data (water content, pore distribution) along the soil profiles, coherently with field observations.
Oblinger, Carolyn J.
2004-01-01
The Triangle Area Water Supply Monitoring Project was initiated in October 1988 to provide long-term water-quality data for six area water-supply reservoirs and their tributaries. In addition, the project provides data that can be used to determine the effectiveness of large-scale changes in water-resource management practices, document differences in water quality among water-supply types (large multiuse reservoir, small reservoir, run-of-river), and tributary-loading and in-lake data for water-quality modeling of Falls and Jordan Lakes. By September 2001, the project had progressed in four phases and included as many as 34 sites (in 1991). Most sites were sampled and analyzed by the U.S. Geological Survey. Some sites were already a part of the North Carolina Division of Water Quality statewide ambient water-quality monitoring network and were sampled by the Division of Water Quality. The network has provided data on streamflow, physical properties, and concentrations of nutrients, major ions, metals, trace elements, chlorophyll, total organic carbon, suspended sediment, and selected synthetic organic compounds. Project quality-assurance activities include written procedures for sample collection, record management and archive, collection of field quality-control samples (blank samples and replicate samples), and monitoring the quality of field supplies. In addition to project quality-assurance activities, the quality of laboratory analyses was assessed through laboratory quality-assurance practices and an independent laboratory quality-control assessment provided by the U.S. Geological Survey Branch of Quality Systems through the Blind Inorganic Sample Project and the Organic Blind Sample Project.
Custer, Christine M.; Custer, Thomas W.; Dummer, Paul; Etterson, Matthew A.; Thogmartin, Wayne E.; Wu, Qian; Kannan, Kurunthachalam; Trowbridge, Annette; McKann, Patrick C.
2013-01-01
The exposure and effects of perfluoroalkyl substances (PFASs) were studied at eight locations in Minnesota and Wisconsin between 2007 and 2011 using tree swallows (Tachycineta bicolor). Concentrations of PFASs were quantified as were reproductive success end points. The sample egg method was used wherein an egg sample is collected, and the hatching success of the remaining eggs in the nest is assessed. The association between PFAS exposure and reproductive success was assessed by site comparisons, logistic regression analysis, and multistate modeling, a technique not previously used in this context. There was a negative association between concentrations of perfluorooctane sulfonate (PFOS) in eggs and hatching success. The concentration at which effects became evident (150–200 ng/g wet weight) was far lower than effect levels found in laboratory feeding trials or egg-injection studies of other avian species. This discrepancy was likely because behavioral effects and other extrinsic factors are not accounted for in these laboratory studies and the possibility that tree swallows are unusually sensitive to PFASs. The results from multistate modeling and simple logistic regression analyses were nearly identical. Multistate modeling provides a better method to examine possible effects of additional covariates and assessment of models using Akaike information criteria analyses. There was a credible association between PFOS concentrations in plasma and eggs, so extrapolation between these two commonly sampled tissues can be performed.
Synthesis of amino-functionalized silica nanoparticles for preparation of new laboratory standards
NASA Astrophysics Data System (ADS)
Alvarez-Toral, Aitor; Fernández, Beatriz; Malherbe, Julien; Claverie, Fanny; Pecheyran, Christophe; Pereiro, Rosario
2017-12-01
Platinum group elements (PGEs) are particularly interesting analytes in different fields, including environmental samples as well as high cost materials that contain them, such as for example automotive catalysts. This type of solid samples could be analysed by laser ablation (LA) coupled to ICP-MS, which allow to significantly reducing the analysis time since the time-consuming processes for sample preparation are not required. There is a considerable demand of standards with high PGEs concentration for quantification purposes, which cannot be carried out easily using LA-ICP-MS because the available standards (i.e. NIST SRM 61 × series) do not have such analytes in the same concentration range. In this paper, a new strategy is proposed for the synthesis of homogeneous laboratory standards with Pt, Pd and Rh concentrations that range from 77 μg/g of Pd up to 2035 μg/g of Rh. The proposed strategy is based on the synthesis of monodisperse amino-functionalized amorphous silica nanoparticles, which can retain metal ions. In addition to Pt, Pd and Rh, three lanthanides were also added to the nanoparticles (La, Ce, Nd). Sturdy pressed pellets can be made from the resulting nanopowder without the use of any binder. Elemental composition of standards made of nanoparticles was analysed by conventional nebulization ICP-MS and their homogeneity was successfully evaluated by LA-ICP-MS.
Breen, Kevin J.
2000-01-01
Assessments to determine whether agricultural pesticides are present in ground water are performed by the Commonwealth of Pennsylvania under the aquifer monitoring provisions of the State Pesticides and Ground Water Strategy. Pennsylvania's Department of Agriculture conducts the monitoring and collects samples; the Department of Environmental Protection (PaDEP) Laboratory analyzes the samples to measure pesticide concentration. To evaluate the quality of the measurements of pesticide concentration for a groundwater assessment, a quality-assurance design was developed and applied to a selected assessment area in Pennsylvania. This report describes the quality-assurance design, describes how and where the design was applied, describes procedures used to collect and analyze samples and to evaluate the results, and summarizes the quality assurance results along with the assessment results.The design was applied in an agricultural area of the Delaware River Basin in Berks, Lebanon, Lehigh, and Northampton Counties to evaluate the bias and variability in laboratory results for pesticides. The design—with random spatial and temporal components—included four data-quality objectives for bias and variability. The spatial design was primary and represented an area comprising 30 sampling cells. A quality-assurance sampling frequency of 20 percent of cells was selected to ensure a sample number of five or more for analysis. Quality-control samples included blanks, spikes, and replicates of laboratory water and spikes, replicates, and 2-lab splits of groundwater. Two analytical laboratories, the PaDEP Laboratory and a U.S. Geological Survey Laboratory, were part of the design. Bias and variability were evaluated by use of data collected from October 1997 through January 1998 for alachlor, atrazine, cyanazine, metolachlor, simazine, pendimethalin, metribuzin, and chlorpyrifos.Results of analyses of field blanks indicate that collection, processing, transport, and laboratory analysis procedures did not contaminate the samples; there were no false-positive results. Pesticides were detected in water when pesticides were spiked into (added to) samples. There were no false negatives for the eight pesticides in all spiked samples. Negative bias was characteristic of analytical results for the eight pesticides, and bias was generally in excess of 10 percent from the ‘true’ or expected concentration (34 of 39 analyses, or 87 percent of the ground-water results) for pesticide concentrations ranging from 0.31 to 0.51 mg/L (micrograms per liter). The magnitude of the negative bias for the eight pesticides, with the exception of cyanazine, would result in reported concentrations commonly 75-80 percent of the expected concentration in the water sample. The bias for cyanazine was negative and within 10 percent of the expected concentration. A comparison of spiked pesticide-concentration recoveries in laboratory water and ground water indicated no effect of the ground-water matrix, and matrix interference was not a source of the negative bias. Results for the laboratory-water spikes submitted in triplicate showed large variability for recoveries of atrazine, cyanazine, and pendimethalin. The relative standard deviation (RSD) was used as a measure of method variability over the course of the study for laboratory waters at a concentration of 0.4 mg/L. An RSD of about 11 percent (or about ?0.05 mg/L)characterizes the method results for alachlor, chlorpyrifos, metolachlor, metribuzin, and simazine. Atrazine and pendimethalin have RSD values of about 17 and 23 percent, respectively. Cyanazine showed the largest RSD at nearly 51 percent. The pesticides with low variability in laboratory-water spikes also had low variability in ground water.The assessment results showed that atrazinewas the most commonly detected pesticide in ground water in the assessment area. Atrazine was detected in water from 22 of the 28 wells sampled, and recovery results for atrazine were some of the worst (largest negative bias). Concentrations of the eight pesticides in ground water from wells were generally less than 0.3 µg/L. Only six individual measurements of the concentrations in water from six of the wells were at or above 0.3 µg/L, five for atrazine and one for metolachlor. There were eight additional detections of metolachlor and simazine at concentrations less than 0.1 µg/L. No well water contained more than one pesticide at concentra-tions at or above 0.3 µg/L. Evidence exists, how-ever, for a pattern of co-occurrence of metolachlor and simazine at low concentrations with higher concentrations of atrazine.Large variability in replicate samples and negative bias for pesticide recovery from spiked samples indicate the need to use data for pesticide recovery in the interpretation of measured pesti-cide concentrations in ground water. Data from samples spiked with known amounts of pesticides were a critical component of a quality-assurance design for the monitoring component of the Pesti-cides and Ground Water Strategy.Trigger concentrations, the concentrations that require action under the Pesticides and Ground Water Strategy, should be considered maximums for action. This consideration is needed because of the magnitude of negative bias.
Bridging the divide: a model-data approach to Polar and Alpine microbiology.
Bradley, James A; Anesio, Alexandre M; Arndt, Sandra
2016-03-01
Advances in microbial ecology in the cryosphere continue to be driven by empirical approaches including field sampling and laboratory-based analyses. Although mathematical models are commonly used to investigate the physical dynamics of Polar and Alpine regions, they are rarely applied in microbial studies. Yet integrating modelling approaches with ongoing observational and laboratory-based work is ideally suited to Polar and Alpine microbial ecosystems given their harsh environmental and biogeochemical characteristics, simple trophic structures, distinct seasonality, often difficult accessibility, geographical expansiveness and susceptibility to accelerated climate changes. In this opinion paper, we explain how mathematical modelling ideally complements field and laboratory-based analyses. We thus argue that mathematical modelling is a powerful tool for the investigation of these extreme environments and that fully integrated, interdisciplinary model-data approaches could help the Polar and Alpine microbiology community address some of the great research challenges of the 21st century (e.g. assessing global significance and response to climate change). However, a better integration of field and laboratory work with model design and calibration/validation, as well as a stronger focus on quantitative information is required to advance models that can be used to make predictions and upscale processes and fluxes beyond what can be captured by observations alone. © FEMS 2016.
Bridging the divide: a model-data approach to Polar and Alpine microbiology
Bradley, James A.; Anesio, Alexandre M.; Arndt, Sandra
2016-01-01
Advances in microbial ecology in the cryosphere continue to be driven by empirical approaches including field sampling and laboratory-based analyses. Although mathematical models are commonly used to investigate the physical dynamics of Polar and Alpine regions, they are rarely applied in microbial studies. Yet integrating modelling approaches with ongoing observational and laboratory-based work is ideally suited to Polar and Alpine microbial ecosystems given their harsh environmental and biogeochemical characteristics, simple trophic structures, distinct seasonality, often difficult accessibility, geographical expansiveness and susceptibility to accelerated climate changes. In this opinion paper, we explain how mathematical modelling ideally complements field and laboratory-based analyses. We thus argue that mathematical modelling is a powerful tool for the investigation of these extreme environments and that fully integrated, interdisciplinary model-data approaches could help the Polar and Alpine microbiology community address some of the great research challenges of the 21st century (e.g. assessing global significance and response to climate change). However, a better integration of field and laboratory work with model design and calibration/validation, as well as a stronger focus on quantitative information is required to advance models that can be used to make predictions and upscale processes and fluxes beyond what can be captured by observations alone. PMID:26832206
ISDP salt batch #2 supernate qualification
DOE Office of Scientific and Technical Information (OSTI.GOV)
Peters, T. B.; Nash, C. A.; Fink, S. D.
2009-01-05
This report covers the laboratory testing and analyses of the second Integrated Salt Disposition Project (ISDP) salt supernate samples, performed in support of initial radioactive operations of Actinide Removal Process (ARP) and Modular Caustic-Side Solvent Extraction Unit (MCU). Major goals of this work include characterizing Tank 22H supernate, characterizing Tank 41H supernate, verifying actinide and strontium adsorption with a standard laboratory-scale test using monosodium titanate (MST) and filtration, and checking cesium mass transfer behavior for the MCU solvent performance when contacted with the liquid produced from MST contact. This study also includes characterization of a post-blend Tank 49H sample asmore » part of the Nuclear Criticality Safety Evaluation (NCSE). This work was specified by Task Technical Request and by Task Technical and Quality Assurance Plan (TTQAP). In addition, a sampling plan will be written to guide analytical future work. Safety and environmental aspects of the work were documented in a Hazard Assessment Package.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
FULLER, R.K.
1999-02-24
This document is the final report for tank 241-AN-101 grab samples. Three grab samples 1AN-98-1, 1AN-98-2 and 1AN-98-3 were taken from riser 16 of tank 241-AN-101 on April 8, 1998 and received by the 222-S Laboratory on April 9, 1998. Analyses were performed in accordance with the ''Compatability Grab Sampling and Analysis Plan'' (TSAP) and the ''Data Quality Objectives for Tank Farms Waste Compatability Program'' (DQO). The analytical results are presented in the data summary report. No notification limits were exceeded.
Non-destructive evaluation of laboratory scale hydraulic fracturing using acoustic emission
NASA Astrophysics Data System (ADS)
Hampton, Jesse Clay
The primary objective of this research is to develop techniques to characterize hydraulic fractures and fracturing processes using acoustic emission monitoring based on laboratory scale hydraulic fracturing experiments. Individual microcrack AE source characterization is performed to understand the failure mechanisms associated with small failures along pre-existing discontinuities and grain boundaries. Individual microcrack analysis methods include moment tensor inversion techniques to elucidate the mode of failure, crack slip and crack normal direction vectors, and relative volumetric deformation of an individual microcrack. Differentiation between individual microcrack analysis and AE cloud based techniques is studied in efforts to refine discrete fracture network (DFN) creation and regional damage quantification of densely fractured media. Regional damage estimations from combinations of individual microcrack analyses and AE cloud density plotting are used to investigate the usefulness of weighting cloud based AE analysis techniques with microcrack source data. Two granite types were used in several sample configurations including multi-block systems. Laboratory hydraulic fracturing was performed with sample sizes ranging from 15 x 15 x 25 cm3 to 30 x 30 x 25 cm 3 in both unconfined and true-triaxially confined stress states using different types of materials. Hydraulic fracture testing in rock block systems containing a large natural fracture was investigated in terms of AE response throughout fracture interactions. Investigations of differing scale analyses showed the usefulness of individual microcrack characterization as well as DFN and cloud based techniques. Individual microcrack characterization weighting cloud based techniques correlated well with post-test damage evaluations.
Using remotely-sensed multispectral imagery to build age models for alluvial fan surfaces
NASA Astrophysics Data System (ADS)
D'Arcy, Mitch; Mason, Philippa J.; Roda Boluda, Duna C.; Whittaker, Alexander C.; Lewis, James
2016-04-01
Accurate exposure age models are essential for much geomorphological field research, and generally depend on laboratory analyses such as radiocarbon, cosmogenic nuclide, or luminescence techniques. These approaches continue to revolutionise geomorphology, however they cannot be deployed remotely or in situ in the field. Therefore other methods are still needed for producing preliminary age models, performing relative dating of surfaces, or selecting sampling sites for the laboratory analyses above. With the widespread availability of detailed multispectral imagery, a promising approach is to use remotely-sensed data to discriminate surfaces with different ages. Here, we use new Landsat 8 Operational Land Imager (OLI) multispectral imagery to characterise the reflectance of 35 alluvial fan surfaces in the semi-arid Owens Valley, California. Alluvial fans are useful landforms to date, as they are widely used to study the effects of tectonics, climate and sediment transport processes on source-to-sink sedimentation. Our target fan surfaces have all been mapped in detail in the field, and have well-constrained exposure ages ranging from modern to ~ 125 ka measured using a high density of 10Be cosmogenic nuclide samples. Despite all having similar granitic compositions, the spectral properties of these surfaces vary systematically with their exposure ages. Older surfaces demonstrate a predictable shift in reflectance across the visible and short-wave infrared spectrum. Simple calculations, such as the brightness ratios of different wavelengths, generate sensitive power law relationships with exposure age that depend on post-depositional alteration processes affecting these surfaces. We investigate what these processes might be in this dryland location, and evaluate the potential for using remotely-sensed multispectral imagery for developing surface age models. The ability to remotely sense relative exposure ages has useful implications for preliminary mapping, selecting sampling sites for laboratory-based exposure age techniques, and correlating existing age constraints to un-sampled surfaces.
The potamochemical symphony: new progress in the high-frequency acquisition of stream chemical data
NASA Astrophysics Data System (ADS)
Floury, Paul; Gaillardet, Jérôme; Gayer, Eric; Bouchez, Julien; Tallec, Gaëlle; Ansart, Patrick; Koch, Frédéric; Gorge, Caroline; Blanchouin, Arnaud; Roubaty, Jean-Louis
2017-12-01
Our understanding of hydrological and chemical processes at the catchment scale is limited by our capacity to record the full breadth of the information carried by river chemistry, both in terms of sampling frequency and precision. Here, we present a proof-of-concept study of a lab in the field
called the River Lab
(RL), based on the idea of permanently installing a suite of laboratory instruments in the field next to a river. Housed in a small shed, this set of instruments performs analyses at a frequency of one every 40 min for major dissolved species (Na+, K+, Mg2+, Ca2+, Cl-, SO42-, NO3-) through continuous sampling and filtration of the river water using automated ion chromatographs. The RL was deployed in the Orgeval Critical Zone Observatory, France for over a year of continuous analyses. Results show that the RL is able to capture long-term fine chemical variations with no drift and a precision significantly better than conventionally achieved in the laboratory (up to ±0.5 % for all major species for over a day and up to 1.7 % over 2 months). The RL is able to capture the abrupt changes in dissolved species concentrations during a typical 6-day rain event, as well as daily oscillations during a hydrological low-flow period of summer drought. Using the measured signals as a benchmark, we numerically assess the effects of a lower sampling frequency (typical of conventional field sampling campaigns) and of a lower precision (typically reached in the laboratory) on the hydrochemical signal. The high-resolution, high-precision measurements made possible by the RL open new perspectives for understanding critical zone hydro-bio-geochemical cycles. Finally, the RL also offers a solution for management agencies to monitor water quality in quasi-real time.
Brown, G.E.; McLain, B.J.
1994-01-01
The analysis of natural-water samples for antimony by automated-hydride atomic absorption spectrophotometry is described. Samples are prepared for analysis by addition of potassium and hydrochloric acid followed by an autoclave digestion. After the digestion, potassium iodide and sodium borohydride are added automatically. Antimony hydride (stibine) gas is generated, then swept into a heated quartz cell for determination of antimony by atomic absorption spectrophotometry. Precision and accuracy data are presented. Results obtained on standard reference water samples agree with means established by interlaboratory studies. Spike recoveries for actual samples range from 90 to 114 percent. Replicate analyses of water samples of varying matrices give relative standard deviations from 3 to 10 percent.
Small RNA profiling of low biomass samples: identification and removal of contaminants
Heintz-Buschart, Anna; Yusuf, Dilmurat; Kaysen, Anne; ...
2018-05-14
Here, sequencing-based analyses of low-biomass samples are known to be prone to misinterpretation due to the potential presence of contaminating molecules derived from laboratory reagents and environments. DNA contamination has been previously reported, yet contamination with RNA is usually considered to be very unlikely due to its inherent instability. Small RNAs (sRNAs) identified in tissues and bodily fluids, such as blood plasma, have implications for physiology and pathology, and therefore the potential to act as disease biomarkers. Thus, the possibility for RNA contaminants demands careful evaluation.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Marshall, R.S.
A simple in-line americium assay instrument (AAI) was installed at an americium recovery process area at LASL for use in process development and for providing process control information. The AAI counts 59.5-keV /sup 241/Am gamma rays, using a NaI(T1) detector and Eberline SAM II electronics. It has a useful range of 3 x 10/sup -5/ to 10 g Am/l and does not suffer from plutonium interference. Comparative analyses of samples assayed in the AAI and samples assayed by the LASL Analytical Laboratory show a combined relative standard deviation of 14%.
Small RNA profiling of low biomass samples: identification and removal of contaminants
DOE Office of Scientific and Technical Information (OSTI.GOV)
Heintz-Buschart, Anna; Yusuf, Dilmurat; Kaysen, Anne
Here, sequencing-based analyses of low-biomass samples are known to be prone to misinterpretation due to the potential presence of contaminating molecules derived from laboratory reagents and environments. DNA contamination has been previously reported, yet contamination with RNA is usually considered to be very unlikely due to its inherent instability. Small RNAs (sRNAs) identified in tissues and bodily fluids, such as blood plasma, have implications for physiology and pathology, and therefore the potential to act as disease biomarkers. Thus, the possibility for RNA contaminants demands careful evaluation.
Fernandez-Calle, Pilar; Pelaz, Sandra; Oliver, Paloma; Alcaide, Maria Jose; Gomez-Rioja, Ruben; Buno, Antonio; Iturzaeta, Jose Manuel
2013-01-01
Technological innovation requires the laboratories to ensure that modifications or incorporations of new techniques do not alter the quality of their results. In an ISO 15189 accredited laboratory, flexible scope accreditation facilitates the inclusion of these changes prior to accreditation body evaluation. A strategy to perform the validation of a biochemistry analyzer in an accredited laboratory having a flexible scope is shown. A validation procedure including the evaluation of imprecision and bias of two Dimension Vista analysers 1500 was conducted. Comparability of patient results between one of them and the lately replaced Dimension RxL Max was evaluated. All studies followed the respective Clinical and Laboratory Standards Institute (CLSI) protocols. 30 chemistry assays were studied. Coefficients of variation, percent bias and total error were calculated for all tests and biological variation was considered as acceptance criteria. Quality control material and patient samples were used as test materials. Interchangeability of the results was established by processing forty patients' samples in both devices. 27 of the 30 studied parameters met allowable performance criteria. Sodium, chloride and magnesium did not fulfil acceptance criteria. Evidence of interchangeability of patient results was obtained for all parameters except magnesium, NT-proBNP, cTroponin I and C-reactive protein. A laboratory having a well structured and documented validation procedure can opt to get a flexible scope of accreditation. In addition, performing these activities prior to use on patient samples may evidence technical issues which must be corrected to minimize their impact on patient results.
A Lean Six Sigma approach to the improvement of the selenium analysis method.
Cloete, Bronwyn C; Bester, André
2012-11-02
Reliable results represent the pinnacle assessment of quality of an analytical laboratory, and therefore variability is considered to be a critical quality problem associated with the selenium analysis method executed at Western Cape Provincial Veterinary Laboratory (WCPVL). The elimination and control of variability is undoubtedly of significant importance because of the narrow margin of safety between toxic and deficient doses of the trace element for good animal health. A quality methodology known as Lean Six Sigma was believed to present the most feasible solution for overcoming the adverse effect of variation, through steps towards analytical process improvement. Lean Six Sigma represents a form of scientific method type, which is empirical, inductive and deductive, and systematic, which relies on data, and is fact-based. The Lean Six Sigma methodology comprises five macro-phases, namely Define, Measure, Analyse, Improve and Control (DMAIC). Both qualitative and quantitative laboratory data were collected in terms of these phases. Qualitative data were collected by using quality-tools, namely an Ishikawa diagram, a Pareto chart, Kaizen analysis and a Failure Mode Effect analysis tool. Quantitative laboratory data, based on the analytical chemistry test method, were collected through a controlled experiment. The controlled experiment entailed 13 replicated runs of the selenium test method, whereby 11 samples were repetitively analysed, whilst Certified Reference Material (CRM) was also included in 6 of the runs. Laboratory results obtained from the controlled experiment was analysed by using statistical methods, commonly associated with quality validation of chemistry procedures. Analysis of both sets of data yielded an improved selenium analysis method, believed to provide greater reliability of results, in addition to a greatly reduced cycle time and superior control features. Lean Six Sigma may therefore be regarded as a valuable tool in any laboratory, and represents both a management discipline, and a standardised approach to problem solving and process optimisation.
Kuchkin, A.; Stebelkov, V.; Zhizhin, K.; ...
2018-01-30
Seven laboratories used the results of bulk uranium isotopic analysis by either inductively coupled plasma mass spectrometry (ICP-MS) or thermal ionization mass spectrometry (TIMS) for characterization of the samples in the Nuclear Forensic International Technical Working Group fourth international collaborative material exercise, CMX-4. Comparison of the measured isotopic compositions of uranium in three exercise samples is implemented for identifying any differences or similarities between the samples. The role of isotopic analyses in the context of a real nuclear forensic investigation is discussed. Several limitations in carrying out ICP-MS or TIMS analysis in CMX-4 are noted.
Lusczynski, Norbert J.
1950-01-01
In 1939, a special program for the systematic collection of chloride data in southeastern Nassau County was inaugurated in which three agencies participated. The Nassau County Department of Public Works constructed the sampling wells, the Ground Water Branch of the U.S. Geological Survey began to collect at period intervals water samples which were analysed at the Mount Prospect Laboratory of the New York Department of Water Supply, Gas and Electricity, The Nassau County Department of Public Works and the U.S. Geological Survey have continued financial cooperation for the maintenance of this program up to the present time.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Kuchkin, A.; Stebelkov, V.; Zhizhin, K.
Seven laboratories used the results of bulk uranium isotopic analysis by either inductively coupled plasma mass spectrometry (ICP-MS) or thermal ionization mass spectrometry (TIMS) for characterization of the samples in the Nuclear Forensic International Technical Working Group fourth international collaborative material exercise, CMX-4. Comparison of the measured isotopic compositions of uranium in three exercise samples is implemented for identifying any differences or similarities between the samples. The role of isotopic analyses in the context of a real nuclear forensic investigation is discussed. Several limitations in carrying out ICP-MS or TIMS analysis in CMX-4 are noted.
Trace gas measurements from whole air samples collected over the Antarctic continent
NASA Technical Reports Server (NTRS)
Heidt, L. E.; Vedder, J. F.; Pollock, Walter H.; Henry, Bruce E.; Lueb, Richard A.
1988-01-01
Whole air samples collected aboard the NASA DC-8 and ER-2 aircraft as part of the Airborne Antarctic Ozone Experiment (AAOE) were analyzed in a field laboratory set up at Punta Arenas, Chile, in August and September, 1987. Mixing ratios obtained from gas chromatographic analyses of these samples are presented for N2O, CFCl3, CFCl2, C2F3Cl3, CH3CCl3, CH4, and CO. Variations in the mixing ratios of these gases along the individual flight paths of the aircraft are used as tracers to indicate the history of air masses over and near the Antarctic continent.
Quantifying inter-laboratory variability in stable isotope analysis of ancient skeletal remains.
Pestle, William J; Crowley, Brooke E; Weirauch, Matthew T
2014-01-01
Over the past forty years, stable isotope analysis of bone (and tooth) collagen and hydroxyapatite has become a mainstay of archaeological and paleoanthropological reconstructions of paleodiet and paleoenvironment. Despite this method's frequent use across anthropological subdisciplines (and beyond), the present work represents the first attempt at gauging the effects of inter-laboratory variability engendered by differences in a) sample preparation, and b) analysis (instrumentation, working standards, and data calibration). Replicate analyses of a 14C-dated ancient human bone by twenty-one archaeological and paleoecological stable isotope laboratories revealed significant inter-laboratory isotopic variation for both collagen and carbonate. For bone collagen, we found a sizeable range of 1.8‰ for δ13Ccol and 1.9‰ for δ15Ncol among laboratories, but an interpretatively insignificant average pairwise difference of 0.2‰ and 0.4‰ for δ13Ccol and δ15Ncol respectively. For bone hydroxyapatite the observed range increased to a troublingly large 3.5‰ for δ13Cap and 6.7‰ for δ18Oap, with average pairwise differences of 0.6‰ for δ13Cap and a disquieting 2.0‰ for δ18Oap. In order to assess the effects of preparation versus analysis on isotopic variability among laboratories, a subset of the samples prepared by the participating laboratories were analyzed a second time on the same instrument. Based on this duplicate analysis, it was determined that roughly half of the isotopic variability among laboratories could be attributed to differences in sample preparation, with the other half resulting from differences in analysis (instrumentation, working standards, and data calibration). These findings have serious implications for choices made in the preparation and extraction of target biomolecules, the comparison of results obtained from different laboratories, and the interpretation of small differences in bone collagen and hydroxyapatite isotope values. To address the issues arising from inter-laboratory comparisons, we devise a novel measure we term the Minimum Meaningful Difference (MMD), and demonstrate its application.
Quantifying Inter-Laboratory Variability in Stable Isotope Analysis of Ancient Skeletal Remains
Pestle, William J.; Crowley, Brooke E.; Weirauch, Matthew T.
2014-01-01
Over the past forty years, stable isotope analysis of bone (and tooth) collagen and hydroxyapatite has become a mainstay of archaeological and paleoanthropological reconstructions of paleodiet and paleoenvironment. Despite this method's frequent use across anthropological subdisciplines (and beyond), the present work represents the first attempt at gauging the effects of inter-laboratory variability engendered by differences in a) sample preparation, and b) analysis (instrumentation, working standards, and data calibration). Replicate analyses of a 14C-dated ancient human bone by twenty-one archaeological and paleoecological stable isotope laboratories revealed significant inter-laboratory isotopic variation for both collagen and carbonate. For bone collagen, we found a sizeable range of 1.8‰ for δ13Ccol and 1.9‰ for δ15Ncol among laboratories, but an interpretatively insignificant average pairwise difference of 0.2‰ and 0.4‰ for δ13Ccol and δ15Ncol respectively. For bone hydroxyapatite the observed range increased to a troublingly large 3.5‰ for δ13Cap and 6.7‰ for δ18Oap, with average pairwise differences of 0.6‰ for δ13Cap and a disquieting 2.0‰ for δ18Oap. In order to assess the effects of preparation versus analysis on isotopic variability among laboratories, a subset of the samples prepared by the participating laboratories were analyzed a second time on the same instrument. Based on this duplicate analysis, it was determined that roughly half of the isotopic variability among laboratories could be attributed to differences in sample preparation, with the other half resulting from differences in analysis (instrumentation, working standards, and data calibration). These findings have serious implications for choices made in the preparation and extraction of target biomolecules, the comparison of results obtained from different laboratories, and the interpretation of small differences in bone collagen and hydroxyapatite isotope values. To address the issues arising from inter-laboratory comparisons, we devise a novel measure we term the Minimum Meaningful Difference (MMD), and demonstrate its application. PMID:25061843
NASA Astrophysics Data System (ADS)
Török, Ákos; Czinder, Balázs; Farkas, Orsolya; Görög, Péter; Kopecskó, Katalin; Lógó, János; Rozgonyi-Boissinot, Nikoletta; Vásárhelyi, Balázs
2016-04-01
An emblematic monument the Citadella fortress of Budapest has been studied in details to assess the condition of stone structure. The fortress is a large stone structure of 220 m in length and 60 m in width. The height of the porous limestone walls are in between 12-16 metres. The fortress was completed in 1854 but has been partly rebuilt due to changes in function and war related structural damages. The present paper provides an overview of the lithology, weathering forms and structural condition of the fortress related to a forthcoming restoration-reconstruction project. To assess the condition of stone both on site and laboratory analyses were performed. Lithological varieties were documented. Major identified lithotypes are porous oolitic limestone, less porous bioclastic limestone and fine grained highly porous limestone. To identify wet zones portable moisture meter was applied. Surface strength and weathering grade were also assessed using Schmidt hammer and Duroscop. Decay features were diagnosed and mapped. The most common forms are white weathering crusts, scaling and blistering of crusts as well as granular disintegration. Black weathering crusts were also recognized. Laboratory tests were focused on mechanical properties of stones and on mineralogical and chemical compositional analyses. Small samples of stone were collected and tested by optical microscopy, SEM-EDX, XRD and Thermogravimetric analyses. Laboratory analyses proved that the major salt responsible for the damage of external walls is gypsum, although significant amount of halite and hygroscopic salts were found both on the external walls and in the interior parts of the fortress. During structural analyses displacement of walls, tilting and major amount of cracks were recognized. Loss of material and subsidence also caused problems and at some places unstable wall sections were recognized.
Aase, Audun; Hajdusek, Ondrej; Øines, Øivind; Quarsten, Hanne; Wilhelmsson, Peter; Herstad, Tove K; Kjelland, Vivian; Sima, Radek; Jalovecka, Marie; Lindgren, Per-Eric; Aaberge, Ingeborg S
2016-01-01
A modified microscopy protocol (the LM-method) was used to demonstrate what was interpreted as Borrelia spirochetes and later also Babesia sp., in peripheral blood from patients. The method gained much publicity, but was not validated prior to publication, which became the purpose of this study using appropriate scientific methodology, including a control group. Blood from 21 patients previously interpreted as positive for Borrelia and/or Babesia infection by the LM-method and 41 healthy controls without known history of tick bite were collected, blinded and analysed for these pathogens by microscopy in two laboratories by the LM-method and conventional method, respectively, by PCR methods in five laboratories and by serology in one laboratory. Microscopy by the LM-method identified structures claimed to be Borrelia- and/or Babesia in 66% of the blood samples of the patient group and in 85% in the healthy control group. Microscopy by the conventional method for Babesia only did not identify Babesia in any samples. PCR analysis detected Borrelia DNA in one sample of the patient group and in eight samples of the control group; whereas Babesia DNA was not detected in any of the blood samples using molecular methods. The structures interpreted as Borrelia and Babesia by the LM-method could not be verified by PCR. The method was, thus, falsified. This study underlines the importance of doing proper test validation before new or modified assays are introduced.
Arsenic exposure in drinking water: an unrecognized health threat in Peru
Sima, Laura; Arias, M Helena Jahuira; Mihalic, Jana; Cabrera, Lilia Z; Danz, David; Checkley, William; Gilman, Robert H
2014-01-01
Abstract Objective To assess the extent of arsenic contamination of groundwater and surface water in Peru and, to evaluate the accuracy of the Arsenic Econo-Quick™ (EQ) kit for measuring water arsenic concentrations in the field. Methods Water samples were collected from 151 water sources in 12 districts of Peru, and arsenic concentrations were measured in the laboratory using inductively-coupled plasma mass spectrometry. The EQ field kit was validated by comparing a subset of 139 water samples analysed by laboratory measurements and the EQ kit. Findings In 86% (96/111) of the groundwater samples, arsenic exceeded the 10 µg/l arsenic concentration guideline given by the World Health Organization (WHO) for drinking water. In 56% (62/111) of the samples, it exceeded the Bangladeshi threshold of 50 µg/l; the mean concentration being 54.5 µg/l (range: 0.1–93.1). In the Juliaca and Caracoto districts, in 96% (27/28) of groundwater samples arsenic was above the WHO guideline; and in water samples collected from the section of the Rímac river running through Lima, all had arsenic concentrations exceeding the WHO limit. When validated against laboratory values, the EQ kit correctly identified arsenic contamination relative to the guideline in 95% (106/111) of groundwater and in 68% (19/28) of surface water samples. Conclusion In several districts of Peru, drinking water shows widespread arsenic contamination, exceeding the WHO arsenic guideline. This poses a public health threat requiring further investigation and action. For groundwater samples, the EQ kit performed well relative to the WHO arsenic limit and therefore could provide a vital tool for water arsenic surveillance. PMID:25177071
DOE Office of Scientific and Technical Information (OSTI.GOV)
Gałuszka, Agnieszka, E-mail: Agnieszka.Galuszka@ujk.edu.pl; Migaszewski, Zdzisław M.; Namieśnik, Jacek
The recent rapid progress in technology of field portable instruments has increased their applications in environmental sample analysis. These instruments offer a possibility of cost-effective, non-destructive, real-time, direct, on-site measurements of a wide range of both inorganic and organic analytes in gaseous, liquid and solid samples. Some of them do not require the use of reagents and do not produce any analytical waste. All these features contribute to the greenness of field portable techniques. Several stationary analytical instruments have their portable versions. The most popular ones include: gas chromatographs with different detectors (mass spectrometer (MS), flame ionization detector, photoionization detector),more » ultraviolet–visible and near-infrared spectrophotometers, X-ray fluorescence spectrometers, ion mobility spectrometers, electronic noses and electronic tongues. The use of portable instruments in environmental sample analysis gives a possibility of on-site screening and a subsequent selection of samples for routine laboratory analyses. They are also very useful in situations that require an emergency response and for process monitoring applications. However, quantification of results is still problematic in many cases. The other disadvantages include: higher detection limits and lower sensitivity than these obtained in laboratory conditions, a strong influence of environmental factors on the instrument performance and a high possibility of sample contamination in the field. This paper reviews recent applications of field portable instruments in environmental sample analysis and discusses their analytical capabilities. - Highlights: • Field portable instruments are widely used in environmental sample analysis. • Field portable instruments are indispensable for analysis in emergency response. • Miniaturization of field portable instruments reduces resource consumption. • In situ analysis is in agreement with green analytical chemistry principles. • Performance requirements in field analysis stimulate technological progress.« less
Current developments in forensic interpretation of mixed DNA samples (Review).
Hu, Na; Cong, Bin; Li, Shujin; Ma, Chunling; Fu, Lihong; Zhang, Xiaojing
2014-05-01
A number of recent improvements have provided contemporary forensic investigations with a variety of tools to improve the analysis of mixed DNA samples in criminal investigations, producing notable improvements in the analysis of complex trace samples in cases of sexual assult and homicide. Mixed DNA contains DNA from two or more contributors, compounding DNA analysis by combining DNA from one or more major contributors with small amounts of DNA from potentially numerous minor contributors. These samples are characterized by a high probability of drop-out or drop-in combined with elevated stutter, significantly increasing analysis complexity. At some loci, minor contributor alleles may be completely obscured due to amplification bias or over-amplification, creating the illusion of additional contributors. Thus, estimating the number of contributors and separating contributor genotypes at a given locus is significantly more difficult in mixed DNA samples, requiring the application of specialized protocols that have only recently been widely commercialized and standardized. Over the last decade, the accuracy and repeatability of mixed DNA analyses available to conventional forensic laboratories has greatly advanced in terms of laboratory technology, mathematical models and biostatistical software, generating more accurate, rapid and readily available data for legal proceedings and criminal cases.
Current developments in forensic interpretation of mixed DNA samples (Review)
HU, NA; CONG, BIN; LI, SHUJIN; MA, CHUNLING; FU, LIHONG; ZHANG, XIAOJING
2014-01-01
A number of recent improvements have provided contemporary forensic investigations with a variety of tools to improve the analysis of mixed DNA samples in criminal investigations, producing notable improvements in the analysis of complex trace samples in cases of sexual assult and homicide. Mixed DNA contains DNA from two or more contributors, compounding DNA analysis by combining DNA from one or more major contributors with small amounts of DNA from potentially numerous minor contributors. These samples are characterized by a high probability of drop-out or drop-in combined with elevated stutter, significantly increasing analysis complexity. At some loci, minor contributor alleles may be completely obscured due to amplification bias or over-amplification, creating the illusion of additional contributors. Thus, estimating the number of contributors and separating contributor genotypes at a given locus is significantly more difficult in mixed DNA samples, requiring the application of specialized protocols that have only recently been widely commercialized and standardized. Over the last decade, the accuracy and repeatability of mixed DNA analyses available to conventional forensic laboratories has greatly advanced in terms of laboratory technology, mathematical models and biostatistical software, generating more accurate, rapid and readily available data for legal proceedings and criminal cases. PMID:24748965
NASA Technical Reports Server (NTRS)
Nuth, J. A.; Johnson, N. M.; Ferguson, F. T.; Hilchenbach, M.; Merouane, S.; Paquette, J. A.; Stenzel, O.; Cottin, H.; Fray, N.; Bardyn, A.;
2017-01-01
The COSIMA instrument onboard the Rosetta spacecraft collected and analyzed samples of individual particles from the coma of Comet67P/ Churyumov-Gerasimenko. Initial results of the analysis of several particles have been presented elsewhere while analyses of the organic component of the dust particles has been shown to compare favor ably to laboratory spectra of IOM extracted from the Orguil and Murchison meteorites. Here we will compare the spectra of the same two particles to laboratory spectra of organic grain coatings produced via Surface Mediated Reactions of CO, H2 and N2 on amorphous iron silicate grains.
NASA Technical Reports Server (NTRS)
Yuen, G. U.; Cronin, J. R.; Blair, N. E.; Desmarais, D. J.; Chang, S.
1991-01-01
Recently, in our laboratories, samples of Murchison acetic acid were decarboxylated successfully and the carbon isotopic composition was measured for the methane released by this procedure. These analyses showed significant differences in C-13/C-12 ratios for the methyl and carboxyl carbons of the acetic acid molecule, strongly suggesting that more than one carbon source may be involved in the synthesis of the Murchison organic compounds. On the basis of this finding, laboratory model systems simulating cosmochemical synthesis are being studied, especially those processes capable of involving two or more starting carbon sources.
U.S. Geological Survey Quality-Assurance Project for Sediment Analysis
Gordon, John D.; Newland, Carla
2000-01-01
Introduction Sediment is derived primarily from natural weathering of rock and is an assemblage of individual mineral grains that are then deposited by some physical agent, such as water, wind, ice, or gravity (Fetter, 1988). The U.S. Geological Survey (USGS) samples sediments and collects data on the amount of sediment in selected waterways. The most pressing sediment-related problems are associated with environmental questions, such as the transport and fate of attached pollutants, effects of sediment on aquatic biota and their habitats, and effects on sediment transport from land-use changes. Current (2000) sediment issues require that sediment studies address multiple objectives in water-resources management (Koltun and others, 1997). To support sediment research, the USGS operates laboratories for the analysis of the physical characteristics of sediment. Sediment laboratories producing data for the USGS have two principal functions: (1) the determination of suspended-sediment concentration in samples and (2) the determination of sand/fine separations. The reliability of these determinations and the usefulness of the data are dependent on the accuracy and reliability of the laboratory analyses (Guy, 1969).
Ball, James W.; McCleskey, R. Blaine; Nordstrom, D. Kirk; Holloway, JoAnn M.; Verplanck, Philip L.; Sturtevant, Sabin A.
2002-01-01
Sixty-seven water analyses are reported for samples collected from 44 hot springs and their overflow drainages and two ambient-temperature acid streams in Yellowstone National Park (YNP) during 1990-2000. Thirty-seven analyses are reported for 1999, 18 for June of 2000, and 12 for September of 2000. These water samples were collected and analyzed as part of research investigations in YNP on microbially mediated sulfur oxidation in stream water, arsenic and sulfur redox speciation in hot springs, and chemical changes in overflow drainages that affect major ions, redox species, and trace elements. Most samples were collected from sources in the Norris Geyser Basin. Two ambient-temperature acidic stream systems, Alluvium and Columbine Creeks and their tributaries in Brimstone Basin, were studied in detail. Analyses were performed at or near the sampling site, in an on-site mobile laboratory truck, or later in a USGS laboratory, depending on stability of the constituent and whether or not it could be preserved effectively. Water temperature, specific conductance, pH, Eh, dissolved oxygen (D.O.), and dissolved H2S were determined on-site at the time of sampling. Alkalinity, acidity, and F were determined within a few days of sample collection by titration with acid, titration with base, and ion-selective electrode or ion chromatography (IC), respectively. Concentrations of S2O3 and SxO6 were determined as soon as possible (minutes to hours later) by IC. Concentrations of Br, Cl, NH4, NO2, NO3, SO4, Fe(II), and Fe(total) were determined within a few days of sample collection. Densities were determined later in the USGS laboratory. Concentrations of Li and K were determined by flame atomic absorption spectrometry. Concentrations of Al, As(total), B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe(total), K, Li, Mg, Mn, Na, Ni, Pb, Se, Si, Sr, V, and Zn were determined by inductively-coupled plasma-optical emission spectrometry. Trace concentrations of Cd, Cr, Cu, Pb, and Sb were determined by Zeeman-corrected graphitefurnace atomic-absorption spectrometry. Trace concentrations of As(total) and As(III) were determined by hydride generation atomic-absorption spectrometry using a flow-injection analysis system. Concentrations of Cl, NO3, Br, and SO4 were determined by IC. Concentrations of Fe(II) and Fe(total) were determined by the ferrozine colorimetric method. Concentrations of NO2 were determined by colorimetry using matrix-matched standards. Concentrations of NH4 were determined by IC, with reanalysis by colorimetry where separation of Na and NH4 peaks was poor. Dissolved organic carbon (DOC) concentrations were determined by the wet persulfate oxidation method.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Williams, L.M.; Bartholomay, R.C.; Campbell, L.J.
1998-10-01
The U.S. Geological (USGS) and the Idaho Department of Water Resources, in cooperation with the U.S. Department of Energy, collected and analyzed water samples to monitor the water quality of the Snake River Plain aquifer from the southern boundary of the Idaho National Engineering and Environmental Laboratory to the Hagerman area, Idaho. Concurrently, replicate samples and blank samples were collected and analyzed as part of the quality-assurance/quality-control program. Samples were analyzed from inorganic constituents, gross radioactivity and radionuclides, organic constituents, and stable isotopes. To evaluate the precision of field and laboratory methods, analytical results of the water-quality and replicate samplesmore » were compared statistically for equivalence on the basis of the precision associated with each result. Statistical comparisons of the data indicated that 95 percent of the results of the replicate pairs were equivalent. Blank-sample analytical results indicated th at the inorganic blank water and volatile organic compound blank water from the USGS National Water Quality Laboratory and the distilled water from the Idaho Department of Water Resources were suitable for blanks; blank water from other sources was not. Equipment-blank analytical results were evaluated to determine if a bias had been introduced and possible sources of bias. Most equipment blanks were analyzed for trace elements and volatile organic compounds; chloroform was found in one equipment blank. Two of the equipment blanks were prepared after collection and analyses of the water-quality samples to determine whether contamination had been introduced during the sampling process. Results of one blank indicated that a hose used to divert water away from pumps and electrical equipment had contaminated the samples with some volatile organic compounds. Results of the other equipment blank, from the apparatus used to filter dissolved organic carbon samples, indicated that the filtering apparatus did not affect water-quality samples.« less
Guidelines for Water Quality Laboratory Operations.
1985-07-01
Semiannually sample cell pressure gauge Autoclaves and Check sterilization effectiveness Daily sterilizers (e.g., B. stearothermophilus , color-indicator...container should have been previously cleaned with chromic acid solution as described previously. Treat the container caps similarly. C. Sterilization . For...microbiological analyses, sterilize the container and its stopper/cap by autoclaving at 121*C for 15 min or by dry heat at 180C for 2 hr. Heat-sensitive
2018-02-01
international proficiency testing sponsored by the Organisation for the Prohibition of Chemical Weapons (The Hague, Netherlands). Traditionally...separate batch of standards at each level for a total of six analyses at each calibration level. Concentrations of the tested calibration levels are...and ruthenium at each calibration level. 11 REFERENCES 1. General Requirements for the Competence of Testing and Calibration Laboratories
Robertson, J.F.; Nagle, Douglas D.; Rhodes, Liesl C.
1994-01-01
Investigations to provide initial qualitative delineation of petroleum hydrocarbon contamination at three former underground storage tank locations at Fort Jackson, South Carolina, were made during March 1994. Ground-water and sediment samples were collected using direct-push technology and analyzed on-site with a gas chromatograph, which provided real-time, semi-quantitative data. In addition, ground-water and sediment samples were collected at selected sites for laboratory analyses to provide a confirmation of the on-site data. These analyses provided qualitative data on the lateral distri- bution of petroleum hydrocarbons. Petroleum hydrocarbons were detected by on-site analysis in ground-water samples from nine locations at Site 1062, suggesting the presence of a contaminant plume. Concentrations ranged from less than the minimum detection limit to 4,511 mg/L (micrograms per liter) for benzene, 15,594 mg/L for toluene, 16,501 mg/L for ethylbenzene, and 19,391 mg/L for total xylenes. Concentrations of Total Petroleum Hydrocarbons-Gasoline Range Organics ranged from 323 mg/L to 3,364 mg/L; Total Petroleum Hydrocarbons-Diesel Range Organics were not detected. Three samples from this site were analyzed for benzene, toluene, ethylbenzene, and total xylenes at a laboratory and results showed concentrations ranging from less than the minimum detection limit to 1,070 mg/L for benzene, 7,930 mg/L for toluene, 6,890 mg/L for ethylbenzene, and 1,524 mg/L for total xylenes. Petroleum hydro- carbons were detected by on-site analysis in only one sample at Site 2438. A concentration of 131,000 micrograms per kilogram Total Petroleum Hydrocarbons-Diesel Range Organics was detected in sample number GP-2-4-13.5. Petroleum hydrocarbons were detected by on-site analysis in only one ground-water sample from Site 2444. A concentration of 3,145 mg/L Total Petroleum Hydrocarbons-Gasoline Range Organics was detected at sampling location GP-3-2.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Scheele, R.D.
In 1995, available subsegment samples of wastes taken from the Hanford Site underground radioactive waste storage tanks 241-C-112 (C-112) and 241-C-109 (C-109) were reanalyzed to determine the nickel concentrations in the samples and to determine whether the use of a nickel crucible in the analytical sample preparation biased the reported nickel concentrations reported by Simpson and coworkers and in the original report that this report supplements. The reanalysis strategy to determine nickel was to use a sodium peroxide flux in a zirconium crucible instead of the previously used potassium hydroxide flux in a nickel crucible. This supplemental report provides themore » results of the reanalyses and updates tables from the original report which reflect the new nickel analyses. Nickel is important with respect to management of the potentially reactive ferrocyanide wastes as it is one of the key defining characteristics of the solids that resulted from scavenging radiocesium using ferrocyanides. In Hanford Site wastes, few other processes introduced nickel into the wastes other than radiocobalt scavenging, which was often coupled with the ferrocyanide-scavenging process. Thus the presence of nickel in a waste provides strong evidence that the original waste was or contained ferrocyanide waste at one time. Given the potential import of nickel as a defining characteristic and marker for ferrocyanide wastes, the Pacific Northwest Laboratory`s (PNL) Analytical Chemistry Laboratory (ACL) reanalyzed available samples from tanks C-112 and C-109 using inductively coupled argon plasma/atomic emission spectrometry (ICP/AES) and an alternative sample preparation method which precluded contamination of the analytical samples with nickel.« less
Ptolemy, Adam S; Britz-McKibbin, Philip
2006-02-17
New strategies for integrating sample pretreatment with chemical analyses under a single format is required for rapid, sensitive and enantioselective analyses of low abundance metabolites in complex biological samples. Capillary electrophoresis (CE) offers a unique environment for controlling analyte/reagent band dispersion and electromigration properties using discontinuous electrolyte systems. Recent work in our laboratory towards developing a high-throughput CE platform for low abundance metabolites via on-line sample preconcentration with chemical derivatization (SPCD) is primarily examined in this review, as there have been surprisingly only a few strategies reported in the literature to date. In-capillary sample preconcentration serves to enhance concentration sensitivity via electrokinetic focusing of long sample injection volumes for lower detection limits, whereas chemical derivatization by zone passing is used to expand detectability and selectivity, notably for enantiomeric resolution of metabolites lacking intrinsic chromophores using nanolitre volumes of reagent. Together, on-line SPCD-CE can provide over a 100-fold improvement in concentration sensitivity, shorter total analysis times, reduced sample handling and improved reliability for a variety of amino acid and amino sugar metabolites, which is also amenable to automated high-throughput screening. This review will highlight basic method development and optimization parameters relevant to SPCD-CE, including applications to bacterial metabolite flux and biomarker analyses. Insight into the mechanism of analyte focusing and labeling by SPCD-CE is also discussed, as well as future directions for continued research.
Kulle, A; Krone, N; Holterhus, P M; Schuler, G; Greaves, R F; Juul, A; de Rijke, Y B; Hartmann, M F; Saba, A; Hiort, O; Wudy, S A
2017-05-01
Disorders or differences in sex development (DSD) comprise a heterogeneous group of conditions with an atypical sex development. For optimal diagnosis, highly specialised laboratory analyses are required across European countries. Working group 3 of EU COST (European Cooperation in Science and Technology) Action BM 1303 'DSDnet' 'Harmonisation of Laboratory Assessment' has developed recommendations on laboratory assessment for DSD regarding the use of technologies and analytes to be investigated. This position paper on steroid hormone analysis in diagnosis and treatment of DSD was compiled by a group of specialists in DSD and/or hormonal analysis, either from participating European countries or international partner countries. The topics discussed comprised analytical methods (immunoassay/mass spectrometry-based methods), matrices (urine/serum/saliva) and harmonisation of laboratory tests. The following positions were agreed upon: support of the appropriate use of immunoassay- and mass spectrometry-based methods for diagnosis and monitoring of DSD. Serum/plasma and urine are established matrices for analysis. Laboratories performing analyses for DSD need to operate within a quality framework and actively engage in harmonisation processes so that results and their interpretation are the same irrespective of the laboratory they are performed in. Participation in activities of peer comparison such as sample exchange or when available subscribing to a relevant external quality assurance program should be achieved. The ultimate aim of the guidelines is the implementation of clinical standards for diagnosis and appropriate treatment of DSD to achieve the best outcome for patients, no matter where patients are investigated or managed. © 2017 The authors.
Kwakye-Awuah, Bright; Labik, Linus Kweku; Nkrumah, Isaac; Williams, Craig
2014-03-01
Ammonium ion adsorption by laboratory-synthesized zeolite (linde type A; LTA) was investigated in batch kinetics experiments. Synthesized zeolite LTA was characterized by X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, thermogravimetric analysis, Fourier transform infrared spectroscopy and particle size analysis. Water samples were taken from the Nyam and Tano rivers in Ghana, and 0.8 g of zeolite was added to 100 ml portions of each sample. Portions of the samples were withdrawn every 30 min for 150 min and the concentration of ammonia in each sample was determined. The removal efficiency of zeolite LTA was evaluated by retrieving the zeolite from the water samples and adding to a fresh sample to repeat the process. Equilibrium data were fitted by Langmuir and Freundlich isotherms. Maximum adsorption capacities were 72.99 mg g(-1) for samples from the River Nyam and 72.87 mg g(-1) for samples from the River Tano. The equilibrium kinetic data were analysed using adsorption kinetic models: pseudo-first order and pseudo-second order kinetic models. Linear regression was used to estimate the adsorption and kinetic parameters. The results showed that the adsorption followed pseudo-second order kinetics and suggest that zeolite LTA is a good adsorbent for the removal of nitrogen ammonia from water.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Cecil, L.D.; Knobel, L.L.; Wegner, S.J.
1989-09-01
From 1952 to 1988, about 140 curies of strontium-90 have been discharged in liquid waste to disposal ponds and wells at the INEL (Idaho National Engineering Laboratory). The US Geological Survey routinely samples ground water from the Snake River Plain aquifer and from discontinuous perched-water zones for selected radionuclides, major and minor ions, and chemical and physical characteristics. Water samples for strontium-90 analyses collected in the field are unfiltered and preserved to an approximate 2-percent solution with reagent-grade hydrochloric acid. Water from four wells completed in the Snake River Plain aquifer was sampled as part of the US Geological Survey'smore » quality-assurance program to evaluate the effect of filtration and preservation methods on strontium-90 concentrations in ground water at the INEL. The wells were selected for sampling on the basis of historical concentrations of strontium-90 in ground water. Water from each well was filtered through either a 0.45- or a 0.1-micrometer membrane filter; unfiltered samples also were collected. Two sets of filtered and two sets of unfiltered water samples were collected at each well. One set of water samples was preserved in the field to an approximate 2-percent solution with reagent-grade hydrochloric acid and the other set of samples was not acidified. 13 refs., 2 figs., 6 tabs.« less
Reinhold, Lilli; Reinhardt, Katja
2011-05-01
In this presentation, the mycotoxin levels-as analysed by the analytical centre for mycotoxin surveillance of the state food laboratory (LAVES Braunschweig)-for approximately 500 food samples are reported. The samples were collected in the year 2009 at retail in the German federal state of Lower Saxony. Aflatoxin and ochratoxin A were analysed in dried fruits, spices, cereals and tree nuts. Ochratoxin A was detected in all samples of dried vine fruits, at levels up to 8.1 μg/kg. Aflatoxins and ochratoxin A were also found in nutmeg and curry powder: the maximum regulatory levels for aflatoxins were exceeded in 25% of the nutmeg samples. Nearly all samples of basmati rice contained aflatoxins, although at levels below the maximum regulatory level in all but one sample. Aflatoxins were also detected in about 50% of hazelnut samples, in 20% of the samples the maximum levels was exceeded (maximum 23.2 μg/kg). In contrast, aflatoxin contents in pistachios were surprisingly low. Fusarium toxins were analysed in cereals and cereal products such as flour, bread, and pasta. Deoxynivalenol (DON) was the predominant toxin found in these samples: DON was found in about 40% of the samples, although the maximum levels were not exceeded (max. 418 μg/kg). Fumonisins (FBs) and zearalenone (ZEA) were specifically analysed in maize products (snacks, flour and oil). Most of these samples (80%) were positive, but at levels not exceeding the maximum levels. Maximum levels were 98 μg/kg (ZEA) and 577 μg/kg (sum of FB1 and FB2). Ergot alkaloids (six major alkaloids) were analysed in rye flour, and approximately 50% were positive. The highest concentration of ergot alkaloids was 1,063 μg/kg; the predominant alkaloids were ergotamine and ergocristine. In conclusion, the results indicate that continuous and efficient control measures for mycotoxins in a wide range of critical foods are necessary to ensure compliance with maximum levels. Although the mycotoxin levels in the vast majority of samples were below maximum levels, year-to-year variation and changes in the production of relevant commodities may result in a different picture in the future.
Shahbazian, M. D.; Valsamakis, A.; Boonyaratanakornkit, J.; Cook, L.; Pang, X. L.; Preiksaitis, J. K.; Schönbrunner, E. R.; Caliendo, A. M.
2013-01-01
Commutability of quantitative reference materials has proven important for reliable and accurate results in clinical chemistry. As international reference standards and commercially produced calibration material have become available to address the variability of viral load assays, the degree to which such materials are commutable and the effect of commutability on assay concordance have been questioned. To investigate this, 60 archived clinical plasma samples, which previously tested positive for cytomegalovirus (CMV), were retested by five different laboratories, each using a different quantitative CMV PCR assay. Results from each laboratory were calibrated both with lab-specific quantitative CMV standards (“lab standards”) and with common, commercially available standards (“CMV panel”). Pairwise analyses among laboratories were performed using mean results from each clinical sample, calibrated first with lab standards and then with the CMV panel. Commutability of the CMV panel was determined based on difference plots for each laboratory pair showing plotted values of standards that were within the 95% prediction intervals for the clinical specimens. Commutability was demonstrated for 6 of 10 laboratory pairs using the CMV panel. In half of these pairs, use of the CMV panel improved quantitative agreement compared to use of lab standards. Two of four laboratory pairs for which the CMV panel was noncommutable showed reduced quantitative agreement when that panel was used as a common calibrator. Commutability of calibration material varies across different quantitative PCR methods. Use of a common, commutable quantitative standard can improve agreement across different assays; use of a noncommutable calibrator can reduce agreement among laboratories. PMID:24025907
Quality Assurance Specifications for Planetary Protection Assays
NASA Astrophysics Data System (ADS)
Baker, Amy
As the European Space Agency planetary protection (PP) activities move forward to support the ExoMars and other planetary missions, it will become necessary to increase staffing of labo-ratories that provide analyses for these programs. Standardization of procedures, a comprehen-sive quality assurance program, and unilateral training of personnel will be necessary to ensure that the planetary protection goals and schedules are met. The PP Quality Assurance/Quality Control (QAQC) program is designed to regulate and monitor procedures performed by labora-tory personnel to ensure that all work meets data quality objectives through the assembly and launch process. Because personnel time is at a premium and sampling schedules are often de-pendent on engineering schedules, it is necessary to have flexible staffing to support all sampling requirements. The most productive approach to having a competent and flexible work force is to establish well defined laboratory procedures and training programs that clearly address the needs of the program and the work force. The quality assurance specification for planetary protection assays has to ensure that labora-tories and associated personnel can demonstrate the competence to perform assays according to the applicable standard AD4. Detailed subjects included in the presentation are as follows: • field and laboratory control criteria • data reporting • personnel training requirements and certification • laboratory audit criteria. Based upon RD2 for primary and secondary validation and RD3 for data quality objectives, the QAQC will provide traceable quality assurance safeguards by providing structured laboratory requirements for guidelines and oversight including training and technical updates, standardized documentation, standardized QA/QC checks, data review and data archiving.
Boggess, Andrew; Crump, Stephen; Gregory, Clint; ...
2017-12-06
Here, unique hazards are presented in the analysis of radiologically contaminated samples. Strenuous safety and security precautions must be in place to protect the analyst, laboratory, and instrumentation used to perform analyses. A validated method has been optimized for the analysis of select nitroaromatic explosives and degradative products using gas chromatography/mass spectrometry via sonication extraction of radiologically contaminated soils, for samples requiring ISO/IEC 17025 laboratory conformance. Target analytes included 2-nitrotoluene, 4-nitrotoluene, 2,6-dinitrotoluene, and 2,4,6-trinitrotoluene, as well as the degradative product 4-amino-2,6-dinitrotoluene. Analytes were extracted from soil in methylene chloride by sonication. Administrative and engineering controls, as well as instrument automationmore » and quality control measures, were utilized to minimize potential human exposure to radiation at all times and at all stages of analysis, from receiving through disposition. Though thermal instability increased uncertainties of these selected compounds, a mean lower quantitative limit of 2.37 µg/mL and mean accuracy of 2.3% relative error and 3.1% relative standard deviation were achieved. Quadratic regression was found to be optimal for calibration of all analytes, with compounds of lower hydrophobicity displaying greater parabolic curve. Blind proficiency testing (PT) of spiked soil samples demonstrated a mean relative error of 9.8%. Matrix spiked analyses of PT samples demonstrated that 99% recovery of target analytes was achieved. To the knowledge of the authors, this represents the first safe, accurate, and reproducible quantitative method for nitroaromatic explosives in soil for specific use on radiologically contaminated samples within the constraints of a nuclear analytical lab.« less
The Geochemical Databases GEOROC and GeoReM - What's New?
NASA Astrophysics Data System (ADS)
Sarbas, B.; Jochum, K. P.; Nohl, U.; Weis, U.
2017-12-01
The geochemical databases GEOROC (http: georoc.mpch-mainz.gwdg.de) and GeoReM (http: georem.mpch-mainz.gwdg.de) are maintained by the Max Planck Institute for Chemistry in Mainz, Germany. Both online databases became crucial tools for geoscientists from different research areas. They are regularly upgraded by new tools and new data from recent publications obtained from a wide range of international journals. GEOROC is a collection of published analyses of volcanic rocks and mantle xenoliths. Since recently, data for plutonic rocks are added. The analyses include major and trace element concentrations, radiogenic and non-radiogenic isotope ratios as well as analytical ages for whole rocks, glasses, minerals and inclusions. Samples come from eleven geological settings and span the whole geological age scale from Archean to Recent. Metadata include, among others, geographic location, rock class and rock type, geological age, degree of alteration, analytical method, laboratory, and reference. The GEOROC web page allows selection of samples by geological setting, geography, chemical criteria, rock or sample name, and bibliographic criteria. In addition, it provides a large number of precompiled files for individual locations, minerals and rock classes. GeoReM is a database collecting information about reference materials of geological and environmental interest, such as rock powders, synthetic and natural glasses as well as mineral, isotopic, biological, river water and seawater reference materials. It contains published data and compilation values (major and trace element concentrations and mass fractions, radiogenic and stable isotope ratios). Metadata comprise, among others, uncertainty, analytical method and laboratory. Reference materials are important for calibration, method validation, quality control and to establish metrological traceability. GeoReM offers six different search strategies: samples or materials (published values), samples (GeoReM preferred values), chemical criteria, chemical criteria based on bibliography, bibliography, as well as methods and institutions.
Cecil, L. DeWayne; Hall, L. Flint; Green, Jaromy R.
2003-01-01
Background concentrations of iodine-129 (129I, half-life = 15.7 million years) resulting from natural production in the earth?s atmosphere, in situ production in the earth by spontaneous fission of uranium-238(238U), and fallout from nuclear weapons tests conducted in the 1950s and 1960s were reevaluated on the basis of 52 analyses of ground- and surface-water samples collected from the eastern Snake River Plain in southeastern Idaho. The background concentration estimated using the results of a subset of 30 ground-water samples analyzed in this reevaluation is 5.4 attocuries per liter (aCi/L; 1 aCi = 10-18 curies) and the 95-percent nonparametric confidence interval is 5.2 to 10.0 aCi/L. In a previous study, a background 129I concentration was estimated on the basis of analyses of water samples from 16 sites on or tributary to the eastern Snake River Plain. At the 99-percent confidence level, background concentrations of 129I in that study were less than or equal to 8.2 aCi/L. During 1993?94, 34 water samples from 32 additional sites were analyzed for 129I to better establish the background concentrations in surface and ground water from the eastern Snake River Plain that is presumed to be unaffected by wastedisposal practices at the Idaho National Engineering and Environmental Laboratory (INEEL). Surface water contained larger 129I concentrations than water from springs and wells contained. Because surface water is more likely to be affected by anthropogenic fallout and evapotranspiration, background 129I concentrations were estimated in the current research using the laboratory results of ground-water samples that were assumed to be unaffected by INEEL disposal practices.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Boggess, Andrew; Crump, Stephen; Gregory, Clint
Here, unique hazards are presented in the analysis of radiologically contaminated samples. Strenuous safety and security precautions must be in place to protect the analyst, laboratory, and instrumentation used to perform analyses. A validated method has been optimized for the analysis of select nitroaromatic explosives and degradative products using gas chromatography/mass spectrometry via sonication extraction of radiologically contaminated soils, for samples requiring ISO/IEC 17025 laboratory conformance. Target analytes included 2-nitrotoluene, 4-nitrotoluene, 2,6-dinitrotoluene, and 2,4,6-trinitrotoluene, as well as the degradative product 4-amino-2,6-dinitrotoluene. Analytes were extracted from soil in methylene chloride by sonication. Administrative and engineering controls, as well as instrument automationmore » and quality control measures, were utilized to minimize potential human exposure to radiation at all times and at all stages of analysis, from receiving through disposition. Though thermal instability increased uncertainties of these selected compounds, a mean lower quantitative limit of 2.37 µg/mL and mean accuracy of 2.3% relative error and 3.1% relative standard deviation were achieved. Quadratic regression was found to be optimal for calibration of all analytes, with compounds of lower hydrophobicity displaying greater parabolic curve. Blind proficiency testing (PT) of spiked soil samples demonstrated a mean relative error of 9.8%. Matrix spiked analyses of PT samples demonstrated that 99% recovery of target analytes was achieved. To the knowledge of the authors, this represents the first safe, accurate, and reproducible quantitative method for nitroaromatic explosives in soil for specific use on radiologically contaminated samples within the constraints of a nuclear analytical lab.« less
Plant, Jon D; Neradelik, Moni B; Polissar, Nayak L; Fadok, Valerie A; Scott, Brian A
2014-02-01
Canine allergen-specific IgE assays in the USA are not subjected to an independent laboratory reliability monitoring programme. The aim of this study was to evaluate the agreement of diagnostic results and treatment recommendations of four serum IgE assays commercially available in the USA. Replicate serum samples from 10 atopic dogs were submitted to each of four laboratories for allergen-specific IgE assays (ACTT(®) , VARL Liquid Gold, ALLERCEPT(®) and Greer(®) Aller-g-complete(®) ). The interlaboratory agreement of standard, regional panels and ensuing treatment recommendations were analysed with the kappa statistic (κ) to account for agreement that might occur merely by chance. Six comparisons of pairs of laboratories and overall agreement among laboratories were analysed for ungrouped allergens (as tested) and also with allergens grouped according to reported cross-reactivity and taxonomy. The overall chance-corrected agreement of the positive/negative test results for ungrouped and grouped allergens was slight (κ = 0.14 and 0.13, respectively). Subset analysis of the laboratory pair with the highest level of diagnostic agreement (κ = 0.36) found slight agreement (κ = 0.13) for ungrouped plants and fungi, but substantial agreement (κ = 0.71) for ungrouped mites. The overall agreement of the treatment recommendations was slight (κ = 0.11). Altogether, 85.1% of ungrouped allergen treatment recommendations were unique to one laboratory or another. Our study indicated that the choice of IgE assay may have a major influence on the positive/negative results and ensuing treatment recommendations. © 2014 The Authors. Veterinary Dermatology published by John Wiley & Sons Ltd on behalf of the ESVD and the ACVD.
Comparison of urine analysis using manual and sedimentation methods.
Kurup, R; Leich, M
2012-06-01
Microscopic examination of urine sediment is an essential part in the evaluation of renal and urinary tract diseases. Traditionally, urine sediments are assessed by microscopic examination of centrifuged urine. However the current method used by the Georgetown Public Hospital Corporation Medical Laboratory involves uncentrifuged urine. To encourage high level of care, the results provided to the physician must be accurate and reliable for proper diagnosis. The aim of this study is to determine whether the centrifuge method is more clinically significant than the uncentrifuged method. In this study, a comparison between the results obtained from centrifuged and uncentrifuged methods were performed. A total of 167 urine samples were randomly collected and analysed during the period April-May 2010 at the Medical Laboratory, Georgetown Public Hospital Corporation. The urine samples were first analysed microscopically by the uncentrifuged, and then by the centrifuged method. The results obtained from both methods were recorded in a log book. These results were then entered into a database created in Microsoft Excel, and analysed for differences and similarities using this application. Analysis was further done in SPSS software to compare the results using Pearson ' correlation. When compared using Pearson's correlation coefficient analysis, both methods showed a good correlation between urinary sediments with the exception of white bloods cells. The centrifuged method had a slightly higher identification rate for all of the parameters. There is substantial agreement between the centrifuged and uncentrifuged methods. However the uncentrifuged method provides for a rapid turnaround time.
Søndergaard, Jens; Asmund, Gert; Larsen, Martin M.
2015-01-01
Trace element determination in seawater is analytically challenging due to the typically very low concentrations of the trace elements and the potential interference of the salt matrix. A common way to address the challenge is to pre-concentrate the trace elements on a chelating resin, then rinse the matrix elements from the resin and subsequently elute and detect the trace elements using inductively coupled plasma mass spectrometry (ICP-MS). This technique typically involves time-consuming pre-treatment of the samples for ‘off-line’ analyses or complicated sample introduction systems involving several pumps and valves for ‘on-line’ analyses. As an alternative, the following method offers a simple method for ‘on-line’ analyses of seawater by ICP-MS. As opposed to previous methods, excess seawater was pumped through the nebulizer of the ICP-MS during the pre-concentration step but the gas flow was adjusted so that the seawater was pumped out as waste without being sprayed into the instrument. Advantages of the method include: • Simple and convenient analyses of seawater requiring no changes to the ‘standard’ sample introduction system except from a resin-filled micro-column connected to the sample tube. The ‘standard’ sample introduction system refers to that used for routine digest-solution analyses of biota and sediment by ICP-MS using only one peristaltic pump; and • Accurate determination of the elements V, Mn, Co, Ni, Cu, Zn, Cd and Pb in a range of different seawater matrices verified by participation in 6 successive rounds of the international laboratory intercalibration program QUASIMEME. PMID:26258050
Ball, James W.; Nordstrom, D. Kirk; McCleskey, R. Blaine; Schoonen, Martin A.A.; Xu, Yong
2001-01-01
Fifty-eight water analyses are reported for samples collected from 19 hot springs and their overflow drainages and one ambient-temperature acid stream in Yellowstone National Park (YNP) during 1996-98. These water samples were collected and analyzed as part of research investigations on microbially mediated sulfur oxidation in stream waters and sulfur redox speciation in hot springs in YNP and chemical changes in overflow drainages that affect major ions, redox species, and trace elements. The research on sulfur redox speciation in hot springs is a collaboration with the State University of New York at Stony Brook, Northern Arizona University, and the U.S. Geological Survey (USGS). One ambient-temperature acidic stream system, Alluvium Creek and its tributaries in Brimstone Basin, was studied in detail. Analyses were performed adjacent to the sampling site, in an on-site mobile laboratory truck, or later in a USGS laboratory, depending on stability and preservability of the constituent. Water temperature, specific conductance, pH, Eh, dissolved oxygen (D.O.), and dissolved H2S were determined on-site at the time of sampling. Alkalinity and F were determined within a few days of sample collection by titration and by ion-selective electrode, respectively. Concentrations of S2O3 and SxO6 were determined as soon as possible (minutes to hours later) by ion chromatography (IC). Concentrations of Cl, SO4, and Br were determined by IC within a few days of sample collection. Concentrations of Fe(II) and Fe(total) were determined by ultraviolet/visible spectrophotometry within a few days of sample collection. Densities were determined later in the USGS laboratory. Concentrations of Li, Na, and K were determined by flame atomic absorption (Li) and emission (Na, K) spectrometry. Concentrations of Al, As(total), B, Ba, Be, Ca, Cd, Co, Cr, Cu, Fe(total), Mg, Mn, Ni, Pb, Si, Sr, V, and Zn were determined by inductively-coupled plasma optical emission spectrometry. Trace concentrations of Cd, Se, As(total), Ni, and Pb were determined by Zeeman-corrected graphite-furnace atomic-absorption spectrometry. Trace concentrations of As(total) and As(III) were determined by hydride generation using a flow-injection analysis system.
Granitto, Matthew; Bailey, Elizabeth A.; Schmidt, Jeanine M.; Shew, Nora B.; Gamble, Bruce M.; Labay, Keith A.
2011-01-01
The Alaska Geochemical Database (AGDB) was created and designed to compile and integrate geochemical data from Alaska in order to facilitate geologic mapping, petrologic studies, mineral resource assessments, definition of geochemical baseline values and statistics, environmental impact assessments, and studies in medical geology. This Microsoft Access database serves as a data archive in support of present and future Alaskan geologic and geochemical projects, and contains data tables describing historical and new quantitative and qualitative geochemical analyses. The analytical results were determined by 85 laboratory and field analytical methods on 264,095 rock, sediment, soil, mineral and heavy-mineral concentrate samples. Most samples were collected by U.S. Geological Survey (USGS) personnel and analyzed in USGS laboratories or, under contracts, in commercial analytical laboratories. These data represent analyses of samples collected as part of various USGS programs and projects from 1962 to 2009. In addition, mineralogical data from 18,138 nonmagnetic heavy mineral concentrate samples are included in this database. The AGDB includes historical geochemical data originally archived in the USGS Rock Analysis Storage System (RASS) database, used from the mid-1960s through the late 1980s and the USGS PLUTO database used from the mid-1970s through the mid-1990s. All of these data are currently maintained in the Oracle-based National Geochemical Database (NGDB). Retrievals from the NGDB were used to generate most of the AGDB data set. These data were checked for accuracy regarding sample location, sample media type, and analytical methods used. This arduous process of reviewing, verifying and, where necessary, editing all USGS geochemical data resulted in a significantly improved Alaska geochemical dataset. USGS data that were not previously in the NGDB because the data predate the earliest USGS geochemical databases, or were once excluded for programmatic reasons, are included here in the AGDB and will be added to the NGDB. The AGDB data provided here are the most accurate and complete to date, and should be useful for a wide variety of geochemical studies. The AGDB data provided in the linked database may be updated or changed periodically. The data on the DVD and in the data downloads provided with this report are current as of date of publication.
Influence of relative humidity on VOC concentrations in indoor air.
Markowicz, Pawel; Larsson, Lennart
2015-04-01
Volatile organic compounds (VOCs) may be emitted from surfaces indoors leading to compromised air quality. This study scrutinized the influence of relative humidity (RH) on VOC concentrations in a building that had been subjected to water damage. While air samplings in a damp room at low RH (21-22%) only revealed minor amounts of 2-ethylhexanol (3 μg/m(3)) and 2,2,4-trimethyl-1,3-pentanediol diisobutyrate (TXIB, 8 μg/m(3)), measurements performed after a rapid increase of RH (to 58-75%) revealed an increase in VOC concentrations which was 3-fold for 2-ethylhexanol and 2-fold for TXIB. Similar VOC emission patterns were found in laboratory analyses of moisture-affected and laboratory-contaminated building materials. This study demonstrates the importance of monitoring RH when sampling indoor air for VOCs in order to avoid misleading conclusions from the analytical results.
Inter-laboratory comparisons of short-lived gamma-emitting radionuclides in nuclear reactor water.
Klemola, S K
2008-01-01
Inter-laboratory comparisons of gamma-emitting nuclides in nuclear power plant coolant water have been carried out in Finland since 1994. The reactor water samples are taken and prepared by one of the two nuclear power plants and delivered to the participants. Since all the participants get their sample within just a few hours it has been possible to analyse and compare results of nuclides with half-lives shorter than 1h. The total number of short-lived nuclides is 26. All the main nuclides are regularly identified and the activities have been obtained with reasonable accuracy throughout the years. The overall deviation of the results has decreased in 13 years. The effects of true coincidence summing and discrepancies in nuclear data have been identified as potential sources of remaining discrepancies. All the participants have found this type of comparison very useful.
Numerical simulation of mechanical properties tests of tungsten mud waste geopolymer
NASA Astrophysics Data System (ADS)
Paszek, Natalia; Krystek, Małgorzata
2018-03-01
Geopolymers are believed to become in the future an environmental friendly alternative for the concrete. The low CO2 emission during the production process and the possibility of ecological management of the industrial wastes are mentioned as main advantages of geopolymers. The main drawback, causing problems with application of geopolymers as a building material is the lack of the theoretical material model. Indicated problem is being solved now by the group of scientists from the Silesian University of Technology. The series of laboratory tests are carried out within the European research project REMINE. The paper introduces the numerical analyses of tungsten mud waste geopolymer samples which have been performed in the Atena software on the basis of the laboratory tests. Numerical models of bended and compressed samples of different shapes are presented in the paper. The results obtained in Atena software were compared with results obtained in Abaqus and Mafem3D software.
NASA Astrophysics Data System (ADS)
Brack, A.; Commeyras, A.; Derenne, S.; Despois, D.; Dhamelincourt, P.; Dobrijevic, M.; Engrand, C.; Geffard, M.; Grenier-Loustalot, M. F.; Largeau, C.
2000-07-01
On Earth, the molecules which participated in the emergence of life about 4 Ga ago have been erased by plate tectonics, the permanent presence of running water, unshielded solar ultraviolet radiation and by oxygen produced by life. Since the environment of the early Mars about 3.5-4 Ga ago was probably very close to that of the early Earth, life might have emerged on Mars as well and might give us some insight into the prebiotic chemistry that took place on Earth about 4 Ga ago. Furthermore, there is a possibility that life still exists on Mars, protected from the harsh environment in some specific locales. In order to search for life on Mars, one should look for potential biogenic markers such as organic matter and inorganic signatures (microfossils, biominerals, biogenic etching, isotopic fingerprints...) which have different degrees of resistance to the Martian environment. As biomarkers could be organic or inorganic in nature, complete organic and mineral analyses should therefore be conducted in parallel on the same sets of samples, going from the least destructive to the most destructive technique of micro-analysis. Furthermore, in situ analyses should be complemented by high precision and high sensitivity laboratory measurements of returned Martian samples. Due to the very oxidized Martian environment, organic molecules should be searched for in protected sites, either surface boulders or near sub-surface, in layers deep enough for avoiding the oxidizing effect of the atmosphere. Molecules that should be looked for include low and high molecular weight organics (like alkanoic acids, peroxiacids, PAHs and amino acids, respectively), and macromolecular com-pounds like kerogens or kerogen-like materials. Previous in situ analyses were performed using pyrolysis systems which allow to detect organic compounds but do not always permit the identification of individual molecules. New possible analytical solutions could include gas chromatography-based techniques coupled with a mass spectrometer using multi GC columns systems, including columns able to separate enantiomers, chemical derivatization cells (using new derivatization schemes in particular for amino acid analysis), high performance liquid chromatography and supercritical fluid chromatography.
Kruse, Niels; Persson, Staffan; Alcolea, Daniel; Bahl, Justyna M C; Baldeiras, Ines; Capello, Elisabetta; Chiasserini, Davide; Bocchio Chiavetto, Luisella; Emersic, Andreja; Engelborghs, Sebastiaan; Eren, Erden; Fladby, Tormod; Frisoni, Giovanni; García-Ayllón, María-Salud; Genc, Sermin; Gkatzima, Olymbia; Heegaard, Niels H H; Janeiro, André M; Kováčech, Branislav; Kuiperij, H Bea; Leitão, Maria J; Lleó, Alberto; Martins, Madalena; Matos, Mafalda; Mollergard, Hanne M; Nobili, Flavio; Öhrfelt, Annika; Parnetti, Lucilla; de Oliveira, Catarina Resende; Rot, Uros; Sáez-Valero, Javier; Struyfs, Hanne; Tanassi, Julia T; Taylor, Peggy; Tsolaki, Magda; Vanmechelen, Eugeen; Verbeek, Marcel M; Zilka, Norbert; Blennow, Kaj; Zetterberg, Henrik; Mollenhauer, Brit
2015-09-01
Decreased levels of alpha-synuclein (aSyn) in cerebrospinal fluid (CSF) in Parkinson's disease and related synucleinopathies have been reported, however, not consistently in all cross-sectional studies. To test the performance of one recently released human-specific enzyme-linked immunosorbent assay (ELISA) for the quantification of aSyn in CSF, we carried out a round robin trial with 18 participating laboratories trained in CSF ELISA analyses within the BIOMARKAPD project in the EU Joint Program - Neurodegenerative Disease Research. CSF samples (homogeneous aliquots from pools) and ELISA kits (one lot) were provided centrally and data reported back to one laboratory for data analysis. Our study showed that although factors such as preanalytical sample handling and lot-to-lot variability were minimized by our study design, we identified high variation in absolute values of CSF aSyn even when the same samples and same lots of assays were applied. We further demonstrate that although absolute concentrations differ between laboratories the quantitative results are comparable. With further standardization this assay may become an attractive tool for comparing aSyn measurements in diverse settings. Recommendations for further validation experiments and improvement of the interlaboratory results obtained are given. Copyright © 2015 Elsevier Inc. All rights reserved.
Comprehensive Census of Bacteria in Clean Rooms by Using DNA Microarray and Cloning Methods▿ †
La Duc, Myron T.; Osman, Shariff; Vaishampayan, Parag; Piceno, Yvette; Andersen, Gary; Spry, J. A.; Venkateswaran, Kasthuri
2009-01-01
A census of clean room surface-associated bacterial populations was derived from the results of both the cloning and sequencing of 16S rRNA genes and DNA microarray (PhyloChip) analyses. Samples from the Lockheed Martin Aeronautics Multiple Testing Facility (LMA-MTF), the Kennedy Space Center Payload Hazard and Servicing Facility (KSC-PHSF), and the Jet Propulsion Laboratory Spacecraft Assembly Facility (JPL-SAF) clean rooms were collected during the various assembly phases of the Phoenix and Mars Science Laboratory (MSL) spacecraft. Clone library-derived analyses detected a larger bacterial diversity prior to the arrival of spacecraft hardware in these clean room facilities. PhyloChip results were in agreement with this trend but also unveiled the presence of anywhere from 9- to 70-fold more bacterial taxa than cloning approaches. Among the facilities sampled, the JPL-SAF (MSL mission) housed a significantly less diverse bacterial population than either the LMA-MTF or KSC-PHSF (Phoenix mission). Bacterial taxa known to thrive in arid conditions were frequently detected in MSL-associated JPL-SAF samples, whereas proteobacterial lineages dominated Phoenix-associated KSC-PHSF samples. Comprehensive bacterial censuses, such as that reported here, will help space-faring nations preemptively identify contaminant biomatter that may compromise extraterrestrial life detection experiments. The robust nature and high sensitivity of DNA microarray technologies should prove beneficial to a wide range of scientific, electronic, homeland security, medical, and pharmaceutical applications and to any other ventures with a vested interest in monitoring and controlling contamination in exceptionally clean environments. PMID:19700540
Comprehensive census of bacteria in clean rooms by using DNA microarray and cloning methods.
La Duc, Myron T; Osman, Shariff; Vaishampayan, Parag; Piceno, Yvette; Andersen, Gary; Spry, J A; Venkateswaran, Kasthuri
2009-10-01
A census of clean room surface-associated bacterial populations was derived from the results of both the cloning and sequencing of 16S rRNA genes and DNA microarray (PhyloChip) analyses. Samples from the Lockheed Martin Aeronautics Multiple Testing Facility (LMA-MTF), the Kennedy Space Center Payload Hazard and Servicing Facility (KSC-PHSF), and the Jet Propulsion Laboratory Spacecraft Assembly Facility (JPL-SAF) clean rooms were collected during the various assembly phases of the Phoenix and Mars Science Laboratory (MSL) spacecraft. Clone library-derived analyses detected a larger bacterial diversity prior to the arrival of spacecraft hardware in these clean room facilities. PhyloChip results were in agreement with this trend but also unveiled the presence of anywhere from 9- to 70-fold more bacterial taxa than cloning approaches. Among the facilities sampled, the JPL-SAF (MSL mission) housed a significantly less diverse bacterial population than either the LMA-MTF or KSC-PHSF (Phoenix mission). Bacterial taxa known to thrive in arid conditions were frequently detected in MSL-associated JPL-SAF samples, whereas proteobacterial lineages dominated Phoenix-associated KSC-PHSF samples. Comprehensive bacterial censuses, such as that reported here, will help space-faring nations preemptively identify contaminant biomatter that may compromise extraterrestrial life detection experiments. The robust nature and high sensitivity of DNA microarray technologies should prove beneficial to a wide range of scientific, electronic, homeland security, medical, and pharmaceutical applications and to any other ventures with a vested interest in monitoring and controlling contamination in exceptionally clean environments.
Isotope hydrology of the Chalk River Laboratories site, Ontario, Canada
Peterman, Zell; Neymark, Leonid; King-Sharp, K.J.; Gascoyne, Mel
2016-01-01
This paper presents results of hydrochemical and isotopic analyses of groundwater (fracture water) and porewater, and physical property and water content measurements of bedrock core at the Chalk River Laboratories (CRL) site in Ontario. Density and water contents were determined and water-loss porosity values were calculated for core samples. Average and standard deviations of density and water-loss porosity of 50 core samples from four boreholes are 2.73 ± 12 g/cc and 1.32 ± 1.24 percent. Respective median values are 2.68 and 0.83 indicating a positive skewness in the distributions. Groundwater samples from four deep boreholes were analyzed for strontium (87Sr/86Sr) and uranium (234U/238U) isotope ratios. Oxygen and hydrogen isotope analyses and selected solute concentrations determined by CRL are included for comparison. Groundwater from borehole CRG-1 in a zone between approximately +60 and −240 m elevation is relatively depleted in δ18O and δ2H perhaps reflecting a slug of water recharged during colder climatic conditions. Porewater was extracted from core samples by centrifugation and analyzed for major dissolved ions and for strontium and uranium isotopes. On average, the extracted water contains 15 times larger concentration of solutes than the groundwater. 234U/238U and correlation of 87Sr/86Sr with Rb/Sr values indicate that the porewater may be substantially older than the groundwater. Results of this study show that the Precambrian gneisses at Chalk River are similar in physical properties and hydrochemical aspects to crystalline rocks being considered for the construction of nuclear waste repositories in other regions.
Ball, James W.; McCleskey, R. Blaine; Nordstrom, D. Kirk; Holloway, JoAnn M.
2008-01-01
Water analyses are reported for 157 samples collected from numerous hot springs, their overflow drainages, and Lemonade Creek in Yellowstone National Park (YNP) during 2003-2005. Water samples were collected and analyzed for major and trace constituents from ten areas of YNP including Terrace and Beryl Springs in the Gibbon Canyon area, Norris Geyser Basin, the West Nymph Creek thermal area, the area near Nymph Lake, Hazle Lake, and Frying Pan Spring, Lower Geyser Basin, Washburn Hot Springs, Mammoth Hot Springs, Potts Hot Spring Basin, the Sulphur Caldron area, and Lemonade Creek near the Solfatara Trail. These water samples were collected and analyzed as part of research investigations in YNP on arsenic, antimony, and sulfur redox distribution in hot springs and overflow drainages, and the occurrence and distribution of dissolved mercury. Most samples were analyzed for major cations and anions, trace metals, redox species of antimony, arsenic, iron, nitrogen, and sulfur, and isotopes of hydrogen and oxygen. Analyses were performed at the sampling site, in an on-site mobile laboratory vehicle, or later in a U.S. Geological Survey laboratory, depending on stability of the constituent and whether it could be preserved effectively. Water samples were filtered and preserved onsite. Water temperature, specific conductance, pH, Eh (redox potential relative to the Standard Hydrogen Electrode), and dissolved hydrogen sulfide were measured onsite at the time of sampling. Acidity was determined by titration, usually within a few days of sample collection. Alkalinity was determined by titration within 1 to 2 weeks of sample collection. Concentrations of thiosulfate and polythionate were determined as soon as possible (generally minutes to hours after sample collection) by ion chromatography in an on-site mobile laboratory vehicle. Total dissolved-iron and ferrous-iron concentrations often were measured onsite in the mobile laboratory vehicle. Concentrations of dissolved aluminum, arsenic, boron, barium, beryllium, calcium, cadmium, cobalt, chromium, copper, iron, potassium, lithium, magnesium, manganese, molybdenum, sodium, nickel, lead, selenium, silica, strontium, vanadium, and zinc were determined by inductively-coupled plasma-optical emission spectrometry. Trace concentrations of dissolved antimony, cadmium, cobalt, chromium, copper, lead, and selenium were determined by Zeeman-corrected graphite-furnace atomic-absorption spectrometry. Dissolved concentrations of total arsenic, arsenite, total antimony, and antimonite were determined by hydride-generation atomic-absorption spectrometry using a flow-injection analysis system. Dissolved concentrations of total mercury and methyl mercury were determined by cold-vapor atomic-fluorescence spectrometry. Concentrations of dissolved chloride, fluoride, nitrate, bromide, and sulfate were determined by ion chromatography. Concentrations of dissolved ferrous and total iron were determined by the FerroZine colorimetric method. Concentrations of dissolved nitrite were determined by colorimetry or chemiluminescence. Concentrations of dissolved ammonium were determined by ion chromatography, with reanalysis by colorimetry when separation of sodium and ammonia peaks was poor. Dissolved organic carbon concentrations were determined by the wet persulfate oxidation method. Hydrogen and oxygen isotope ratios were determined using the hydrogen and CO2 equilibration techniques, respectively.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Zhou, Jianying; Dann, Geoffrey P.; Shi, Tujin
2012-03-10
Sodium dodecyl sulfate (SDS) is one of the most popular laboratory reagents used for highly efficient biological sample extraction; however, SDS presents a significant challenge to LC-MS-based proteomic analyses due to its severe interference with reversed-phase LC separations and electrospray ionization interfaces. This study reports a simple SDS-assisted proteomic sample preparation method facilitated by a novel peptide-level SDS removal protocol. After SDS-assisted protein extraction and digestion, SDS was effectively (>99.9%) removed from peptides through ion substitution-mediated DS- precipitation with potassium chloride (KCl) followed by {approx}10 min centrifugation. Excellent peptide recovery (>95%) was observed for less than 20 {mu}g of peptides.more » Further experiments demonstrated the compatibility of this protocol with LC-MS/MS analyses. The resulting proteome coverage from this SDS-assisted protocol was comparable to or better than those obtained from other standard proteomic preparation methods in both mammalian tissues and bacterial samples. These results suggest that this SDS-assisted protocol is a practical, simple, and broadly applicable proteomic sample processing method, which can be particularly useful when dealing with samples difficult to solubilize by other methods.« less
Sampling and Chemical Analysis of Potable Water for ISS Expeditions 12 and 13
NASA Technical Reports Server (NTRS)
Straub, John E. II; Plumlee, Deborah K.; Schultz, John R.
2007-01-01
The crews of Expeditions 12 and 13 aboard the International Space Station (ISS) continued to rely on potable water from two different sources, regenerated humidity condensate and Russian ground-supplied water. The Space Shuttle launched twice during the 12- months spanning both expeditions and docked with the ISS for delivery of hardware and supplies. However, no Shuttle potable water was transferred to the station during either of these missions. The chemical quality of the ISS onboard potable water supplies was verified by performing ground analyses of archival water samples at the Johnson Space Center (JSC) Water and Food Analytical Laboratory (WAFAL). Since no Shuttle flights launched during Expedition 12 and there was restricted return volume on the Russian Soyuz vehicle, only one chemical archive potable water sample was collected with U.S. hardware and returned during Expedition 12. This sample was collected in March 2006 and returned on Soyuz 11. The number and sensitivity of the chemical analyses performed on this sample were limited due to low sample volume. Shuttle flights STS-121 (ULF1.1) and STS-115 (12A) docked with the ISS in July and September of 2006, respectively. These flights returned to Earth with eight chemical archive potable water samples that were collected with U.S. hardware during Expedition 13. The average collected volume increased for these samples, allowing full chemical characterization to be performed. This paper presents a discussion of the results from chemical analyses performed on Expeditions 12 and 13 archive potable water samples. In addition to the results from the U.S. samples analyzed, results from pre-flight samples of Russian potable water delivered to the ISS on Progress vehicles and in-flight samples collected with Russian hardware during Expeditions 12 and 13 and analyzed at JSC are also discussed.
Macy, Jamie P.; Monroe, Stephen A.
2006-01-01
The National Park Service initiated a Level 1 Water-Quality Inventory program to provide water-quality data to park managers so informed natural resource management decisions could be made. Level 1 water-quality data were collected by the U.S. Geological Survey Arizona Water Science Center at 57 sites in 13 National Park units located in the Southern Colorado Plateau Inventory and Monitoring network in water years 2005 and 2006. These data describe the current water-quality at selected sites within the park units and provide information for monitoring future trends. Water samples were collected three times at each type of site including wells, springs, seeps, tinajas, rivers, a lake, and an irrigation ditch. Field measurements were taken at each site and they included pH, specific conductance, temperature, barometric pressure, dissolved oxygen, alkalinity, turbidity, and discharge rates where applicable. Water samples collected were sent to the U.S. Geological Survey National Water Quality Laboratory and analyzed for major ions, trace elements, and nutrients. The National Water Quality Laboratory also analyzed selected samples for mercury and petroleum hydrocarbons. Additional samples at selected sites were collected and analyzed for cyanide, radiochemistry, and suspended sediment by U.S. Geological Survey contract labs. Fecal-indicator bacteria (Escherichia coli) were sampled for at selected sites as another indicator of water quality. Quality control for this study was achieved through proper training of field personnel, use of standard U.S. Geological Survey field and laboratory protocols, collection of sample blanks and replicates, and a thorough review of the water-quality analyses. Measured field pH ranged from 6.0 to 8.8, within normal range for springs and rivers, at most sites. Concentrations of dissolved solids ranged from 48 to 8,680 mg/L and the majority of samples had concentrations of dissolved solids below 900 mg/L. Trace-element concentrations at most sites were at or near the laboratory reporting levels. The highest overall trace-element concentrations were found at U.S. Highway 160 Spring near Park Entrance to Mesa Verde National Park. Concentrations of uranium in samples at all sites ranged from below the detection limit to 55.7 ?g/L. Water samples from selected sites were analyzed for total petroleum hydrocarbons and concentrations of total petroleum hydrocarbons were at or above the laboratory detection limit in samples at six National Park units. Ten sites were sampled for Escherichia coli and positive counts were found at 9 out of the ten sites, the highest colony counts were found at Chinle Creek at Chinle, AZ in Canyon de Chelly National Monument. Measured concentrations of dissolved ammonia, nitrite, and nitrate were at or near laboratory reporting levels at most sites; nitrate concentrations ranged from below the reporting limit (0.047 mg/L) to 9.77 mg/L. Samples that were analyzed for mercury had concentrations below or at the laboratory reporting level. Concentrations of cyanide were less than the laboratory reporting level for all samples except two, Spruce Tree House Spring in Mesa Verde National Park and Pine Tree Canyon Tinaja in Canyon de Chelly National Monument, which had average concentrations of .042 and .011 ?g/L respectively. Gross alpha/beta radioactivity counts were below the U.S. Environmental Protection Agency maximum contaminant level except for samples from Casa Chiquita Well Middle at Chaco Culture National Historical Park which averaged 35 pCi/L. Suspended-sediment concentrations were variable and ranged from 10 to 150,000 mg/L.
Jacobsen, Sonja; Patel, Pranav; Schmidt-Chanasit, Jonas; Leparc-Goffart, Isabelle; Teichmann, Anette; Zeller, Herve; Niedrig, Matthias
2016-03-01
Since the re-emergence of Chikungunya virus (CHIKV) in Reunion in 2005 and the recent outbreak in the Caribbean islands with an expansion to the Americas the CHIK diagnostic became very important. We evaluate the performance of laboratories regarding molecular and serological diagnostic of CHIK worldwide. A panel of 12 samples for molecular and 13 samples for serology were provided to 60 laboratories in 40 countries for evaluating the sensitivity and specificity of molecular and serology testing. The panel for molecular diagnostic testing was analysed by 56 laboratories returning 60 data sets of results whereas the 56 and 60 data sets were returned for IgG and IgM diagnostic from the participating laboratories. Twenty-three from 60 data sets performed optimal, 7 acceptable and 30 sets of results require improvement. From 50 data sets only one laboratory shows an optimal performance for IgM detection, followed by 9 data sets with acceptable and the rest need for improvement. From 46 IgG serology data sets 20 provide an optimal, 2 an acceptable and 24 require improvement performance. The evaluation of some of the diagnostic performances allows linking the quality of results to the in-house methods or commercial assays used. The external quality assurance for CHIK diagnostics provides a good overview on the laboratory performance regarding sensitivity and specificity for the molecular and serology diagnostic required for the quick and reliable analysis of suspected CHIK patients. Nearly half of the laboratories have to improve their diagnostic profile to achieve a better performance. Copyright © 2016 Z. Published by Elsevier B.V. All rights reserved.
Spatial patterns of denitrification and its functional genes in peatlands
NASA Astrophysics Data System (ADS)
Mander, Ülo; Ligi, Teele; Truu, Marika; Truu, Jaak; Pärn, Jaan; Egorov, Sergey; Järveoja, Järvi; Vohla, Christina; Maddison, Martin; Soosaar, Kaido; Oopkaup, Kristjan; Teemusk, Alar; Preem, Jens-Konrad; Uuemaa, Evelyn
2014-05-01
This study is aimed to analyse relationships between the environmental factors and the spatial distribution of the main functional genes nirS, nirK, and nosZ regulating the denitrification process. Variations in hydrological regime, soil temperature and peat quality have been taken into the consideration at both local and global scale. Measurements of greenhouse gas (GHG) emissions using static chambers, groundwater analysis, gas and peat sampling for further laboratory analysis has been conducted in various peatlands in Iceland (two study areas, 2011), Transylvania/Romania (2012), Santa Catarina/Brazil (2012), Quebec/Canada (2012), Bashkortostan/Russian Federation (two study areas, 2012), Sichuan/China (2012), Estonia (two study areas, 2012), Florida/USA (2013, Sologne/France (2013), Jugra in West Siberia/Russia (2013), Uganda (2013), French Guyana (two study areas, 2013), Tasmania (two study areas, 2014) and New Zealand (two study areas, 2014). In each study area at least 2 transects along the groundwater depth gradient, one preferably in undisturbed, another one in drained area, and at least 3 rows of sampling sites (3-5 replicate chambers and 1 piezometer and soil sampling plot in each) in both has been established for studies. In each transect GHG emission was measured during 2-3 days in at least 5 sessions. In addition, organic sediments from the artificial riverine wetlands in Ohio/USA in 2009 and relevant gas emission studies have been used in the analyses. In the laboratories of Estonian University of Life Sciences and the University of Tartu, the peat chemical quality (pH, N, P, C, NH4, NO3) and N2O, CO2, and CH4 concentration in gas samples (50mL glass bottles and exetainers) were analysed. The peat samples for further pyrosequencing and qPCR analyses are stored in fridge by -22oC. This presentation will consider the variation of GHG emissions and hydrological conditions in the study sites. In addition, several selected biophysical factors will be taken into account. Further study will include peatland sites in Montana/USA, Columbia (Andes), Tierra del Fuego/Argentina, Pyrenees/Spain, Savo/Finland, the Netherlands, Okawango/Botswana, Heilongjiang/China, and Kamchatka/Russian Federation. Also, additional analysis will be conducted on the relationships between the intensity of CH4 emissions and methanogenesis regulating functional genes mcrA, pmoA, and dsrAB.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Cooke, Gary A.; Pestovich, John A.; Huber, Heinz J.
This report presents the results for solid phase characterization (SPC) of solid samples removed from tank 241-C-108 (C-108) on August 12-13,2012, using the off-riser sampler. Samples were received at the 222-S Laboratory on August 13 and were described and photographed. The SPC analyses that were performed include scanning electron microscopy (SEM) using the ASPEX(R)l scanning electron microscope, X-ray diffraction (XRD) using the Rigaku(R) 2 MiniFlex X-ray diffractometer, and polarized light microscopy (PLM) using the Nikon(R) 3 Eclipse Pol optical microscope. The SEM is equipped with an energy dispersive X-ray spectrometer (EDS) to provide chemical information. Gary A. Cooke conducted themore » SEM analysis, John A. Pestovich performed the XRD analysis, and Dr. Heinz J. Huber performed the PLM examination. The results of these analyses are presented here.« less
NASA Astrophysics Data System (ADS)
Wijaya, I. M. W.; Soedjono, E. S.
2018-03-01
Municipal wastewater is the main contributor to diverse water pollution problems. In order to prevent the pollution risks, wastewater have to be treated before discharged to the main water. Selection of appropriated treatment process need the characteristic information of wastewater as design consideration. This study aims to analyse the physicochemical characteristic of municipal wastewater from inlet and outlet of ABR unit around Surabaya City. Medokan Semampir and Genteng Candi Rejo has been selected as wastewater sampling point. The samples were analysed in laboratory with parameters, such as pH, TSS, COD, BOD, NH4 +, NO3 -, NO2 -, P, and detergent. The results showed that all parameters in both locations are under the national standard of discharged water quality. In other words, the treated water is securely discharged to the river
Antibacterial properties of grapefruit seed extract against Paenibacillus larvae subsp. larvae.
Semprini, P; Langella, V; Pasini, B; Falda, M T; Calvarese, S
2004-01-01
Twenty-one samples of grapefruit seed extract (GSE) either from marketed products or provided by an apiculturist were analysed to verify their inhibition activity, in particular against Paenibacillus larvae subsp. larvae, responsible for American foulbrood. The bactericide capacity of GSE has been measured in Bacillus subtilis BGA, Bacillus cereus 11778, Bacillus cereus K250 and Micrococcus luteus 9341a; these bacteria are normally used in the laboratory to study inhibitors. The results showed that not all GSE have the same inhibitory activity and two of those analysed do not inhibit the five bacteria used. Considering that 19 samples inhibited American foulbrood bacillus, the authors conclude that the use of a natural product (such as GSE) to control this important disease of bees, can be used as a substitute for chemotherapeutic products, after appropriate expedients.
Ball, James W.; McMleskey, R. Blaine; Nordstrom, D. Kirk
2010-01-01
Water analyses are reported for 104 samples collected from numerous thermal and non-thermal features in Yellowstone National Park (YNP) during 2006-2008. Water samples were collected and analyzed for major and trace constituents from 10 areas of YNP including Apollinaris Spring and Nymphy Creek along the Norris-Mammoth corridor, Beryl Spring in Gibbon Canyon, Norris Geyser Basin, Lower Geyser Basin, Crater Hills, the Geyser Springs Group, Nez Perce Creek, Rabbit Creek, the Mud Volcano area, and Washburn Hot Springs. These water samples were collected and analyzed as part of research investigations in YNP on arsenic, antimony, iron, nitrogen, and sulfur redox species in hot springs and overflow drainages, and the occurrence and distribution of dissolved mercury. Most samples were analyzed for major cations and anions, trace metals, redox species of antimony, arsenic, iron, nitrogen, and sulfur, and isotopes of hydrogen and oxygen. Analyses were performed at the sampling site, in an on-site mobile laboratory vehicle, or later in a U.S. Geological Survey laboratory, depending on stability of the constituent and whether it could be preserved effectively. Water samples were filtered and preserved on-site. Water temperature, specific conductance, pH, emf (electromotive force or electrical potential), and dissolved hydrogen sulfide were measured on-site at the time of sampling. Dissolved hydrogen sulfide was measured a few to several hours after sample collection by ion-specific electrode on samples preserved on-site. Acidity was determined by titration, usually within a few days of sample collection. Alkalinity was determined by titration within 1 to 2 weeks of sample collection. Concentrations of thiosulfate and polythionate were determined as soon as possible (generally a few to several hours after sample collection) by ion chromatography in an on-site mobile laboratory vehicle. Total dissolved iron and ferrous iron concentrations often were measured on-site in the mobile laboratory vehicle. Concentrations of dissolved aluminum, arsenic, boron, barium, beryllium, calcium, cadmium, cobalt, chromium, copper, iron, potassium, lithium, magnesium, manganese, molybdenum, sodium, nickel, lead, selenium, silica, strontium, vanadium, and zinc were determined by inductively coupled plasma-optical emission spectrometry. Trace concentrations of dissolved antimony, cadmium, cobalt, chromium, copper, lead, and selenium were determined by Zeeman-corrected graphite-furnace atomic-absorption spectrometry. Dissolved concentrations of total arsenic, arsenite, total antimony, and antimonite were determined by hydride generation atomic-absorption spectrometry using a flow-injection analysis system. Dissolved concentrations of total mercury and methylmercury were determined by cold-vapor atomic fluorescence spectrometry. Concentrations of dissolved chloride, fluoride, nitrate, bromide, and sulfate were determined by ion chromatography. For many samples, concentrations of dissolved fluoride also were determined by ion-specific electrode. Concentrations of dissolved ferrous and total iron were determined by the FerroZine colorimetric method. Concentrations of dissolved ammonium were determined by ion chromatography, with reanalysis by colorimetry when separation of sodium and ammonia peaks was poor. Dissolved organic carbon concentrations were determined by the wet persulfate oxidation method. Hydrogen and oxygen isotope ratios were determined using the hydrogen and CO2 equilibration techniques, respectively.
The forensiX evidence collection tube and its impact on DNA preservation and recovery.
Garvin, Alex M; Holzinger, Ralf; Berner, Florian; Krebs, Walter; Hostettler, Bernhard; Lardi, Elges; Hertli, Christian; Quartermaine, Roy; Stamm, Christoph
2013-01-01
Biological samples are vulnerable to degradation from the time they are collected until they are analysed at the laboratory. Biological contaminants, such as bacteria, fungi, and enzymes, as well as environmental factors, such as sunlight, heat, and humidity, can increase the rate of DNA degradation. Currently, DNA samples are normally dried or frozen to limit their degradation prior to their arrival at the laboratory. In this study, the effect of the sample drying rate on DNA preservation was investigated, as well as a comparison between drying and freezing methods. The drying performances of two commercially available DNA collection tools (swab and drying tube) with different drying rates were evaluated. The swabs were used to collect human saliva, placed into the drying tubes, and stored in a controlled environment at 25°C and 60% relative humidity, or frozen at -20°C, for 2 weeks. Swabs that were stored in fast sample drying tubes yielded 95% recoverable DNA, whereas swabs stored in tubes with slower sample drying rates yielded only 12% recoverable DNA; saliva stored in a microtube at -20°C was used as a control. Thus, DNA sampling tools that offer rapid drying can significantly improve the preservation of DNA collected on a swab, increasing the quantity of DNA available for subsequent analysis.
Desmarchelier, Aurélien; Anizan, Sébastien; Minh Tien, Mai; Savoy, Marie-Claude; Bion, Cindy
2018-04-01
An LC-MS/MS method is presented for screening five tetracyclines and their epimers in a broad range of food products. The scope of matrices includes meat-, fish-, seafood-based products, various dairy ingredients, infant formulae and fats. The method principle is based on a liquid-liquid extraction with aqueous ethylenediaminetetraacetic acid (EDTA) and acetonitrile followed by a freezing step to promote phase separation at low temperature. After defatting with hexane, sample extracts were evaporated and reconstituted before injection onto the LC-MS/MS system. The addition of oxalic acid in the aqueous mobile phase was mandatory to maintain good peak shape and sensitivity over the run. The screening is based upon a double preparation of each sample, one 'as such' and a second one with the analytes spiked in the sample, in order to mitigate the risk of false negative response. The method was validated according to the European Community Reference Laboratories Residues Guidelines. A total of 93 samples were included in the validation by two independent laboratories giving both false-negative and false-positive rates at 0% for all compounds. Over the last two years, 2600 samples were analysed routinely and only one chicken sample was found above the regulatory limit.
[Determination of ethylene glycol in biological fluids--propylene glycol interferences].
Gomółka, Ewa; Cudzich-Czop, Sylwia; Sulka, Adrianna
2013-01-01
Many laboratories in Poland do not use gas chromatography (GC) method for determination of ethylene glycol (EG) and methanol in blood of poisoned patients, they use non specific spectrophotometry methods. One of the interfering substances is propylene glycol (PG)--compound present in many medical and cosmetic products: drops, air freshens, disinfectants, electronic cigarettes and others. In Laboratory of Analytical Toxicology and Drug Monitoring in Krakow determination of EG is made by GC method. The method enables to distinguish and make resolution of (EG) and (PG) in biological samples. In the years 2011-2012 in several serum samples from diagnosed patients PG was present in concentration from several to higher than 100 mg/dL. The aim of the study was to estimate PG interferences of serum EG determination by spectrophotometry method. Serum samples containing PG and EG were used in the study. The samples were analyzed by two methods: GC and spectrophotometry. Results of serum samples spiked with PG with no EG analysed by spectrophotometry method were improper ("false positive"). The results were correlated to PG concentration in samples. Calculated cross-reactivity of PG in the method was 42%. Positive results of EG measured by spectrophotometry method must be confirmed by reference GC method. Spectrophotometry method shouldn't be used for diagnostics and monitoring of patients poisoned by EG.
NASA Astrophysics Data System (ADS)
Briois, Christelle; Thissen, Roland; Thirkell, Laurent; Aradj, Kenzi; Bouabdellah, Abdel; Boukrara, Amirouche; Carrasco, Nathalie; Chalumeau, Gilles; Chapelon, Olivier; Colin, Fabrice; Coll, Patrice; Cottin, Hervé; Engrand, Cécile; Grand, Noel; Lebreton, Jean-Pierre; Orthous-Daunay, François-Régis; Pennanech, Cyril; Szopa, Cyril; Vuitton, Véronique; Zapf, Pascal; Makarov, Alexander
2016-10-01
For decades of space exploration, mass spectrometry has proven to be a reliable instrumentation for the characterisation of the nature and energy of ionic and neutral, atomic and molecular species in the interplanetary medium and upper planetary atmospheres. It has been used as well to analyse the chemical composition of planetary and small bodies environments. The chemical complexity of these environments calls for the need to develop a new generation of mass spectrometers with significantly increased mass resolving power. The recently developed OrbitrapTM mass analyser at ultra-high resolution shows promising adaptability to space instrumentation, offering improved performances for in situ measurements. In this article, we report on our project named ;Cosmorbitrap; aiming at demonstrating the adaptability of the Orbitrap technology for in situ space exploration. We present the prototype that was developed in the laboratory for demonstration of both technical feasibility and analytical capabilities. A set of samples containing elements with masses ranging from 9 to 208 u has been used to evaluate the performance of the analyser, in terms of mass resolving power (reaching 474,000 at m/z 9) and ability to discriminate between isobaric interferences, accuracy of mass measurement (below 15 ppm) and determination of relative isotopic abundances (below 5%) of various samples. We observe a good agreement between the results obtained with the prototype and those of a commercial instrument. As the background pressure is a key parameter for in situ exploration of atmosphere planetary bodies, we study the effect of background gas on the performance of the Cosmorbitrap prototype, showing an upper limit for N2 in our set-up at 10-8 mbar. The results demonstrate the strong potential to adapt this technology to space exploration.
NASA Technical Reports Server (NTRS)
Sheridan, Patrick J.
1999-01-01
Herein is reported activities to support the characterization of the aerosol in the upper troposphere (UT) and lower stratosphere (LS) collected during the Airborne Southern Hemisphere Ozone Experiment/Measurements for Assessing the Effects of Stratospheric Aircraft (ASHOE/MAESA) missions in 1994. Through a companion proposal, another group was to measure the size distribution of aerosols in the 0.008 to 2 micrometer diameter range and to collect for us impactor samples of particles larger than about 0.02 gm. In the first year, we conducted laboratory studies related to particulate deposition patterns on our collection substrates, and have performed the analysis of many ASHOE/MAESA aerosol samples from 1994 using analytical electron microscopy (AEM). We have been building an "aerosol climatology" with these data that documents the types and relative abundances of particles observed at different latitudes and altitudes. The second year (and non-funded extension periods) saw continued analyses of impactor aerosol samples, including more ASHOE/MAESA samples, some northern hemisphere samples from the NASA Stratospheric Photochemistry Aerosols and Dynamics Expedition (SPADE) program for comparison, and a few aerosol samples from the NASA Stratospheric TRacers of Atmospheric Transport (STRAT) program. A high-resolution field emission microscope was used for the analysis and re-analysis of a number of samples to determine if this instrument was superior in performance to our conventional electron microscope. In addition, some basic laboratory studies were conducted to determine the minimum detectable and analyzable particle size for different types of aerosols. In all, 61 aerosol samples were analyzed, with a total of over 30,000 individual particle analyses. In all analyzed samples, sulfate particles comprised the major aerosol number fraction. It must be stressed that particles composed of more than one species, for example sulfate and organic carbon, were classified according to the major fraction. Thus, many of the particles classified as sulfate may have contained significant mass fractions of carbonaceous or other material. These particles for the most part did not show two physical phases, however. Nonsulfate particles were classified according to the physical and chemical characteristics of each particle, and were grouped into the major nonsulfate particle classes, including C-rich, crustal, metallic, and salts. Our UT and LS sample analyses indicate a maximum for crustal and C-rich particle abundance in the Northern Hemisphere upper troposphere, and a salt particle maximum in the Southern Hemisphere upper troposphere. Metallic particles are clearly more prevalent in the troposphere than in the stratosphere, but interhemispheric differences appear small.
Comazzi, S; Cozzi, M; Bernardi, S; Zanella, D R; Aresu, L; Stefanello, D; Marconato, L; Martini, V
2018-02-01
Flow cytometry (FC) is increasingly being used for immunophenotyping and staging of canine lymphoma. The aim of this retrospective study was to assess pre-analytical variables that might influence the diagnostic utility of FC of lymph node (LN) fine needle aspirate (FNA) specimens from dogs with lymphoproliferative diseases. The study included 987 cases with LN FNA specimens sent for immunophenotyping that were submitted to a diagnostic laboratory in Italy from 2009 to 2015. Cases were grouped into 'diagnostic' and 'non-diagnostic'. Pre-analytical factors analysed by univariate and multivariate analyses were animal-related factors (breed, age, sex, size), operator-related factors (year, season, shipping method, submitting veterinarian) and sample-related factors (type of sample material, cellular concentration, cytological smears, artefacts). The submitting veterinarian, sample material, sample cellularity and artefacts affected the likelihood of having a diagnostic sample. The availability of specimens from different sites and of cytological smears increased the odds of obtaining a diagnostic result. Major artefacts affecting diagnostic utility included poor cellularity and the presence of dead cells. Flow cytometry on LN FNA samples yielded conclusive results in more than 90% of cases with adequate sample quality and sampling conditions. Copyright © 2018 Elsevier Ltd. All rights reserved.
Flegar-Meštrić, Zlata; Perkov, Sonja; Radeljak, Andrea
2016-03-26
Considering the fact that the results of laboratory tests provide useful information about the state of health of patients, determination of reference value is considered an intrinsic part in the development of laboratory medicine. There are still huge differences in the analytical methods used as well as in the associated reference intervals which could consequently significantly affect the proper assessment of patient health. In a constant effort to increase the quality of patients' care, there are numerous international initiatives for standardization and/or harmonization of laboratory diagnostics in order to achieve maximum comparability of laboratory test results and improve patient safety. Through the standardization and harmonization processes of analytical methods the ability to create unique reference intervals is achieved. Such reference intervals could be applied globally in all laboratories using methods traceable to the same reference measuring system and analysing the biological samples from the populations with similar socio-demographic and ethnic characteristics. In this review we outlined the results of the harmonization processes in Croatia in the field of population based reference intervals for clinically relevant blood and serum constituents which are in accordance with ongoing activity for worldwide standardization and harmonization based on traceability in laboratory medicine.
Flegar-Meštrić, Zlata; Perkov, Sonja; Radeljak, Andrea
2016-01-01
Considering the fact that the results of laboratory tests provide useful information about the state of health of patients, determination of reference value is considered an intrinsic part in the development of laboratory medicine. There are still huge differences in the analytical methods used as well as in the associated reference intervals which could consequently significantly affect the proper assessment of patient health. In a constant effort to increase the quality of patients’ care, there are numerous international initiatives for standardization and/or harmonization of laboratory diagnostics in order to achieve maximum comparability of laboratory test results and improve patient safety. Through the standardization and harmonization processes of analytical methods the ability to create unique reference intervals is achieved. Such reference intervals could be applied globally in all laboratories using methods traceable to the same reference measuring system and analysing the biological samples from the populations with similar socio-demographic and ethnic characteristics. In this review we outlined the results of the harmonization processes in Croatia in the field of population based reference intervals for clinically relevant blood and serum constituents which are in accordance with ongoing activity for worldwide standardization and harmonization based on traceability in laboratory medicine. PMID:27019800
Ozarda, Yesim; Ichihara, Kiyoshi; Barth, Julian H; Klee, George
2013-05-01
The reference intervals (RIs) given in laboratory reports have an important role in aiding clinicians in interpreting test results in reference to values of healthy populations. In this report, we present a proposed protocol and standard operating procedures (SOPs) for common use in conducting multicenter RI studies on a national or international scale. The protocols and consensus on their contents were refined through discussions in recent C-RIDL meetings. The protocol describes in detail (1) the scheme and organization of the study, (2) the target population, inclusion/exclusion criteria, ethnicity, and sample size, (3) health status questionnaire, (4) target analytes, (5) blood collection, (6) sample processing and storage, (7) assays, (8) cross-check testing, (9) ethics, (10) data analyses, and (11) reporting of results. In addition, the protocol proposes the common measurement of a panel of sera when no standard materials exist for harmonization of test results. It also describes the requirements of the central laboratory, including the method of cross-check testing between the central laboratory of each country and local laboratories. This protocol and the SOPs remain largely exploratory and may require a reevaluation from the practical point of view after their implementation in the ongoing worldwide study. The paper is mainly intended to be a basis for discussion in the scientific community.
NASA Astrophysics Data System (ADS)
Kostadinova-Avramova, M.; Kovacheva, M.
2015-10-01
Archaeological baked clay remains provide valuable information about the geomagnetic field in historical past, but determination of the geomagnetic field characteristics, especially intensity, is often a difficult task. This study was undertaken to elucidate the reasons for unsuccessful intensity determination experiments obtained from two different Bulgarian archaeological sites (Nessebar - Early Byzantine period and Malenovo - Early Iron Age). With this aim, artificial clay samples were formed in the laboratory and investigated. The clay used for the artificial samples preparation differs according to its initial state. Nessebar clay was baked in the antiquity, but Malenovo clay was raw, taken from the clay deposit near the site. The obtained artificial samples were repeatedly heated eight times in known magnetic field to 700 °C. X-ray diffraction analyses and rock-magnetic experiments were performed to obtain information about the mineralogical content and magnetic properties of the initial and laboratory heated clays. Two different protocols were applied for the intensity determination-Coe version of Thellier and Thellier method and multispecimen parallel differential pTRM protocol. Various combinations of laboratory fields and mutual positions of the directions of laboratory field and carried thermoremanence were used in the performed Coe experiment. The obtained results indicate that the failure of this experiment is probably related to unfavourable grain sizes of the prevailing magnetic carriers combined with the chosen experimental conditions. The multispecimen parallel differential pTRM protocol in its original form gives excellent results for the artificial samples, but failed for the real samples (samples coming from previously studied kilns of Nessebar and Malenovo sites). Obviously the strong dependence of this method on the homogeneity of the used subsamples hinders its implementation in its original form for archaeomaterials. The latter are often heterogeneous due to variable heating conditions in the different parts of the archaeological structures. The study draws attention to the importance of multiple heating for the stabilization of grain size distribution in baked clay materials and the need of elucidation of this question.