Technology development in support of the TWRS process flowsheet. Revision 1

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

Washenfelder, D.J.

1995-10-11

The Tank Waste Remediation System is to treat and dispose of Hanford`s Single-Shell and Double-Shell Tank Waste. The TWRS Process Flowsheet, (WHC-SD-WM-TI-613 Rev. 1) described a flowsheet based on a large number of assumptions and engineering judgements that require verification or further definition through process and technology development activities. This document takes off from the TWRS Process Flowsheet to identify and prioritize tasks that should be completed to strengthen the technical foundation for the flowsheet.

Processing of irradiated, enriched uranium fuels at the Savannah River Plant

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

Hyder, M L; Perkins, W C; Thompson, M C

Uranium fuels containing /sup 235/U at enrichments from 1.1% to 94% are processed and recovered, along with neptunium and plutonium byproducts. The fuels to be processed are dissolved in nitric acid. Aluminum-clad fuels are disssolved using a mercury catalyst to give a solution rich in aluminum. Fuels clad in more resistant materials are dissolved in an electrolytic dissolver. The resulting solutions are subjected to head-end treatment, including clarification and adjustment of acid and uranium concentration before being fed to solvent extraction. Uranium, neptunium, and plutonium are separated from fission products and from one another by multistage countercurrent solvent extraction withmore » dilute tri-n-butyl phosphate in kerosene. Nitric acid is used as the salting agent in addition to aluminum or other metal nitrates present in the feed solution. Nuclear safety is maintained through conservative process design and the use of monitoring devices as secondary controls. The enriched uranium is recovered as a dilute solution and shipped off-site for further processing. Neptunium is concentrated and sent to HB-Line for recovery from solution. The relatively small quantities of plutonium present are normally discarded in aqueous waste, unless the content of /sup 238/Pu is high enough to make its recovery desirable. Most of the /sup 238/Pu can be recovered by batch extraction of the waste solution, purified by counter-current solvent extraction, and converted to oxide in HB-Line. By modifying the flowsheet, /sup 239/Pu can be recovered from low-enriched uranium in the extraction cycle; neptunium is then not recovered. The solvent is subjected to an alkaline wash before reuse to remove degraded solvent and fission products. The aqueous waste is concentrated and partially deacidified by evaporation before being neutralized and sent to the waste tanks; nitric acid from the overheads is recovered for reuse.« less

Impact of Salt Waste Processing Facility Streams on the Nitric-Glycolic Flowsheet in the Chemical Processing Cell

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

Martino, C.

An evaluation of the previous Chemical Processing Cell (CPC) testing was performed to determine whether the planned concurrent operation, or “coupled” operations, of the Defense Waste Processing Facility (DWPF) with the Salt Waste Processing Facility (SWPF) has been adequately covered. Tests with the nitricglycolic acid flowsheet, which were both coupled and uncoupled with salt waste streams, included several tests that required extended boiling times. This report provides the evaluation of previous testing and the testing recommendation requested by Savannah River Remediation. The focus of the evaluation was impact on flammability in CPC vessels (i.e., hydrogen generation rate, SWPF solvent components,more » antifoam degradation products) and processing impacts (i.e., acid window, melter feed target, rheological properties, antifoam requirements, and chemical composition).« less

Next Generation Solvent (NGS): Development for Caustic-Side Solvent Extraction of Cesium

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

Moyer, Bruce A.; Birdwell, Jr, Joseph F.; Bonnesen, Peter V.

This report summarizes the FY 2010 and 2011 accomplishments at Oak Ridge National Laboratory (ORNL) in developing the Next Generation Caustic-Side Solvent Extraction (NG-CSSX) process, referred to commonly as the Next Generation Solvent (NGS), under funding from the U.S. Department of Energy, Office of Environmental Management (DOE-EM), Office of Technology Innovation and Development. The primary product of this effort is a process solvent and preliminary flowsheet capable of meeting a target decontamination factor (DF) of 40,000 for worst-case Savannah River Site (SRS) waste with a concentration factor of 15 or higher in the 18-stage equipment configuration of the SRS Modularmore » Caustic-Side Solvent Extraction Unit (MCU). In addition, the NG-CSSX process may be readily adapted for use in the SRS Salt Waste Processing Facility (SWPF) or in supplemental tank-waste treatment at Hanford upon appropriate solvent or flowsheet modifications. Efforts in FY 2010 focused on developing a solvent composition and process flowsheet for MCU implementation. In FY 2011 accomplishments at ORNL involved a wide array of chemical-development activities and testing up through single-stage hydraulic and mass-transfer tests in 5-cm centrifugal contactors. Under subcontract from ORNL, Argonne National Laboratory (ANL) designed a preliminary flowsheet using ORNL cesium distribution data, and Tennessee Technological University confirmed a chemical model for cesium distribution ratios (DCs) as a function of feed composition. Interlaboratory efforts were coordinated with complementary engineering tests carried out (and reported separately) by personnel at Savannah River National Laboratory (SRNL) and Savannah River Remediation (SRR) with helpful advice by Parsons Engineering and General Atomics on aspects of possible SWPF implementation.« less

Next Generation Solvent Development for Caustic-Side Solvent Extraction of Cesium

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

Moyer, Bruce A.; Birdwell, Joseph F.; Bonnesen, Peter V.

This report summarizes the FY 2010 and 2011 accomplishments at Oak Ridge National Laboratory (ORNL) in developing the Next Generation Caustic-Side Solvent Extraction (NG-CSSX) process, referred to commonly as the Next Generation Solvent (NGS), under funding from the U.S. Department of Energy, Office of Environmental Management (DOE-EM), Office of Technology Innovation and Development. The primary product of this effort is a process solvent and preliminary flowsheet capable of meeting a target decontamination factor (DF) of 40,000 for worst-case Savannah River Site (SRS) waste with a concentration factor of 15 or higher in the 18-stage equipment configuration of the SRS Modularmore » Caustic-Side Solvent Extraction Unit (MCU). In addition, the NG-CSSX process may be readily adapted for use in the SRS Salt Waste Processing Facility (SWPF) or in supplemental tank-waste treatment at Hanford upon appropriate solvent or flowsheet modifications. Efforts in FY 2010 focused on developing a solvent composition and process flowsheet for MCU implementation. In FY 2011 accomplishments at ORNL involved a wide array of chemical-development activities and testing up through single-stage hydraulic and mass-transfer tests in 5-cm centrifugal contactors. Under subcontract from ORNL, Argonne National Laboratory (ANL) designed a preliminary flowsheet using ORNL cesium distribution data, and Tennessee Technological University confirmed a chemical model for cesium distribution ratios (DCs) as a function of feed composition. Inter laboratory efforts were coordinated with complementary engineering tests carried out (and reported separately) by personnel at Savannah River National Laboratory (SRNL) and Savannah River Remediation (SRR) with helpful advice by Parsons Engineering and General Atomics on aspects of possible SWPF implementation.« less

Counter-current motion in counter-current chromatography.

PubMed

Ito, Yoichiro

2014-12-12

After the CCC2012 meeting, I have received an e-mail regarding the terminology of "Countercurrent Chromatography". It stated that the term "Countercurrent" is a misnomer, because its stationary phase is motionless in the column and that the method should be renamed as liquid-liquid separations or centrifugal separations. However, it was found that these names are already used for various other techniques as found via Google search. The term "Countercurrent Chromatography" was originally made after two preparative methods of Countercurrent distribution and liquid Chromatography, both having no countercurrent motion in the column. However, it is surprising to find that this F1 hybrid method "Countercurrent Chromatography" can clearly exhibit countercurrent motion within the separation column in both hydrodynamic and hydrostatic equilibrium systems. This justifies that "Countercurrent Chromatography" is a proper term for this chromatographic method. Published by Elsevier B.V.

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

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

Edwards, T.; Peeler, D.

2014-10-28

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

Material compatibility evaluation for DWPF nitric-glycolic acid-literature review

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

Mickalonis, J.; Skidmore, E.

2013-06-01

Glycolic acid is being evaluated as an alternative for formic and nitric acid in the DWPF flowsheet. Demonstration testing and modeling for this new flowsheet has shown that glycolic acid and glycolate has a potential to remain in certain streams generated during the production of the nuclear waste glass. A literature review was conducted to assess the impact of glycolic acid on the corrosion of the materials of construction for the DWPF facility as well as facilities downstream which may have residual glycolic acid and glycolates present. The literature data was limited to solutions containing principally glycolic acid.

Enhanced separation of rare earth elements

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

Lyon, K.; Greenhalgh, M.; Herbst, R. S.

2016-09-01

Industrial rare earth separation processes utilize PC88A, a phosphonic acid ligand, for solvent extraction separations. The separation factors of the individual rare earths, the equipment requirements, and chemical usage for these flowsheets are well characterized. Alternative ligands such as Cyanex® 572 and the associated flowsheets are being investigated at the pilot scale level to determine if significant improvements to the current separation processes can be realized. These improvements are identified as higher separation factors, reduced stage requirements, or reduced chemical consumption. Any of these improvements can significantly affect the costs associated with these challenging separation proccesses. A mid/heavy rare earthmore » element (REE) separations flowsheet was developed and tested for each ligand in a 30 stage mixer-settler circuit to compare the separation performance of PC88A and Cyanex® 572. The ligand-metal complex strength of Cyanex® 572 provides efficient extraction of REE while significantly reducing the strip acid requirements. Reductions in chemical consumption have a significant impact on process economics for REE separations. Partitioning results summarized Table 1 indicate that Cyanex® 572 offers the same separation performance as PC88A while reducing acid consumption by 30% in the strip section for the mid/heavy REE separation. Flowsheet Effluent Compositions PC88A Cyanex® 572 Raffinate Mid REE Heavy REE 99.40% 0.60% 99.40% 0.60% Rich Mid REE Heavy REE 2.20% 97.80% 0.80% 99.20% Liquor Strip Acid Required 3.4 M 2.3 M Table 1 – Flowsheet results comparing separation performance of PC88A and Cyanex® 572 for a mid/heavy REE separation.« less

Coal Technology Program progress report for April 1976

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

Not Available

In the Hydrocarbonization Research program, two successful experiments were completed in the bench-scale hydrocarbonizer. A settling test at a lower temperature (390/sup 0/F) using 20 percent toluene in Solvent Refined Coal (SRC) Unfiltered Oil (UFO) produced a 30 percent clarified product in 2 hr. Characterization tests include distillation curves for Wilsonville's SRC-UFO and a particle size distribution of Pittsburg and Midway Coal Mining Company's (PAMCO) SRC-UFO. Studies of intermediate-temperature pyrolysis of large blocks have been maintained with char samples continuing to demonstrate pyrophoricity, even after heating to 700/sup 0/C. Simulated distillation analysis of tars produced by the last eight experimentsmore » are being compared with those performed at Laramie upon tars produced by the Hanna No. 2 experiment. In Coal-Fueled MIUS, stainless steel tubing to be used in one of the furnace tube bundles was ordered and the bid package for the furnace completed. Tests continued on the coal feed system and with the cold flow fluidized bed model. For the Synthoil process, flow diagrams, material balances, and utilities requirements were completed for the entire facility. For the Hydrocarbonization process, flowsheets were reviewed for compatibility; equipment lists were brought up to date; and utilities requirements were compiled from the individual flowsheets. The char recovery and storage subsystem flowsheet was completed. (auth)« less

Needs assessment for nondestructive testing and materials characterization for improved reliability in structural ceramics for heat engines

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

Johnson, D.R.; McClung, R.W.; Janney, M.A.

1987-08-01

A needs assessment was performed for nondestructive testing and materials characterization to achieve improved reliability in ceramic materials for heat engine applications. Raw materials, green state bodies, and sintered ceramics were considered. The overall approach taken to improve reliability of structural ceramics requires key inspections throughout the fabrication flowsheet, including raw materials, greed state, and dense parts. The applications of nondestructive inspection and characterization techniques to ceramic powders and other raw materials, green ceramics, and sintered ceramics are discussed. The current state of inspection technology is reviewed for all identified attributes and stages of a generalized flowsheet for advanced structuralmore » ceramics, and research and development requirements are identified and listed in priority order. 164 refs., 3 figs.« less

Coal technology program progress report, February 1976

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

None

Final testing of the 20-atm bench-scale system is underway in preparation for experiments with hydrogen. Laboratory-scale testing of a number of inexpensive pure compounds to improve the settling rate of solids in Solvent Refined Coal (SRC) unfiltered oil (UFO), bench-scale testing of the effect of the Tretolite additive on settling, and characterization tests on a new sample of UFO from the PAMCO-SRC process are reported. Experimental engineering support of an in situ gasification process include low-temperature pyrolyses at exceptionally low heating rates (0.3/sup 0/C/min). Highly pyrophoric chars were consistently produced. Aqueous by-products from coal conversion technologies and oil shale retortingmore » have been analyzed directly to determine major organic components. A report is being prepared discussing various aspects of the engineering evaluations of nuclear process heat for coal. A bench-scale test program on thermochemical water splitting for hydrogen production is under consideration. In the coal-fueled MIUS program, preparations for procurement of tubing for the matrix in the fluidized-bed furnace and for fabrication of the furnace continued. Analyses of the AiResearch gas turbine and recuperator under coal-fueled MIUS operating conditions are near completion. Process flow diagrams and heat and material balances were completed for most of the units in the synthoil process. Overall utilities requirements were calculated and the coal preparation flowsheets were finalized. For hydrocarbonization, the flowsheet was revised to include additional coal data. Flowsheets were finalized for the acid gas separation and recycle, and the oil-solids separation. (LTN)« less

Heat integrated ethanol dehydration flowsheets

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

Hutahaean, L.S.; Shen, W.H.; Brunt, V. Van

1995-04-01

zA theoretical evaluation of heat-integrated heterogeneous-azeotropic ethanol-water distillation flowsheets is presented. Simulations of two column flowsheets using several different hydrocarbon entrainers reveal a region of potential heat integration and substantial reduction in operating energy. In this paper, methods for comparing hydrocarbon entrainers are shown. Two aspects of entrainers are related to operating and capital costs. The binary azeotropic composition of the entrainer-ethanol mixture is related to the energy requirements of the flowsheet. A temperature difference in the azeotrophic column is related to the size of the column and overall process staging requirements. Although the hydrophobicity of an entrainer is essentialmore » for specification of staging in the dehydration column, no substantial increase in operating energy results from an entrainer that has a higher water content. Likewise, liquid-liquid equilibria between several entrainer-ethanol-water mixtures have no substantial effect on either staging or operation. Rather, increasing the alcohol content of the entrainer-ethanol azeotrope limits its recovery in the dehydration column, and increases the recycle and reflux streams. These effects both contribute to increasing the separation energy requirements and reducing the region of potential heat integration. A cost comparison with a multieffect extractive distillation flowsheet reveals that the costs are comparable; however, the extractive distillation flowsheet is more cost effective as operating costs increase.« less

Process for cobalt separation and recovery in the presence of nickel from sulphate solutions by Cyanex 272

NASA Astrophysics Data System (ADS)

Park, Kyung-Ho; Mohapatra, Debasish

2006-10-01

The present paper deals with the extraction of cobalt from a solution containing cobalt and nickel in a sulphate medium similar to the leach liquor obtained by the dilute sulphuric acid pressure leaching of the Pacific Ocean nodules matte followed by copper extraction. The commercial extractant Cyanex 272 (bis (2, 4, 4-trimethylpentyl) phosphinic acid) is used for this purpose. The leach liquor used for the present study contains Co =1.78 g/L and Ni=16.78 g/L. Before cobalt extraction, impurities, such as copper and iron, are removed from the leach liquor by the precipitation method. Increasing the concentration of Cyanex 272 increased the extraction percentage of cobalt due to the increase of equilibrium pH. Cobalt extraction efficiency of >99.9 % is achieved with 0.20 M Cyanex 272 in two counter-current stages at an aqueous: organic (A:O) phase ratio of 1.5∶1. Complete stripping of cobalt from the loaded organic containing 2.73 g/L Co was carried out at pH 1.4 by a synthetic cobalt spent electrolyte in two stages at an A:O ratio of 1∶2. The enrichment of cobalt during extraction and stripping operations was about 3.5 times. A complete process flowsheet for the separation and recovery of cobalt is presented.

Hanford Low-Activity Waste Processing: Demonstration of the Off-Gas Recycle Flowsheet - 13443

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

Ramsey, William G.; Esparza, Brian P.

2013-07-01

Vitrification of Hanford Low-Activity Waste (LAW) is nominally the thermal conversion and incorporation of sodium salts and radionuclides into borosilicate glass. One key radionuclide present in LAW is technetium-99. Technetium-99 is a low energy, long-lived beta emitting radionuclide present in the waste feed in concentrations on the order of 1-10 ppm. The long half-life combined with a high solubility in groundwater results in technetium-99 having considerable impact on performance modeling (as potential release to the environment) of both the waste glass and associated secondary waste products. The current Hanford Tank Waste Treatment and Immobilization Plant (WTP) process flowsheet calls formore » the recycle of vitrification process off-gas condensates to maximize the portion of technetium ultimately immobilized in the waste glass. This is required as technetium acts as a semi-volatile specie, i.e. considerable loss of the radionuclide to the process off-gas stream can occur during the vitrification process. To test the process flowsheet assumptions, a prototypic off-gas system with recycle capability was added to a laboratory melter (on the order of 1/200 scale) and testing performed. Key test goals included determination of the process mass balance for technetium, a non-radioactive surrogate (rhenium), and other soluble species (sulfate, halides, etc.) which are concentrated by recycling off-gas condensates. The studies performed are the initial demonstrations of process recycle for this type of liquid-fed melter system. This paper describes the process recycle system, the waste feeds processed, and experimental results. Comparisons between data gathered using process recycle and previous single pass melter testing as well as mathematical modeling simulations are also provided. (authors)« less

Material Compatibility Evaluation for DWPF Nitric-Glycolic Acid - Literature Review

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

Mickalonis, J. I.; Skidmore, T. E.

Glycolic acid is being evaluated as an alternative for formic and nitric acid in the DWPF flowsheet. Demonstration testing and modeling for this new flowsheet has shown that glycolic acid and glycolate has a potential to remain in certain streams generated during the production of the nuclear waste glass. A literature review was conducted to assess the impact of glycolic acid on the corrosion of the materials of construction for the DWPF facility as well as facilities downstream which may have residual glycolic acid and glycolates present. The literature data was limited to solutions containing principally glycolic acid. The reportedmore » corrosion rates and degradation characteristics have shown the following for the materials of construction.« less

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

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

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

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

A laboratory exercise using a physical model for demonstrating countercurrent heat exchange.

PubMed

Loudon, Catherine; Davis-Berg, Elizabeth C; Botz, Jason T

2012-03-01

A physical model was used in a laboratory exercise to teach students about countercurrent exchange mechanisms. Countercurrent exchange is the transport of heat or chemicals between fluids moving in opposite directions separated by a permeable barrier (such as blood within adjacent blood vessels flowing in opposite directions). Greater exchange of heat or chemicals between the fluids occurs when the flows are in opposite directions (countercurrent) than in the same direction (concurrent). When a vessel loops back on itself, countercurrent exchange can occur between the two arms of the loop, minimizing loss or uptake at the bend of the loop. Comprehension of the physical principles underlying countercurrent exchange helps students to understand how kidneys work and how modifications of a circulatory system can influence the movement of heat or chemicals to promote or minimize exchange and reinforces the concept that heat and chemicals move down their temperature or concentration gradients, respectively. One example of a well-documented countercurrent exchanger is the close arrangement of veins and arteries inside bird legs; therefore, the setup was arranged to mimic blood vessels inside a bird leg, using water flowing inside tubing as a physical proxy for blood flow within blood vessels.

Evaluation of Nursing Documentation Completion of Stroke Patients in the Emergency Department: A Pre-Post Analysis Using Flowsheet Templates and Clinical Decision Support.

PubMed

Richardson, Karen J; Sengstack, Patricia; Doucette, Jeffrey N; Hammond, William E; Schertz, Matthew; Thompson, Julie; Johnson, Constance

2016-02-01

The primary aim of this performance improvement project was to determine whether the electronic health record implementation of stroke-specific nursing documentation flowsheet templates and clinical decision support alerts improved the nursing documentation of eligible stroke patients in seven stroke-certified emergency departments. Two system enhancements were introduced into the electronic record in an effort to improve nursing documentation: disease-specific documentation flowsheets and clinical decision support alerts. Using a pre-post design, project measures included six stroke management goals as defined by the National Institute of Neurological Disorders and Stroke and three clinical decision support measures based on entry of orders used to trigger documentation reminders for nursing: (1) the National Institutes of Health's Stroke Scale, (2) neurological checks, and (3) dysphagia screening. Data were reviewed 6 months prior (n = 2293) and 6 months following the intervention (n = 2588). Fisher exact test was used for statistical analysis. Statistical significance was found for documentation of five of the six stroke management goals, although effect sizes were small. Customizing flowsheets to meet the needs of nursing workflow showed improvement in the completion of documentation. The effects of the decision support alerts on the completeness of nursing documentation were not statistically significant (likely due to lack of order entry). For example, an order for the National Institutes of Health Stroke Scale was entered only 10.7% of the time, which meant no alert would fire for nursing in the postintervention group. Future work should focus on decision support alerts that trigger reminders for clinicians to place relevant orders for this population.

Prioritized List of Research Needs to support MRWFD Case Study Flowsheet Advancement

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

Law, Jack Douglas; Soelberg, Nicholas Ray

In FY-13, a case study evaluation was performed of full recycle technologies for both the processing of light-water reactor (LWR) used nuclear fuels as well as fast reactor (FR) fuel in the full recycle option. This effort focused on the identification of the case study processes and the initial preparation of material balance flowsheets for the identified technologies. In identifying the case study flowsheets, it was decided that two cases would be developed: one which identifies the flowsheet as currently developed and another near-term target flowsheet which identifies the flowsheet as envisioned within two years, pending the results of ongoingmore » research. The case study focus is on homogeneous aqueous recycle of the U/TRU resulting from the processing of LWR fuel as feed for metal fuel fabrication. The metal fuel is utilized in a sodium-cooled fast reactor, and the used fast reactor fuel is processed using electrochemical separations. The recovered U/TRU from electrochemical separations is recycled to fuel fabrication and the fast reactor. Waste streams from the aqueous and electrochemical processing are treated and prepared for disposition. Off-gas from the separations and waste processing are also treated. As part of the FY-13 effort, preliminary process unknowns and research needs to advance the near-term target flowsheets were identified. In FY-14, these research needs were updated, expanded and prioritized. This report again updates the prioritized list of research needs based upon results to date in FY-15. The research needs are listed for each of the main portions of the flowsheet: 1) Aqueous headend, 2) Headend tritium pretreatment off-gas, 3) Aqueous U/Pu/Np recovery, 4) Aqueous TRU product solidification, 5) Aqueous actinide/lanthanide separation, 6) Aqueous off-gas treatment, 7) Aqueous HLW management, 8) Treatment of aqueous process wastes, 9) E-chem actinide separations, 10) E-chem off-gas, 11) E-chem HLW management. The identified research needs were prioritized within each of these areas. No effort was made to perform an overall prioritization. This information will be used by the MRWFD Campaign leadership in research planning for FY-16. Additionally, this information will be incorporated into the next version of the Case Study Report scheduled to be issued September 2015.« less

FY13 GLYCOLIC-NITRIC ACID FLOWSHEET DEMONSTRATIONS OF THE DWPF CHEMICAL PROCESS CELL WITH SIMULANTS

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

Lambert, D.; Zamecnik, J.; Best, D.

Savannah River Remediation is evaluating changes to its current Defense Waste Processing Facility flowsheet to replace formic acid with glycolic acid in order to improve processing cycle times and decrease by approximately 100x the production of hydrogen, a potentially flammable gas. Higher throughput is needed in the Chemical Processing Cell since the installation of the bubblers into the melter has increased melt rate. Due to the significant maintenance required for the safety significant gas chromatographs and the potential for production of flammable quantities of hydrogen, eliminating the use of formic acid is highly desirable. Previous testing at the Savannah Rivermore » National Laboratory has shown that replacing formic acid with glycolic acid allows the reduction and removal of mercury without significant catalytic hydrogen generation. Five back-to-back Sludge Receipt and Adjustment Tank (SRAT) cycles and four back-to-back Slurry Mix Evaporator (SME) cycles were successful in demonstrating the viability of the nitric/glycolic acid flowsheet. The testing was completed in FY13 to determine the impact of process heels (approximately 25% of the material is left behind after transfers). In addition, back-to-back experiments might identify longer-term processing problems. The testing was designed to be prototypic by including sludge simulant, Actinide Removal Product simulant, nitric acid, glycolic acid, and Strip Effluent simulant containing Next Generation Solvent in the SRAT processing and SRAT product simulant, decontamination frit slurry, and process frit slurry in the SME processing. A heel was produced in the first cycle and each subsequent cycle utilized the remaining heel from the previous cycle. Lower SRAT purges were utilized due to the low hydrogen generation. Design basis addition rates and boilup rates were used so the processing time was shorter than current processing rates.« less

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

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

The Liquid Waste Organization (LWO) has requested that the Savannah River National Laboratory (SRNL) to assess the impact of a 100K gallon decant volume from Tank 40H on the existing sludge-only Sludge Batch 4 (SB4)-Frit 510 flowsheet and the coupled operations flowsheet (SB4 with the Actinide Removal Process (ARP)). Another potential SB4 flowsheet modification of interest includes the addition of 3 wt% sodium (on a calcined oxide basis) to a decanted sludge-only or coupled operations flowsheet. These potential SB4 flowsheet modifications could result in significant compositional shifts to the SB4 system. This paper study provides an assessment of the impactmore » of these compositional changes to the projected glass operating windows and to the variability study for the Frit 510-SB4 system. The influence of the compositional changes on melt rate was not assessed in this study nor was it requested. Nominal Stage paper study assessments were completed using the projected compositions for the various flowsheet options coupled with Frit 510 (i.e., variation was not applied to the sludge and frit compositions). In order to gain insight into the impacts of sludge variation and/or frit variation (due to the procurement specifications) on the projected operating windows, three versions of the Variation Stage assessment were performed: (1) the traditional Variation Stage assessment in which the nominal Frit 510 composition was coupled with the extreme vertices (EVs) of each sludge, (2) an assessment of the impact of possible frit variation (within the accepted frit specification tolerances) on each nominal SB4 option, and (3) an assessment of the impact of possible variation in the Frit 510 composition due to the vendor's acceptance specifications coupled with the EVs of each sludge case. The results of the Nominal Stage assessment indicate very little difference among the various flowsheet options. All of the flowsheets provide DWPF with the possibility of targeting waste loadings (WLs) from the low 30s to the low 40s with Frit 510. In general, the Tank 40H decant has a slight negative impact on the operating window, but DWPF still has the ability to target current WLs (34%) and higher WLs if needed. While the decant does not affect practical WL targets in DWPF, melt rate could be reduced due to the lower Na{sub 2}O content. If true, the addition of 3 wt% Na{sub 2}O to the glass system may regain melt rate, assuming that the source of alkali is independent of the impact on melt rate. Coupled operations with Frit 510 via the addition of ARP to the decanted SB4 flowsheet also appears to be viable based on the projected operating windows. The addition of both ARP and 3 wt% Na{sub 2}O to a decanted Tank 40H sludge may be problematic using Frit 510. Although the Nominal Stage assessments provide reasonable operating windows for the SB4 flowsheets being considered with Frit 510, introduction of potential sludge and/or frit compositional variation does have a negative impact. The magnitude of the impact on the projected operating windows is dependent on the specific flowsheet options as well as the applied variation. The results of the traditional Variation Stage assessments indicate that the three proposed Tank 40H decanted flowsheet options (Case No.2--100K gallon decant, Case No.3--100K gallon decant and 3 wt% Na{sub 2}O addition and Case No.4--100K gallon decant and ARP) demonstrate a relatively high degree of robustness to possible sludge variation over WLs of interest with Frit 510. However, the case where the addition of both ARP and 3 wt% Na{sub 2}O is considered was problematic during the traditional Variation Stage assessment. The impact of coupling the frit specifications with the nominal SB4 flowsheet options on the projected operating windows is highly dependent on whether the upper WLs are low viscosity or liquidus temperature limited in the Nominal Stage assessments. Systems that are liquidus temperature limited exhibit a high degree of robustness to the applied frit and sludge variation, while those that are low viscosity limited show significant reductions (6 percentage points) in the upper WLs that can be obtained. When both frit and sludge variations are applied, the paper study results indicate that DWPF could be severely restricted in terms of projected operating windows for the ARP and Na{sub 2}O addition options. An experimental variability study was not performed using the final SB4 composition and Frit 510 since glasses in the ComPro{trademark} data base were identified that bounded the potential operating window of this system. The bounding ARP case was not considered in that assessment. After the flowsheet cases were identified, an electronic search of ComPro{trademark} identified approximately 12 historical glasses within the compositional regions defined by at least one of the five flowsheet options, but the compositional coverage did not appear adequate to bound all cases.« less

A Laboratory Exercise Using a Physical Model for Demonstrating Countercurrent Heat Exchange

ERIC Educational Resources Information Center

Loudon, Catherine; Davis-Berg, Elizabeth C.; Botz, Jason T.

2012-01-01

A physical model was used in a laboratory exercise to teach students about countercurrent exchange mechanisms. Countercurrent exchange is the transport of heat or chemicals between fluids moving in opposite directions separated by a permeable barrier (such as blood within adjacent blood vessels flowing in opposite directions). Greater exchange of…

Isolation of dimeric, trimeric, tetrameric and pentameric procyanidins from unroasted cocoa beans (Theobroma cacao L.) using countercurrent chromatography.

PubMed

Esatbeyoglu, Tuba; Wray, Victor; Winterhalter, Peter

2015-07-15

The main procyanidins, including dimeric B2 and B5, trimeric C1, tetrameric and pentameric procyanidins, were isolated from unroasted cocoa beans (Theobroma cacao L.) using various techniques of countercurrent chromatography, such as high-speed countercurrent chromatography (HSCCC), low-speed rotary countercurrent chromatography (LSRCCC) and spiral-coil LSRCCC. Furthermore, dimeric procyanidins B1 and B7, which are not present naturally in the analysed cocoa beans, were obtained after semisynthesis of cocoa bean polymers with (+)-catechin as nucleophile and separated by countercurrent chromatography. In this way, the isolation of dimeric procyanidin B1 in considerable amounts (500mg, purity>97%) was possible in a single run. This is the first report concerning the isolation and semisynthesis of dimeric to pentameric procyanidins from T. cacao by countercurrent chromatography. Additionally, the chemical structures of tetrameric (cinnamtannin A2) and pentameric procyanidins (cinnamtannin A3) were elucidated on the basis of (1)H NMR spectroscopy. Interflavanoid linkage was determined by NOE-correlations, for the first time. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

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

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

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

Experimental study of heat and mass transfer in a buoyant countercurrent exchange flow

NASA Astrophysics Data System (ADS)

Conover, Timothy Allan

Buoyant Countercurrent Exchange Flow occurs in a vertical vent through which two miscible fluids communicate, the higher-density fluid, residing above the lower-density fluid, separated by the vented partition. The buoyancy- driven zero net volumetric flow through the vent transports any passive scalars, such as heat and toxic fumes, between the two compartments as the fluids seek thermodynamic and gravitational equilibrium. The plume rising from the vent into the top compartment resembles a pool fire plume. In some circumstances both countercurrent flows and pool fires can ``puff'' periodically, with distinct frequencies. One experimental test section containing fresh water in the top compartment and brine (NaCl solution) in the bottom compartment provided a convenient, idealized flow for study. This brine flow decayed in time as the concentrations approached equilibrium. A second test section contained fresh water that was cooled by heat exchangers above and heated by electrical elements below and operated steadily, allowing more time for data acquisition. Brine transport was reduced to a buoyancy- scaled flow coefficient, Q*, and heat transfer was reduced to an analogous coefficient, H*. Results for vent diameter D = 5.08 cm were consistent between test sections and with the literature. Some results for D = 2.54 cm were inconsistent, suggesting viscosity and/or molecular diffusion of heat become important at smaller scales. Laser Doppler Velocimetry was used to measure velocity fields in both test sections, and in thermal flow a small thermocouple measured temperature simultaneously with velocity. Measurement fields were restricted to the plume base region, above the vent proper. In baseline periodic flow, instantaneous velocity and temperature were ensemble averaged, producing a movie of the average variation of each measure during a puffing flow cycle. The temperature movie revealed the previously unknown cold core of the puff during its early development. The renewal-length model for puffing frequency of pool fire plumes was extended to puffing countercurrent flows by estimating inflow dilution. Puffing frequencies at several conditions were reduced to Strouhal number based on dilute plume density. Results for D = 5.08 cm compared favorably to published measurements of puffing pool fires, suggesting that the two different flows obey the same periodic dynamic process.

[Advances in studies on multi-stage countercurrent extraction technology in traditional Chinese medicine].

PubMed

Xie, Zhi-Peng; Liu, Xue-Song; Chen, Yong; Cai, Ming; Qu, Hai-Bin; Cheng, Yi-Yu

2007-05-01

Multi-stage countercurrent extraction technology, integrating solvent extraction, repercolation with dynamic and countercurrent extraction, is a novel extraction technology for the traditional Chinese medicine. This solvent-saving, energy-saving and high-extraction-efficiency technology can at the most drive active compounds to diffuse from the herbal materials into the solvent stage by stage by creating concentration differences between the herbal materials and the solvents. This paper reviewed the basic principle, the influence factors and the research progress and trends of the equipments and the application of the multi-stage countercurrent extraction.

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

Deng, Yueying; Kruger, Albert A.

The Hanford Tank Waste Treatment and Immobilization Plant (WTP) Statement of Work (Department of Energy Contract DE-AC27-01RV14136, Section C) requires the contractor to develop and use process models for flowsheet analyses and pre-operational planning assessments. The Dynamic (G2) Flowsheet is a discrete-time process model that enables the project to evaluate impacts to throughput from eventdriven activities such as pumping, sampling, storage, recycle, separation, and chemical reactions. The model is developed by the Process Engineering (PE) department, and is based on the Flowsheet Bases, Assumptions, and Requirements Document (24590-WTP-RPT-PT-02-005), commonly called the BARD. The terminologies of Dynamic (G2) Flowsheet and Dynamicmore » (G2) Model are interchangeable in this document. The foundation of this model is a dynamic material balance governed by prescribed initial conditions, boundary conditions, and operating logic. The dynamic material balance is achieved by tracking the storage and material flows within the plant as time increments. The initial conditions include a feed vector that represents the waste compositions and delivery sequence of the Tank Farm batches, and volumes and concentrations of solutions in process equipment before startup. The boundary conditions are the physical limits of the flowsheet design, such as piping, volumes, flowrates, operation efficiencies, and physical and chemical environments that impact separations, phase equilibriums, and reaction extents. The operating logic represents the rules and strategies of running the plant.« less

Preparative isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. using supercritical fluid extraction combined with consecutive high-speed countercurrent chromatography.

PubMed

Yan, Rongwei; Shen, Jie; Liu, Xiaojing; Zou, Yong; Xu, Xinjun

2018-05-01

The objective of this study was to develop a consecutive preparation method for the isolation and purification of hainanmurpanin, meranzin, and phebalosin from leaves of Murraya exotica L. The process involved supercritical fluid extraction with CO 2 , solvent extraction, and two-step high-speed countercurrent chromatography. Pressure, temperature, and the volume of entrainer were optimized as 27 MPa, 52°C, and 60 mL by response surface methodology in supercritical fluid extraction with CO 2 , and the yield of the crude extracts was 7.91 g from 100 g of leaves. Subsequently, 80% methanol/water was used to extract and condense the three compounds from the crude extracts, and 4.23 g of methanol/water extracts was obtained. Then, a two-step high-speed countercurrent chromatography procedure was developed for the isolation of the three target compounds from methanol/water extracts, including conventional high-speed countercurrent chromatography for further enrichment and consecutive high-speed countercurrent chromatography for purification. The yield of concentrates from high-speed countercurrent chromatography was 2.50 g from 4.23 g of methanol/water extracts. Finally, the consecutive high-speed countercurrent chromatography produced 103.2 mg of hainanmurpanin, 244.7 mg of meranzin, and 255.4 mg of phebalosin with purities up to 97.66, 99.36, and 98.64%, respectively, from 900 mg of high-speed countercurrent chromatography concentrates in one run of three consecutive sample loadings without exchanging a solvent system. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The 9th International Countercurrent Chromatography Conference held at Dominican University, Chicago, USA, August 1-3, 2016.

PubMed

Friesen, J Brent; McAlpine, James B; Chen, Shao-Nong; Pauli, Guido F

2017-10-20

The 9th International Countercurrent Chromatography Conference (CCC 2016) was held at Dominican University near Chicago, IL (USA), from August 1st-3rd, 2016. The biennial CCC 20XX conferences provide an opportunity for countercurrent chromatography and centrifugal partition chromatography (CCC/CPC) manufactures, marketers, theorists, and research scientists to gather together socially, learn from each other, and advance countercurrent separation technology. A synopsis of the conference proceedings as well as a series of short reviews of the special edition articles is included in this document. Many productive discussions and collegial conversation at CCC 2016 attested to the liveliness, connectivity, and productivity of the global countercurrent research community and bodes well for the success of the 10th conference at the University of Braunschweig, Germany on August 1-3, 2018. Copyright © 2017 Elsevier B.V. All rights reserved.

Spiral counter-current chromatography: Design, development, application, and challenges.

PubMed

Huang, Xin-Yi; Sun, Xiao-Ming; Pei, Dong; Di, Duo-Long

2017-01-01

Depending on the rapid growth in the radial gradient of the centrifugal force, spiral counter-current chromatography can greatly improve the retention of stationary phase, especially for the aqueous two-phase systems with ultra-polar and high viscosity that are not well retained in the conventional multilayer coils counter-current chromatography. As a result, it is an attractive and alternative technology that is suited for separation of hydrophilic compounds and has led to many exciting progress in recent years. This review presents the recent advances and applications of spiral counter-current chromatography, including its major benefits and limitations, some novel methods to improve the separation efficiency and its applications in separation of real samples. In addition, the remaining challenges and future perspectives on development of spiral counter-current chromatography also are proposed in this article. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Literature review: Assessment of DWPF melter and melter off-gas system lifetime

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

Reigel, M. M.

2015-07-30

A glass melter for use in processing radioactive waste is a challenging environment for the materials of construction (MOC) resulting from a combination of high temperatures, chemical attack, and erosion/corrosion; therefore, highly engineered materials must be selected for this application. The focus of this report is to review the testing and evaluations used in the selection of the Defense Waste Processing Facility (DWPF), glass contact MOC specifically the Monofrax ® K-3 refractory and Inconel ® 690 alloy. The degradation or corrosion mechanisms of these materials during pilot scale testing and in-service operation were analyzed over a range of oxidizing andmore » reducing flowsheets; however, DWPF has primarily processed a reducing flowsheet (i.e., Fe 2+/ΣFe of 0.09 to 0.33) since the start of radioactive operations. This report also discusses the materials selection for the DWPF off-gas system and the corrosion evaluation of these materials during pilot scale testing and non-radioactive operations of DWPF Melter #1. Inspection of the off-gas components has not been performed during radioactive operations with the exception of maintenance because of plugging.« less

Literature review: Assessment of DWPF melter and melter off-gas system lifetime

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

Reigel, M.

2015-07-30

A glass melter for use in processing radioactive waste is a challenging environment for the materials of construction (MOC) resulting from a combination of high temperatures, chemical attack, and erosion/corrosion; therefore, highly engineered materials must be selected for this application. The focus of this report is to review the testing and evaluations used in the selection of the Defense Waste Processing Facility (DWPF), glass contact MOC specifically the Monofrax® K-3 refractory and Inconel® 690 alloy. The degradation or corrosion mechanisms of these materials during pilot scale testing and in-service operation were analyzed over a range of oxidizing and reducing flowsheets;more » however, DWPF has primarily processed a reducing flowsheet (i.e., Fe 2+/ΣFe of 0.09 to 0.33) since the start of radioactive operations. This report also discusses the materials selection for the DWPF off-gas system and the corrosion evaluation of these materials during pilot scale testing and non-radioactive operations of DWPF Melter #1. Inspection of the off-gas components has not been performed during radioactive operations with the exception of maintenance because of plugging.« less

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

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

Smith, T.

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

Interim glycol flowsheet reduction/oxidation (redox) model for the Defense Waste Processing Facility (DWPF)

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

Jantzen, C. M.; Williams, M. S.; Zamecnik, J. R.

Control of the REDuction/OXidation (REDOX) state of glasses containing high concentrations of transition metals, such as High Level Waste (HLW) glasses, is critical in order to eliminate processing difficulties caused by overly reduced or overly oxidized melts. Operation of a HLW melter at Fe +2/ΣFe ratios of between 0.09 and 0.33, a range which is not overly oxidizing or overly reducing, helps retain radionuclides in the melt, i.e. long-lived radioactive 99Tc species in the less volatile reduced Tc 4+ state, 104Ru in the melt as reduced Ru +4 state as insoluble RuO 2, and hazardous volatile Cr 6+ in themore » less soluble and less volatile Cr +3 state in the glass. The melter REDOX control balances the oxidants and reductants from the feed and from processing additives such as antifoam. Currently, the Defense Waste Processing Facility (DWPF) is running a formic acid-nitric acid (FN) flowsheet where formic acid is the main reductant and nitric acid is the main oxidant. During decomposition formate and formic acid releases H 2 gas which requires close control of the melter vapor space flammability. A switch to a nitric acid-glycolic acid (GN) flowsheet is desired as the glycolic acid flowsheet releases considerably less H 2 gas upon decomposition. This would greatly simplify DWPF processing. Development of an EE term for glycolic acid in the GN flowsheet is documented in this study.« less

Counter-current acid leaching process for copper azole treated wood waste.

PubMed

Janin, Amélie; Riche, Pauline; Blais, Jean-François; Mercier, Guy; Cooper, Paul; Morris, Paul

2012-09-01

This study explores the performance of a counter-current leaching process (CCLP) for copper extraction from copper azole treated wood waste for recycling of wood and copper. The leaching process uses three acid leaching steps with 0.1 M H2SO4 at 75degrees C and 15% slurry density followed by three rinses with water. Copper is recovered from the leachate using electrodeposition at 5 amperes (A) for 75 min. Ten counter-current remediation cycles were completed achieving > or = 94% copper extraction from the wood during the 10 cycles; 80-90% of the copper was recovered from the extract solution by electrodeposition. The counter-current leaching process reduced acid consumption by 86% and effluent discharge volume was 12 times lower compared with the same process without use of counter-current leaching. However, the reuse of leachates from one leaching step to another released dissolved organic carbon and caused its build-up in the early cycles.

Literature Review: Assessment of DWPF Melter and Melter Off-gas System Lifetime

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

Reigel, M.

2015-07-30

Testing to date for the MOC for the Hanford Waste Treatment and Immobilization Plant (WTP) melters is being reviewed with the lessons learned from DWPF in mind and with consideration to the changes in the flowsheet/feed compositions that have occurred since the original testing was performed. This information will be presented in a separate technical report that identifies any potential gaps for WTP processing.

Terms used by nurses to describe patient problems: can SNOMED III represent nursing concepts in the patient record?

PubMed Central

Henry, S B; Holzemer, W L; Reilly, C A; Campbell, K E

1994-01-01

OBJECTIVE: To analyze the terms used by nurses in a variety of data sources and to test the feasibility of using SNOMED III to represent nursing terms. DESIGN: Prospective research design with manual matching of terms to the SNOMED III vocabulary. MEASUREMENTS: The terms used by nurses to describe patient problems during 485 episodes of care for 201 patients hospitalized for Pneumocystis carinii pneumonia were identified. Problems from four data sources (nurse interview, intershift report, nursing care plan, and nurse progress note/flowsheet) were classified based on the substantive area of the problem and on the terminology used to describe the problem. A test subset of the 25 most frequently used terms from the two written data sources (nursing care plan and nurse progress note/flowsheet) were manually matched to SNOMED III terms to test the feasibility of using that existing vocabulary to represent nursing terms. RESULTS: Nurses most frequently described patient problems as signs/symptoms in the verbal nurse interview and intershift report. In the written data sources, problems were recorded as North American Nursing Diagnosis Association (NANDA) terms and signs/symptoms with similar frequencies. Of the nursing terms in the test subset, 69% were represented using one or more SNOMED III terms. PMID:7719788

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

Williams, M. S.; Miller, D. H.; Fowley, M. D.

The Savannah River National Laboratory (SRNL) was tasked to support validation of the Defense Waste Processing Facility (DWPF) melter offgas flammability model for the nitric-glycolic (NG) flowsheet. The work supports Deliverable 4 of the DWPF & Saltstone Facility Engineering Technical Task Request (TTR)1 and is supplemental to the Cold Cap Evaluation Furnace (CEF) testing conducted in 2014.2 The Slurry-fed Melt Rate Furnace (SMRF) was selected for the supplemental testing as it requires significantly less resources than the CEF and could provide a tool for more rapid analysis of melter feeds in the future. The SMRF platform has been used previouslymore » to evaluate melt rate behavior of DWPF glasses, but was modified to accommodate analysis of the offgas stream. Additionally, the Melt Rate Furnace (MRF) and Quartz Melt Rate Furnace (QMRF) were utilized for evaluations. MRF data was used exclusively for melt behavior observations and REDuction/OXidation (REDOX) prediction comparisons and will be briefly discussed in conjunction with its support of the SMRF testing. The QMRF was operated similarly to the SMRF for the same TTR task, but will be discussed in a separate future report. The overall objectives of the SMRF testing were to; 1) Evaluate the efficacy of the SMRF as a platform for steady state melter testing with continuous feeding and offgas analysis; and 2) Generate supplemental melter offgas flammability data to support the melter offgas flammability modelling effort for DWPF implementation of the NG flowsheet.« less

SCIX IMPACT ON DWPF CPC

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

Koopman, D.

2011-07-14

A program was conducted to systematically evaluate potential impacts of the proposed Small Column Ion Exchange (SCIX) process on the Defense Waste Processing Facility (DWPF) Chemical Processing Cell (CPC). The program involved a series of interrelated tasks. Past studies of the impact of crystalline silicotitanate (CST) and monosodium titanate (MST) on DWPF were reviewed. Paper studies and material balance calculations were used to establish reasonable bounding levels of CST and MST in sludge. Following the paper studies, Sludge Batch 10 (SB10) simulant was modified to have both bounding and intermediate levels of MST and ground CST. The SCIX flow sheetmore » includes grinding of the CST which is larger than DWPF frit when not ground. Nominal ground CST was not yet available, therefore a similar CST ground previously in Savannah River National Laboratory (SRNL) was used. It was believed that this CST was over ground and that it would bound the impact of nominal CST on sludge slurry properties. Lab-scale simulations of the DWPF CPC were conducted using SB10 simulants with no, intermediate, and bounding levels of CST and MST. Tests included both the Sludge Receipt and Adjustment Tank (SRAT) and Slurry Mix Evaporator (SME) cycles. Simulations were performed at high and low acid stoichiometry. A demonstration of the extended CPC flowsheet was made that included streams from the site interim salt processing operations. A simulation using irradiated CST and MST was also completed. An extensive set of rheological measurements was made to search for potential adverse consequences of CST and MST and slurry rheology in the CPC. The SCIX CPC impact program was conducted in parallel with a program to evaluate the impact of SCIX on the final DWPF glass waste form and on the DWPF melter throughput. The studies must be considered together when evaluating the full impact of SCIX on DWPF. Due to the fact that the alternant flowsheet for DWPF has not been selected, this study did not consider the impact of proposed future alternative DWPF CPC flowsheets. The impact of the SCIX streams on DWPF processing using the selected flowsheet need to be considered as part of the technical baseline studies for coupled processing with the selected flowsheet. In addition, the downstream impact of aluminum dissolution on waste containing CST and MST has not yet been evaluated. The current baseline would not subject CST to the aluminum dissolution process and technical concerns with performing the dissolution with CST have been expressed. Should this option become feasible, the downstream impact should be considered. The main area of concern for DWPF from aluminum dissolution is an impact on rheology. The SCIX project is planning for SRNL to complete MST, CST, and sludge rheology testing to evaluate any expected changes. The impact of ground CST transport and flush water on the DWPF CPC feed tank (and potential need for decanting) has not been defined or studied.« less

Flowsheet Analysis of U-Pu Co-Crystallization Process as a New Reprocessing System

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

Shunji Homma; Jun-ichi Ishii; Jiro Koga

2006-07-01

A new fuel reprocessing system by U-Pu co-crystallization process is proposed and examined by flowsheet analysis. This reprocessing system is based on the fact that hexavalent plutonium in nitric acid solution is co-crystallized with uranyl nitrate, whereas it is not crystallized when uranyl nitrate does not exist in the solution. The system consists of five steps: dissolution of spent fuel, plutonium oxidation, U-Pu co-crystallization as a co-decontamination, re-dissolution of the crystals, and U re-crystallization as a U-Pu separation. The system requires a recycling of the mother liquor from the U-Pu co-crystallization step and the appropriate recycle ratio is determined bymore » flowsheet analysis such that the satisfactory decontamination is achieved. Further flowsheet study using four different compositions of LWR spent fuels demonstrates that the constant ratio of plutonium to uranium in mother liquor from the re-crystallization step is achieved for every composition by controlling the temperature. It is also demonstrated by comparing to the Purex process that the size of the plant based on the proposed system is significantly reduced. (authors)« less

Combinative application of pH-zone-refining and conventional high-speed counter-current chromatography for preparative separation of caged polyprenylated xanthones from gamboge.

PubMed

Xu, Min; Fu, Wenwei; Zhang, Baojun; Tan, Hongsheng; Xiu, Yanfeng; Xu, Hongxi

2016-02-01

An efficient method for the preparative separation of four structurally similar caged xanthones from the crude extracts of gamboge was established, which involves the combination of pH-zone-refining counter-current chromatography and conventional high-speed counter-current chromatography for the first time. pH-zone-refining counter-current chromatography was performed with the solvent system composed of n-hexane/ethyl acetate/methanol/water (7:3:8:2, v/v/v/v), where 0.1% trifluoroacetic acid was added to the upper organic stationary phase as a retainer and 0.03% triethylamine was added to the aqueous mobile phase as an eluter. From 3.157 g of the crude extract, 1.134 g of gambogic acid, 180.5 mg of gambogenic acid and 572.9 mg of a mixture of two other caged polyprenylated xanthones were obtained. The mixture was further separated by conventional high-speed counter-current chromatography with a solvent system composed of n-hexane/ethyl acetate/methanol/water (5:5:10:5, v/v/v/v) and n-hexane/methyl tert-butyl ether/acetonitrile/water (8:2:6:4,v/v/v/v), yielding 11.6 mg of isogambogenic acid and 10.4 mg of β-morellic acid from 218.0 mg of the mixture, respectively. The purities of all four of the compounds were over 95%, as determined by high-performance liquid chromatography, and the chemical structures of the four compounds were confirmed by electrospray ionization mass spectrometry and NMR spectroscopy. The combinative application of pH-zone-refining counter-current chromatography and conventional high-speed counter-current chromatography shows great advantages in isolating and enriching the caged polyprenylated xanthones. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation and purification of hydrolyzable tannin from Geranium wilfordii Maxim by reversed-phase and normal-phase high-speed counter-current chromatography.

PubMed

Liu, Dan; Su, Zhiguo; Wang, Changhai; Gu, Ming; Xing, Siliang

2010-08-01

Three hydrolyzable tannins, geraniin, corilagin and gallic acid, main active components of Geranium wilfordii Maxim, have been separated and purified in one-step by both reversed-phase and normal-phase high-speed counter-current chromatography. Gallic acid, corilagin and geraniin were purified from 70% aqueous acetone extract of G. wilfordii Maxim with solvent system n-hexane-ethyl acetate-methanol-acetic acid-water (1:10:0.2:0.2:20) by reversed-phase high-speed counter-current chromatography at purities of 94.2, 91.0 and 91.3%, at yields of 89.3, 82.9 and 91.7%, respectively. Gallic acid, corilagin and geraniin were purified with solvent system n-hexane-ethyl acetate-methanol-acetic acid-water (0.2:10:2:1:5) by normal-phase high-speed counter-current chromatography at purities of 85.9, 92.2 and 87.6%, at yields of 87.4, 94.6 and 94.3%, respectively. It was successful for both reversed-phase and normal-phase high-speed counter-current chromatography to separate high-polarity of low-molecular-weight substances.

Scaling of Counter-Current Imbibition Process in Low-Permeability Porous Media, TR-121

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

Kvoscek, A.R.; Zhou, D.; Jia, L.

2001-01-17

This project presents the recent work on imaging imbibition in low permeability porous media (diatomite) with X-ray completed tomography. The viscosity ratio between nonwetting and wetting fluids is varied over several orders of magnitude yielding different levels of imbibition performance. Also performed is mathematical analysis of counter-current imbibition processes and development of a modified scaling group incorporating the mobility ratio. This modified group is physically based and appears to improve scaling accuracy of countercurrent imbibition significantly.

Phytoplankton community structure and nitrogen nutrition in Leeuwin Current and coastal waters off the Gascoyne region of Western Australia

NASA Astrophysics Data System (ADS)

Hanson, Christine E.; Waite, Anya M.; Thompson, Peter A.; Pattiaratchi, Charitha B.

2007-04-01

Within the coastal waters of the eastern Indian Ocean adjacent to Western Australia, we tested the hypothesis that regenerated production (and, by inference, the microbial food web) would predominate in oligotrophic Leeuwin Current (LC) and offshore (OS) surface waters. Conversely, we expected that new production would be more important within the ˜5 times more productive shelf countercurrents (Ningaloo and Capes Currents; NC&CC) and the LC&OS deep chlorophyll maximum (DCM). Phytoplankton species composition and abundance were assessed using both light microscopy and chemotaxonomic methods, and isotopic nitrogen uptake experiments ( 15NO 3-, 15NH 4+) were performed at trace (0.05 μM) and saturating (5.0 μM) levels. Phytoplankton community structure was statistically distinct between LC&OS and countercurrent regions. Picoplankton (unicellular cyanobacteria and prochlorophytes) accounted for a mean of 55-65% of pigment biomass in LC&OS waters, with haptophytes as the other primary contributor (21-32%). Conversely, within countercurrent and shelf regions, diatoms (up to 22%) and haptophytes (up to 57%) were more abundant, although cyanobacteria still played an important role (up to 40% of pigment biomass). Absolute NO 3- uptake rates for all samples ranged between 0.5 and 7.1 nmol L -1 h -1, and in countercurrent waters were not significantly different at the surface (3.0±2.1 nmol L -1 h -1; mean±SD) compared to the DCM (2.7±2.3 nmol L -1 h -1). However, in LC&OS waters, rates were significantly lower at the surface (1.2±0.7 nmol L -1 h -1) than the DCM (3.9±2.5 nmol L -1 h -1; p=0.05). These values represent conservative estimates for the region due to methodological difficulties encountered with nitrogen uptake experiments in these oligotrophic waters. In contrast with the distinct community composition between different water types, mean estimates of the f-ratio were similar across sampling depths and water types: 0.17±0.07 at the surface and 0.16±0.06 at the DCM of shelf countercurrent waters, and 0.14±0.05 at the surface and 0.14±0.09 at the DCM of LC&OS waters. These results demonstrate the importance of ammonium-based production in both oligotrophic LC&OS waters and the more productive upwelling-influenced countercurrents. They also highlight the utility of chemotaxonomic methods in studying pelagic ecosystem structure along the Gascoyne region of Western Australia.

Diffusive shunting of gases and other molecules in the renal vasculature: physiological and evolutionary significance.

PubMed

Ngo, Jennifer P; Ow, Connie P C; Gardiner, Bruce S; Kar, Saptarshi; Pearson, James T; Smith, David W; Evans, Roger G

2016-11-01

Countercurrent systems have evolved in a variety of biological systems that allow transfer of heat, gases, and solutes. For example, in the renal medulla, the countercurrent arrangement of vascular and tubular elements facilitates the trapping of urea and other solutes in the inner medulla, which in turn enables the formation of concentrated urine. Arteries and veins in the cortex are also arranged in a countercurrent fashion, as are descending and ascending vasa recta in the medulla. For countercurrent diffusion to occur, barriers to diffusion must be small. This appears to be characteristic of larger vessels in the renal cortex. There must also be gradients in the concentration of molecules between afferent and efferent vessels, with the transport of molecules possible in either direction. Such gradients exist for oxygen in both the cortex and medulla, but there is little evidence that large gradients exist for other molecules such as carbon dioxide, nitric oxide, superoxide, hydrogen sulfide, and ammonia. There is some experimental evidence for arterial-to-venous (AV) oxygen shunting. Mathematical models also provide evidence for oxygen shunting in both the cortex and medulla. However, the quantitative significance of AV oxygen shunting remains a matter of controversy. Thus, whereas the countercurrent arrangement of vasa recta in the medulla appears to have evolved as a consequence of the evolution of Henle's loop, the evolutionary significance of the intimate countercurrent arrangement of blood vessels in the renal cortex remains an enigma. Copyright © 2016 the American Physiological Society.

DISSOLUTION OF PLUTONIUM METAL IN 8-10 M NITRIC ACID

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

Rudisill, T.; Pierce, R.

2012-02-21

The H-Canyon facility will be used to dissolve Pu metal for subsequent purification and conversion to plutonium dioxide (PuO{sub 2}) using Phase II of HB-Line. To support the new mission, the development of a Pu metal dissolution flowsheet which utilizes concentrated (8-10 M) nitric acid (HNO{sub 3}) solutions containing potassium fluoride (KF) is required. Dissolution of Pu metal in concentrated HNO{sub 3} is desired to eliminate the need to adjust the solution acidity prior to purification by anion exchange. The preferred flowsheet would use 8-10 M HNO{sub 3}, 0.015-0.07 M KF, and 0.5-1.0 g/L Gd to dissolve the Pu upmore » to 6.75 g/L. An alternate flowsheet would use 8-10 M HNO{sub 3}, 0.1-0.2 M KF, and 1-2 g/L B to dissolve the Pu. The targeted average Pu metal dissolution rate is 20 mg/min-cm{sup 2}, which is sufficient to dissolve a 'standard' 2250-g Pu metal button in 24 h. Plutonium metal dissolution rate measurements showed that if Gd is used as the nuclear poison, the optimum dissolution conditions occur in 10 M HNO{sub 3}, 0.04-0.05 M KF, and 0.5-1.0 g/L Gd at 112 to 116 C (boiling). These conditions will result in an estimated Pu metal dissolution rate of {approx}11-15 mg/min-cm{sup 2} and will result in dissolution times of 36-48 h for standard buttons. The recommended minimum and maximum KF concentrations are 0.03 M and 0.07 M, respectively. The maximum KF concentration is dictated by a potential room-temperature Pu-Gd-F precipitation issue at low Pu concentrations. The purpose of the experimental work described in this report was two-fold. Initially a series of screening experiments was performed to measure the dissolution rate of Pu metal as functions of the HNO{sub 3}, KF, and Gd or B concentrations. The objective of the screening tests was to propose optimized conditions for subsequent flowsheet demonstration tests. Based on the rate measurements, this study found that optimal dissolution conditions in solutions containing 0.5-1.0 g/L Gd occurred in 8-10 M HNO{sub 3} with 0.04-0.05 M KF at 112 to 116 C (boiling). The testing also showed that solutions containing 8-10 M HNO{sub 3}, 0.1-0.2 M KF, and 1-2 g/L B achieved acceptable dissolution rates in the same temperature range. To confirm that conditions identified by the dissolution rate measurements for solutions containing Gd or B can be used to dissolve Pu metal up to 6.75 g/L in the presence of Fe, demonstration experiments were performed using concentrations in the optimal ranges. In two of the demonstration experiments using Gd and in one experiment using B, the offgas generation during the dissolution was measured and samples were analyzed for H{sub 2}. The experimental methods used to perform the dissolution rate measurements and flowsheet demonstrations and a discussion of the results are presented.« less

Cost analysis of cassava cellulose utilization scenarios for ethanol production on flowsheet simulation platform.

PubMed

Zhang, Jian; Fang, Zhenhong; Deng, Hongbo; Zhang, Xiaoxi; Bao, Jie

2013-04-01

Cassava cellulose accounts for one quarter of cassava residues and its utilization is important for improving the efficiency and profit in commercial scale cassava ethanol industry. In this study, three scenarios of cassava cellulose utilization for ethanol production were experimentally tested under same conditions and equipment. Based on the experimental results, a rigorous flowsheet simulation model was established on Aspen plus platform and the cost of cellulase enzyme and steam energy in the three cases was calculated. The results show that the simultaneous co-saccharification of cassava starch/cellulose and ethanol fermentation process (Co-SSF) provided a cost effective option of cassava cellulose utilization for ethanol production, while the utilization of cassava cellulose from cassava ethanol fermentation residues was not economically sound. Comparing to the current fuel ethanol selling price, the Co-SSF process may provide an important choice for enhancing cassava ethanol production efficiency and profit in commercial scale. Copyright © 2013 Elsevier Ltd. All rights reserved.

Preparative isolation and purification of astaxanthin from the microalga Chlorococcum sp. by high-speed counter-current chromatography.

PubMed

Li, H B; Chen, F

2001-08-03

High-speed counter-current chromatography was applied to the isolation and purification of astaxanthin from microalgae. The crude astaxanthin was obtained by extraction with organic solvents after the astaxanthin esters were saponified. Preparative high-speed counter-current chromatography with a two-phase solvent system composed of n-hexane-ethyl acetate-ethanol-water (5:5:6.5:3, v/v) was successfully performed yielding astaxanthin at 97% purity from 250 mg of the crude extract in a one-step separation.

DWPF Simulant CPC Studies For SB8

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

Newell, J. D.

2013-09-25

Prior to processing a Sludge Batch (SB) in the Defense Waste Processing Facility (DWPF), flowsheet studies using simulants are performed. Typically, the flowsheet studies are conducted based on projected composition(s). The results from the flowsheet testing are used to 1) guide decisions during sludge batch preparation, 2) serve as a preliminary evaluation of potential processing issues, and 3) provide a basis to support the Shielded Cells qualification runs performed at the Savannah River National Laboratory (SRNL). SB8 was initially projected to be a combination of the Tank 40 heel (Sludge Batch 7b), Tank 13, Tank 12, and the Tank 51more » heel. In order to accelerate preparation of SB8, the decision was made to delay the oxalate-rich material from Tank 12 to a future sludge batch. SB8 simulant studies without Tank 12 were reported in a separate report.1 The data presented in this report will be useful when processing future sludge batches containing Tank 12. The wash endpoint target for SB8 was set at a significantly higher sodium concentration to allow acceptable glass compositions at the targeted waste loading. Four non-coupled tests were conducted using simulant representing Tank 40 at 110-146% of the Koopman Minimum Acid requirement. Hydrogen was generated during high acid stoichiometry (146% acid) SRAT testing up to 31% of the DWPF hydrogen limit. SME hydrogen generation reached 48% of of the DWPF limit for the high acid run. Two non-coupled tests were conducted using simulant representing Tank 51 at 110-146% of the Koopman Minimum Acid requirement. Hydrogen was generated during high acid stoichiometry SRAT testing up to 16% of the DWPF limit. SME hydrogen generation reached 49% of the DWPF limit for hydrogen in the SME for the high acid run. Simulant processing was successful using previously established antifoam addition strategy. Foaming during formic acid addition was not observed in any of the runs. Nitrite was destroyed in all runs and no N2O was detected during SME processing. Mercury behavior was consistent with that seen in previous SRAT runs. Mercury was stripped below the DWPF limit on 0.8 wt% for all runs. Rheology yield stress fell within or below the design basis of 1-5 Pa. The low acid Tank 40 run (106% acid stoichiometry) had the highest yield stress at 3.78 Pa.« less

pH-zone-refining elution-extrusion countercurrent chromatography: Separation of hydroxyanthraquinones from Cassiae semen.

PubMed

Bu, Zhisi; Lv, Liqiong; Li, Xingnuo; Chu, Chu; Tong, Shengqiang

2017-11-01

Seven hydroxyanthraquinones were successfully separated from the traditional Chinese medicinal herb Cassiae semen by conventional and pH-zone-refining countercurrent chromatography with an environmentally friendly biphasic solvent system, in which elution-extrusion mode was investigated for pH-zone-refining countercurrent chromatography for the first time. A two-phase solvent system composed of n-hexane/ethyl acetate/ethanol/water (5:3:4:4, v/v/v/v) was used for the conventional countercurrent chromatography while the same system with a different volume ratio n-hexane/ethyl acetate/ethanol/water (3:5:2:6, v/v/v/v) was used for pH-zone-refining countercurrent chromatography, in which 20 mmol/L of trifluoroacetic acid was added in the organic phase as a retainer and 15 mmol/L of ammonia was added to the aqueous phase as an eluter. A 400 mg crude sample could be well separated by pH-zone-refining countercurrent chromatography, yielding 53 mg of aurantio-obtusin, 40 mg of chryso-obtusin, 18 mg of obtusin, 24 mg of obtusifolin, 10 mg of emodin, and 105 mg of the mixture of chrysophanol and physcion with a purity of over 95.8, 95.7, 96.9, 93.5, 97.4, 77.1, and 19.8%, as determined by high-performance liquid chromatography. Furthermore, the difference in elution sequence between conventional and pH-zone-refining mode was observed and discussed. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Tank waste remediation system baseline tank waste inventory estimates for fiscal year 1995

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

Shelton, L.W., Westinghouse Hanford

1996-12-06

A set of tank-by-tank waste inventories is derived from historical waste models, flowsheet records, and analytical data to support the Tank Waste Remediation System flowsheet and retrieval sequence studies. Enabling assumptions and methodologies used to develop the inventories are discussed. These provisional inventories conform to previously established baseline inventories and are meant to serve as an interim basis until standardized inventory estimates are made available.

Next-generation purex flowsheets with acetohydroxamic acid as complexant for FBR and thermal-fuel reprocessing

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

Kumar, Shekhar; Koganti, S.B.

2008-07-01

Acetohydroxamic acid (AHA) is a novel complexant for recycle of nuclear-fuel materials. It can be used in ordinary centrifugal extractors, eliminating the need for electro-redox equipment or complex maintenance requirements in a remotely maintained hot cell. In this work, the effect of AHA on Pu(IV) distribution ratios in 30% TBP system was quantified, modeled, and integrated in SIMPSEX code. Two sets of batch experiments involving macro Pu concentrations (conducted at IGCAR) and one high-Pu flowsheet (literature) were simulated for AHA based U-Pu separation. Based on the simulation and validation results, AHA based next-generation reprocessing flowsheets are proposed for co-processing basedmore » FBR and thermal-fuel reprocessing as well as evaporator-less macro-level Pu concentration process required for MOX fuel fabrication. Utilization of AHA results in significant simplification in plant design and simpler technology implementations with significant cost savings. (authors)« less

Metallurgical Plant Optimization Through the use of Flowsheet Simulation Modelling

NASA Astrophysics Data System (ADS)

Kennedy, Mark William

Modern metallurgical plants typically have complex flowsheets and operate on a continuous basis. Real time interactions within such processes can be complex and the impacts of streams such as recycles on process efficiency and stability can be highly unexpected prior to actual operation. Current desktop computing power, combined with state-of-the-art flowsheet simulation software like Metsim, allow for thorough analysis of designs to explore the interaction between operating rate, heat and mass balances and in particular the potential negative impact of recycles. Using plant information systems, it is possible to combine real plant data with simple steady state models, using dynamic data exchange links to allow for near real time de-bottlenecking of operations. Accurate analytical results can also be combined with detailed unit operations models to allow for feed-forward model-based-control. This paper will explore some examples of the application of Metsim to real world engineering and plant operational issues.

High Temperature Heat Exchanger Design and Fabrication for Systems with Large Pressure Differentials

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

Chordia, Lalit; Portnoff, Marc A.; Green, Ed

The project’s main purpose was to design, build and test a compact heat exchanger for supercritical carbon dioxide (sCO 2) power cycle recuperators. The compact recuperator is required to operate at high temperature and high pressure differentials, 169 bar (~2,500 psi), between streams of sCO 2. Additional project tasks included building a hot air-to-sCO 2 Heater heat exchanger (HX) and design, build and operate a test loop to characterize the recuperator and heater heat exchangers. A novel counter-current microtube recuperator was built to meet the high temperature high differential pressure criteria and tested. The compact HX design also incorporated amore » number of features that optimize material use, improved reliability and reduced cost. The air-to-sCO 2 Heater HX utilized a cross flow, counter-current, micro-tubular design. This compact HX design was incorporated into the test loop and exceeded design expectations. The test loop design to characterize the prototype Brayton power cycle HXs was assembled, commissioned and operated during the program. Both the prototype recuperator and Heater HXs were characterized. Measured results for the recuperator confirmed the predictions of the heat transfer models developed during the project. Heater HX data analysis is ongoing.« less

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

KIRKBRIDE, R.A.

The Tank Waste Remediation System Operation and Utilization Plan updates the operating scenario and plans for the delivery of feed to BNFL Inc., retrieval of waste from single-shell tanks, and the overall process flowsheets for Phases I and II of the privatization of the Tank Waste Remediation System. The plans and flowsheets are updated with the most recent tank-by-tank inventory and sludge washing data. Sensitivity cases were run to evaluate the impact or benefits of proposed changes to the BNFL Inc. contract and to evaluate a risk-based SST retrieval strategy.

How-to-Do-It: Countercurrent Heat Exchange in Vertebrate Limbs.

ERIC Educational Resources Information Center

Franklin, George B.; Plakke, Ronald K.

1988-01-01

Describes principals of physics that are manifested in simple biological systems of heat conservation structures. Outlines materials needed, data collection, analysis, and discussion questions for construction and operation of two models, one that is a countercurrent heat exchange model and one that is not. (RT)

New Adsorption Methods.

ERIC Educational Resources Information Center

Wankat, Phillip C.

1984-01-01

Discusses a simple method for following the movement of a solute in an adsorption or ion exchange system. This movement is used to study a variety of operational methods, including continuous flow and pulsed flow counter-current operations and simulated counter-current systems. Effect of changing thermodynamic variables is also considered. (JM)

Counter-current carbon dioxide purification of partially deacylated sunflower oil

USDA-ARS?s Scientific Manuscript database

High oleic sunflower oil was partially deacylated by propanolysis to produce a mixture of diglycerides and triglycerides. To remove by-product fatty acid propyl esters (FAPEs) from this reaction mixture, a liquid carbon dioxide (L-CO2) counter-current fractionation method was developed. The fracti...

Elution-extrusion counter-current chromatography for the separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix.

PubMed

Chu, Chu; Zhang, Shidi; Tong, Shengqiang; Li, Xingnuo; Li, Qingyong; Yan, Jizhong

2015-09-01

In this work, a simple and efficient protocol for the rapid separation of two pairs of isomeric monoterpenes from Paeoniae Alba Radix was developed by combining macroporous resin and elution-extrusion counter-current chromatography. The crude extract was firstly subjected to a D101 macroporous resin column eluted with water and a series of different concentrations of ethanol. Then, effluents of 30 and 95% ethanol were collected as sample 1 and sample 2 for further counter-current chromatography purification. Finally, a pair of isomers, 96 mg of compound 1 and 48 mg of compound 2 with purities of 91.1 and 96.2%, respectively, was isolated from 200 mg of sample 1. The other pair of isomers, 14 mg of compound 3 and 8 mg of compound 4 with purities of 93.6 and 88.9%, respectively, was isolated from 48 mg of sample 2. Their purities were analyzed by high-performance liquid chromatography, and their chemical structures were identified by mass spectrometry and (1) H NMR spectroscopy. Compared to a normal counter-current chromatography separation, the separation time and solvent consumption of elution-extrusion counter-current chromatography were reduced while the resolutions were still good. The established protocol is promising for the separation of natural products with great disparity of content in herbal medicines. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A numerical world ocean general circulation model Part I. Basic design and barotropic experiment

NASA Astrophysics Data System (ADS)

Han, Young-June

1984-08-01

A new six-layer world ocean general circulation model based on the primitive system of equations is described in detail and its performance in the case of a homogeneous ocean is described. These test integrations show that the model is capable of reproducing the observed mean barotropic or vertically-integrated transport, as well as the seasonal variability of the major ocean gyres. The surface currents, however, are dominated by the Ekman transport, and such non-linear features as the western boundary currents and the equatorial countercurrents are poorly represented. The abyssal boundary countercurrents are also absent due to the lack of thermohaline forcing. The most conspicuous effect of the bottom topography on a homogeneous ocean is seen in the Southern ocean where the calculated Antarctic circumpolar transport through the Drake passage ( ≈ 10 Sv, with bathymetry included) greatly underestimates the observed transport (≈ 100 Sv).

New analytical spiral tube assembly for separation of proteins by counter-current chromatography.

PubMed

Ma, Xiaofeng; Ito, Yoichiro

2015-07-31

A new spiral column assembly for analytical separation by counter-current chromatography is described. The column is made from a plastic spiral tube support which has 12 interwoven spiral grooves. The PTFE tubing of 1.6mm ID was first flattened by extruding through a narrow slit and inserted into the grooves to make 5 spiral layers with about 60ml capacity. The performance of the spiral column assembly was tested with separation of three stable protein samples including cytochrome C, myoglobin and lysozyme in a polymer phase system composed of polyethylene glycol 1000 and dibasic potassium phosphate each at 12.5% (w/w) in water. At 2ml/min, three protein samples were well resolved in 1h. The separation time may be further shortened by application of higher revolution speed and flow rate by improving the strength of the spiral tube support in the future. Published by Elsevier B.V.

Purification of Proteins From Cell-Culture Medium or Cell-Lysate by High-Speed Counter-Current Chromatography Using Cross-Axis Coil Planet Centrifuge

PubMed Central

Shibusawa, Yoichi; Ito, Yoichiro

2014-01-01

This review describes protein purifications from cell culture medium or cell-lysate by high speed counter-current chromatography using the cross-axis coil planet centrifuge. Purifications were performed using aqueous two phase systems composed of polyethylene glycols and dextrans. PMID:25360182

SIMULATION OF NON-AZEOTROPIC REFRIGERANT MIXTURES FOR USE IN A DUAL-CIRCUIT REFRIGERATOR/FREEZER WITH COUNTERCURRENT HEAT EXCHANGES

EPA Science Inventory

The paper discusses a refrigerator/freezer (RF) system that has two complete and independent refrigeration cycles for the two compartments. It uses a non-azeotropic refrigerant mixture (NARM) in each cycle and countercurrent heat exchangers throughout. This RF is housed in a stan...

Application of off-line two-dimensional high-performance countercurrent chromatography on the chloroform-soluble extract of Cuscuta auralis seeds.

PubMed

Rho, Taewoong; Yoon, Kee Dong

2018-05-01

In this study, the chloroform-soluble extract of Cuscuta auralis was separated successfully using off-line two-dimensional high-performance countercurrent chromatography, yielding a γ-pyrone, two alkaloids, a flavonoid, and four lignans. The first-dimensional countercurrent separation using a methylene chloride/methanol/water (11:6:5, v/v/v) system yielded three subfractions (fractions I-III). The second-dimensional countercurrent separations, conducted on fractions I-III using n-hexane/ethyl acetate/methanol/water/acetic acid (5:5:5:5:0, 3:7:3:7:0, and 1:9:1:9:0.01, v/v/v/v/v) systems, gave maltol (1), (-)-(13S)-cuscutamine (2), (+)-(13R)-cuscutamine (3), (+)-pinoresinol (4), (+)-epipinoresinol (5), kaempferol (6), piperitol (7), and (9R)-hydroxy-d-sesamin (8). To the best of our knowledge, maltol was identified for the first time in Cuscuta species. Furthermore, this report details the first full assignment of spectroscopic data of two cuscutamine epimers, (-)-(13S)-cuscutamine and (+)-(13R)-cuscutamine. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Candidate space processing techniques for biomaterials other than preparative electrophoresis

NASA Technical Reports Server (NTRS)

Brooks, D. E.

1976-01-01

The advantages of performing the partition and countercurrent distribution (CCD) of cells in phase separated aqueous polymer systems under reduced gravity were assessed. Other possible applications considered for the space processing program include the freezing front separation of cells, adsorption of cells at the air-water interface, and the macrophage electrophoretic mobility test for cancer.

Structure and Variability of the Mesoscale Circulation in the Caribbean sea as Deduced From Satellite Altimetry

DTIC Science & Technology

1998-06-01

countercurrent along Costa Rica and Panama, which ends on the Colombian coast. This flow is usually called the Darien Countercurrent. Also, a counter flow...Marine Geology , vol. 68,25-52, 1985. Le Traon, P. Y., P. Gaspar, F. Bouyssel, and H. Makhmara, Using Topex / Poseidon Data to Enhance ERS-1 Data

Recovery of butanol by counter-current carbon dioxide fractionation with its potential application to butanol fermentation

USDA-ARS?s Scientific Manuscript database

A counter-current CO2 fractionation method was studied as a means to recover butanol (also known as 1-butanol or n-butanol) and other compounds that are typically obtained from biobutanol fermentation broth from aqueous solutions. The influence of operating parameters, such as solvent-to-feed ratio,...

Separation and characterisation of five polar herbicides using countercurrent chromatography with detection by negative ion electrospray ionisation mass spectrometry.

PubMed

Kidwell, H; Jones, J J; Games, D E

2001-01-01

Five polar herbicides were separated and characterised using high-speed analytical countercurrent chromatography (HSACCC) in conjunction with online electrospray mass spectrometry (ESI-MS). The countercurrent chromatography used a standard isocratic biphasic solvent system of hexane/ethyl acetate/methanol/water in reverse phase to effect the separation of these five environmentally important compounds. The chromatograph was coupled to a triple quadrupole mass spectrometer via a standard electrospray liquid chromatography interface that was able to give mass spectra in negative ion mode of each compound. Limits of detection are reported for this series of compounds along with representative negative ion ESI-MS data and calibrations for the separation. Copyright 2001 John Wiley & Sons, Ltd.

Counter-current convection in a volcanic conduit

NASA Astrophysics Data System (ADS)

Fowler, A. C.; Robinson, Marguerite

2018-05-01

Volcanoes of Strombolian type are able to maintain their semi-permanent eruptive states through the constant convective recycling of magma within the conduit leading from the magma chamber. In this paper we study the form of this convection using an analytic model of degassing two-phase flow in a vertical channel. We provide solutions for the flow at small Grashof and large Prandtl numbers, and we suggest that permanent steady-state counter-current convection is only possible if an initial bubbly counter-current flow undergoes a régime transition to a churn-turbulent flow. We also suggest that the magma in the chamber must be under-pressured in order for the flow to be maintained, and that this compromises the assumed form of the flow.

Geological and technological evaluation of gold-bearing mineral material after photo-electrochemical activation leaching

NASA Astrophysics Data System (ADS)

Manzyrev, DV

2017-02-01

The paper reports the lab test results on simulation of heap leaching of unoxidized rebellious ore extracted from deep levels of Pogromnoe open pit mine, with different flowsheets and photo-electrochemically activated solutions. It has been found that pre-treatment of rebellious ore particles -10 mm in size by photo-electrochemically activated solutions at the stage preceding agglomeration with the use of rich cyanide solutions enhances gold recovery by 6%.

A flowsheet model of a well-mixed fluidized bed dryer: Applications in controllability assessment and optimization

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

Langrish, T.A.G.; Harvey, A.C.

2000-01-01

A model of a well-mixed fluidized-bed dryer within a process flowsheeting package (SPEEDUP{trademark}) has been developed and applied to a parameter sensitivity study, a steady-state controllability analysis and an optimization study. This approach is more general and would be more easily applied to a complex flowsheet than one which relied on stand-alone dryer modeling packages. The simulation has shown that industrial data may be fitted to the model outputs with sensible values of unknown parameters. For this case study, the parameter sensitivity study has found that the heat loss from the dryer and the critical moisture content of the materialmore » have the greatest impact on the dryer operation at the current operating point. An optimization study has demonstrated the dominant effect of the heat loss from the dryer on the current operating cost and the current operating conditions, and substantial cost savings (around 50%) could be achieved with a well-insulated and airtight dryer, for the specific case studied here.« less

Small-scale and large-scale testing of photo-electrochemically activated leaching technology in Aprelkovo and Delmachik Mines

NASA Astrophysics Data System (ADS)

Sekisov, AG; Lavrov, AYu; Rubtsov, YuI

2017-02-01

The paper gives a description of tests and trials of the technology of heap gold leaching from rebellious ore in Aprelkovo and Delmachik Mines. Efficiency of leaching flowsheets with the stage-wise use of activated solutions of different reagents, including active forms of oxygen, is evaluated. Carbonate-peroxide solutions are used at the first stage of leaching to oxidize sulfide and sulfide-arsenide ore minerals to recover iron and copper from them. The second stage leaching uses active cyanide solutions to leach encapsulated and disperse gold and silver.

Flowsheets and source terms for radioactive waste projections

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

Forsberg, C.W.

1985-03-01

Flowsheets and source terms used to generate radioactive waste projections in the Integrated Data Base (IDB) Program are given. Volumes of each waste type generated per unit product throughput have been determined for the following facilities: uranium mining, UF/sub 6/ conversion, uranium enrichment, fuel fabrication, boiling-water reactors (BWRs), pressurized-water reactors (PWRs), and fuel reprocessing. Source terms for DOE/defense wastes have been developed. Expected wastes from typical decommissioning operations for each facility type have been determined. All wastes are also characterized by isotopic composition at time of generation and by general chemical composition. 70 references, 21 figures, 53 tables.

Counter-current carbon dioxide extraction of fat from soy skim

USDA-ARS?s Scientific Manuscript database

This research aims to investigate the use of counter-current carbon dioxide extraction method as a means to reduce residual fat in soy skim after the enzyme-assisted aqueous extraction of soybeans. Extractions with liquid CO2 at 25°C and 10.34 MPa and supercritical CO2 at 50°C and 25.16 MPa are comp...

Isolation of a furan fatty acid from Hevea brasiliensis latex employing the combined use of pH-zone-refining and conventional countercurrent chromatography.

PubMed

Englert, Michael; Ulms, Kerstin; Wendlinger, Christine; Vetter, Walter

2016-02-01

Furan fatty acids are valuable and bioactive minor fatty acids that usually contribute <0.1% to the fatty acid content of food samples. Their biological role still remains unclear as authentic furan fatty acid standards are not readily available and thorough experimental studies verifying the relevance of furan fatty acids are thus virtually impossible. An efficient protocol for the isolation of the furan fatty acid 9-(3-methyl-5-pentylfuran-2-yl)-nonanoic acid from hydrolyzed and centrifuged latex of Hevea brasiliensis was developed using countercurrent chromatography. A first run using pH-zone-refining countercurrent chromatography provided 48.4 mg of 9-(3-methyl-5-pentylfuran-2-yl)-nonanoic acid from 210 mg latex extract in a purity of 95%. The purity was increased to 99% by means of one second run in conventional countercurrent chromatography mode. The Structure and purity of 9-(3-methyl-5-pentylfuran-2-yl)-nonanoic acid were determined by gas chromatography coupled to mass spectrometry and (1)H and (13)C NMR spectroscopy. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Application of ultrasound counter currentextraction in patent of traditional Chinese medicine].

PubMed

Miao, Yan-ni; Wu, Bin; Yue, Xue-lian

2015-07-01

The patent information of ultrasound countercurrent extraction used in traditional Chinese medicine was analyzed in this paper by the samples from Derwent World Patent Database (DWPI) and the Chinese Patent Abstracts Database (CNABS). The application of ultrasound countercurrent was discussed with the patent applicant,the amount of the annual distribution, and the pharmaceutical raw materials and other aspects. While the technical parameters published in the patent was deeply analyzed, such as material crushing, extraction solvent, extraction time and temperature, extraction equipment and ultrasonic frequency. Thought above research, various technical parameters of ultrasound countercurrent extraction used in traditional Chinese was summarize. The analysis conclusion of the paper can be used in discovering the technical advantages, optimizing extraction conditions, and providing a reference to extraction technological innovation of traditional Chinese medicine.

SLUDGE BATCH 6/TANK 40 SIMULANT CHEMICAL PROCESS CELL SIMULATIONS

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

Koopman, David

2010-04-28

Phase III simulant flowsheet testing was completed using the latest composition estimates for SB6/Tank 40 feed to DWPF. The goals of the testing were to determine reasonable operating conditions and assumptions for the startup of SB6 processing in the DWPF. Testing covered the region from 102-159% of the current DWPF stoichiometric acid equation. Nitrite ion concentration was reduced to 90 mg/kg in the SRAT product of the lowest acid run. The 159% acid run reached 60% of the DWPF Sludge Receipt and Adjustment Tank (SRAT) limit of 0.65 lb H2/hr, and then sporadically exceeded the DWPF Slurry Mix Evaporator (SME)more » limit of 0.223 lb H2/hr. Hydrogen generation rates peaked at 112% of the SME limit, but higher than targeted wt% total solids levels may have been partially responsible for rates seen. A stoichiometric factor of 120% met both objectives. A processing window for SB6 exists from 102% to something close to 159% based on the simulant results. An initial recommendation for SB6 processing is at 115-120% of the current DWPF stoichiometric acid equation. The addition of simulated Actinide Removal Process (ARP) and Modular Caustic Side Solvent Extraction Unit (MCU) streams to the SRAT cycle had no apparent impact on the preferred stoichiometric factor. Hydrogen generation occurred continuously after acid addition in three of the four tests. The three runs at 120%, 118.4% with ARP/MCU, and 159% stoichiometry were all still producing around 0.1 lb hydrogen/hr at DWPF scale after 36 hours of boiling in the SRAT. The 120% acid run reached 23% of the SRAT limit and 37% of the SME limit. Conversely, nitrous oxide generation was subdued compared to previous sludge batches, staying below 29 lb/hr in all four tests or about a fourth as much as in comparable SB4 testing. Two processing issues, identified during SB6 Phase II flowsheet testing and qualification simulant testing, were monitored during Phase III. Mercury material balance closure was impacted by acid stoichiometry, and significant mercury was not accounted for in the highest acid run. Coalescence of elemental mercury droplets in the mercury water wash tank (MWWT) appeared to degrade with increasing stoichiometry. Observations were made of mercury scale formation in the SRAT condenser and MWWT. A tacky mercury amalgam with Rh, Pd, and Cu, plus some Ru and Ca formed on the impeller at 159% acid. It contained a significant fraction of the available Pd, Cu, and Rh as well as about 25% of the total mercury charged. Free (elemental) mercury was found in all of the SME products. Ammonia scrubbers were used during the tests to capture off-gas ammonia for material balance purposes. Significant ammonium ion formation was again observed during the SRAT cycle, and ammonia gas entered the off-gas as the pH rose during boiling. Ammonium ion production was lower than in the SB6 Phase II and the qualification simulant testing. Similar ammonium ion formation was seen in the ARP/MCU simulation as in the 120% flowsheet run. A slightly higher pH caused most of the ammonium to vaporize and collect in the ammonia scrubber reflux solution. Two periods of foaminess were noted. Neither required additional antifoam to control the foam growth. A steady foam layer formed during reflux in the 120% acid run. It was about an inch thick, but was 2-3 times more volume of bubbles than is typically seen during reflux. A similar foam layer also was seen during caustic boiling of the simulant during the ARP addition. While frequently seen with the radioactive sludge, foaminess during caustic boiling with simulants has been relatively rare. Two further flowsheet tests were performed and will be documented separately. One test was to evaluate the impact of process conditions that match current DWPF operation (lower rates). The second test was to evaluate the impact of SRAT/SME processing on the rheology of a modified Phase III simulant that had been made five times more viscous using ultrasonication.« less

Removal of cesium from simulated liquid waste with countercurrent two-stage adsorption followed by microfiltration.

PubMed

Han, Fei; Zhang, Guang-Hui; Gu, Ping

2012-07-30

Copper ferrocyanide (CuFC) was used as an adsorbent to remove cesium. Jar test results showed that the adsorption capacity of CuFC was better than that of potassium zinc hexacyanoferrate. Lab-scale tests were performed by an adsorption-microfiltration process, and the mean decontamination factor (DF) was 463 when the initial cesium concentration was 101.3μg/L, the dosage of CuFC was 40mg/L and the adsorption time was 20min. The cesium concentration in the effluent continuously decreased with the operation time, which indicated that the used adsorbent retained its adsorption capacity. To use this capacity, experiments on a countercurrent two-stage adsorption (CTA)-microfiltration (MF) process were carried out with CuFC adsorption combined with membrane separation. A calculation method for determining the cesium concentration in the effluent was given, and batch tests in a pressure cup were performed to verify the calculated method. The results showed that the experimental values fitted well with the calculated values in the CTA-MF process. The mean DF was 1123 when the dilution factor was 0.4, the initial cesium concentration was 98.75μg/L and the dosage of CuFC and adsorption time were the same as those used in the lab-scale test. The DF obtained by CTA-MF process was more than three times higher than the single-stage adsorption in the jar test. Copyright © 2012 Elsevier B.V. All rights reserved.

Significant volume reduction of tank waste by selective crystallization: 1994 Annual report

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

Herting, D.L.; Lunsford, T.R.

1994-09-27

The objective of this technology task plan is to develop and demonstrate a scaleable process of reclaim sodium nitrate (NaNO{sub 3}) from Hanford waste tanks as a clean nonradioactive salt. The purpose of the so-called Clean Salt Process is to reduce the volume of low level waste glass by as much as 70%. During the reporting period of October 1, 1993, through May 31, 1994, progress was made on four fronts -- laboratory studies, surrogate waste compositions, contracting for university research, and flowsheet development and modeling. In the laboratory, experiments with simulated waste were done to explore the effects ofmore » crystallization parameters on the size and crystal habit of product NaNO{sub 3} crystals. Data were obtained to allows prediction of decontamination factor as a function of solid/liquid separation parameters. Experiments with actual waste from tank 101-SY were done to determine the extent of contaminant occlusions in NaNO{sub 3} crystals. In preparation for defining surrogate waste compositions, single shell tanks were categorized according to the weight percent NaNO{sub 3} in each tank. A detailed process flowsheet and computer model were created using the ASPENPlus steady state process simulator. This is the same program being used by the Tank Waste Remediation System (TWRS) program for their waste pretreatment and disposal projections. Therefore, evaluations can be made of the effect of the Clean Salt Process on the low level waste volume and composition resulting from the TWRS baseline flowsheet. Calculations, using the same assumptions as used for the TWRS baseline where applicable indicate that the number of low level glass vaults would be reduced from 44 to 16 if the Clean Salt Process were incorporated into the baseline flowsheet.« less

Validation and Refinement of a Pain Information Model from EHR Flowsheet Data.

PubMed

Westra, Bonnie L; Johnson, Steven G; Ali, Samira; Bavuso, Karen M; Cruz, Christopher A; Collins, Sarah; Furukawa, Meg; Hook, Mary L; LaFlamme, Anne; Lytle, Kay; Pruinelli, Lisiane; Rajchel, Tari; Settergren, Theresa Tess; Westman, Kathryn F; Whittenburg, Luann

2018-01-01

Secondary use of electronic health record (EHR) data can reduce costs of research and quality reporting. However, EHR data must be consistent within and across organizations. Flowsheet data provide a rich source of interprofessional data and represents a high volume of documentation; however, content is not standardized. Health care organizations design and implement customized content for different care areas creating duplicative data that is noncomparable. In a prior study, 10 information models (IMs) were derived from an EHR that included 2.4 million patients. There was a need to evaluate the generalizability of the models across organizations. The pain IM was selected for evaluation and refinement because pain is a commonly occurring problem associated with high costs for pain management. The purpose of our study was to validate and further refine a pain IM from EHR flowsheet data that standardizes pain concepts, definitions, and associated value sets for assessments, goals, interventions, and outcomes. A retrospective observational study was conducted using an iterative consensus-based approach to map, analyze, and evaluate data from 10 organizations. The aggregated metadata from the EHRs of 8 large health care organizations and the design build in 2 additional organizations represented flowsheet data from 6.6 million patients, 27 million encounters, and 683 million observations. The final pain IM has 30 concepts, 4 panels (classes), and 396 value set items. Results are built on Logical Observation Identifiers Names and Codes (LOINC) pain assessment terms and extend the need for additional terms to support interoperability. The resulting pain IM is a consensus model based on actual EHR documentation in the participating health systems. The IM captures the most important concepts related to pain. Schattauer GmbH Stuttgart.

The dispersal of the Amazon's water

NASA Technical Reports Server (NTRS)

Muller-Karger, Frank E.; Mcclain, Charles R.; Richardson, Philip L.

1988-01-01

New information obtained with NASA's Coastal Zone Color Scanner and with drifting buoys reveals that the discharge of the Amazon is carried offshore around a retroflection of the North Brazil Current and into the North Equatorial Countercurrent towards Africa between June and January each year. From about February to May, the countercurrent and the retroflection weaken or vanish, and Amazon water flows northwestward toward the Caribbean Sea.

Reacting flow studies in a dump combustor: Enhanced volumetric heat release rates and flame anchorability

NASA Astrophysics Data System (ADS)

Behrens, Alison Anne

Reacting flow studies in a novel dump combustor facility focused on increasing volumetric heat release rates, under stable burning conditions, and understanding the physical mechanisms governing flame anchoring in an effort to extend range and maneuverability of compact, low drag, air-breathing engines. Countercurrent shear flow was enhanced within the combustor as the primary control variable. Experiments were performed burning premixed JP10/air and methane/air in a dump combustor using reacting flow particle image velocimetry (PIV) and chemiluminescence as the primary diagnostics. Stable combustion studies burning lean mixtures of JP10/air aimed to increase volumetric heat release rates through the implementation of countercurrent shear control. Countercurrent shear flow was produced by creating a suction flow from a low pressure cavity connected to the dump combustor via a gap directly below the trailing edge. Chemiluminescence measurements showed that enhancing countercurrent shear within the combustor doubles volumetric heat release rates. PIV measurements indicate that counterflow acts to increase turbulent kinetic energy while maintaining constant strain rates. This acts to increase flame surface area through flame wrinkling without disrupting the integrity of the flame. Flame anchorability is one of the most important fundamental aspects to understand when trying to enhance turbulent combustion in a high-speed engine without increasing drag. Studies burning methane/air mixtures used reacting flow PIV to study flame anchoring. The operating point with the most stable flame anchor exhibited a correspondingly strong enthalpy flux of products into reactants via a single coherent structure positioned downstream of the step. However, the feature producing a strong flame anchor, i.e. a single coherent structure, also is responsible for combustion instabilities, therefore making this operating point undesirable. Counterflow control was found to create the best flow features for stable, robust, compact combustion. Enhancing countercurrent shear flow within a dump combustor enhances burning rates, provides a consistent pump of reaction-initiating combustion products required for sustained combustion, while maintaining flow three dimensionality needed to disrupt combustion instabilities. Future studies will focus on geometric and control scenarios that further reduce drag penalties while creating these same flow features found with countercurrent shear thus producing robust operating points.

Inert gas clearance from tissue by co-currently and counter-currently arranged microvessels

PubMed Central

Lu, Y.; Michel, C. C.

2012-01-01

To elucidate the clearance of dissolved inert gas from tissues, we have developed numerical models of gas transport in a cylindrical block of tissue supplied by one or two capillaries. With two capillaries, attention is given to the effects of co-current and counter-current flow on tissue gas clearance. Clearance by counter-current flow is compared with clearance by a single capillary or by two co-currently arranged capillaries. Effects of the blood velocity, solubility, and diffusivity of the gas in the tissue are investigated using parameters with physiological values. It is found that under the conditions investigated, almost identical clearances are achieved by a single capillary as by a co-current pair when the total flow per tissue volume in each unit is the same (i.e., flow velocity in the single capillary is twice that in each co-current vessel). For both co-current and counter-current arrangements, approximate linear relations exist between the tissue gas clearance rate and tissue blood perfusion rate. However, the counter-current arrangement of capillaries results in less-efficient clearance of the inert gas from tissues. Furthermore, this difference in efficiency increases at higher blood flow rates. At a given blood flow, the simple conduction-capacitance model, which has been used to estimate tissue blood perfusion rate from inert gas clearance, underestimates gas clearance rates predicted by the numerical models for single vessel or for two vessels with co-current flow. This difference is accounted for in discussion, which also considers the choice of parameters and possible effects of microvascular architecture on the interpretation of tissue inert gas clearance. PMID:22604885

Radiolarian indicators of El Nino and anti-El Nino events in Holocene sediments of Santa Barbara basin

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

Weinheimer, A.L.

Radiolarian distributions and physical oceanographic data from the Santa Barbara basin indicate the following. Strong anti-El Nino periods can be characterized by (1) intermediate radiolarian density, (2) high percentage of transition-central radiolarian fauna, and (3) low percentage and number of warm-water radiolarian fauna. This distribution pattern is attributed to strong wind-driven upwelling and reduced northward transport by the California Countercurrent during anti-El Nino periods. Strong El Nino periods are typically (1) high in radiolarian density, and (2) low in percentage but high in number of warm-water fauna. This distribution is attributed to reduced wind-driven upwelling, enhanced northward countercurrent transport, andmore » geostrophic doming of the cold-water masses in the shear zone between the California Current and California Countercurrent.« less

Preparative isolation of a cytotoxic principle of a forest mushroom Suillus luteus by sodium dodecyl sulfate based "salting-in" countercurrent chromatography.

PubMed

Yang, Zhi; Hu, Xueqian; Wu, Shihua

2016-02-01

In the course of screening new anticancer natural products, an edible forest mushroom Suillus luteus (L. Ex Franch). Gray was found to have potent cytotoxicity against several human cancer cells. However, the lipophilic sample made some countercurrent chromatography solvent systems emulsify, which caused difficulties in the separation of its cytotoxic components. Here, we found that the addition of an organic salt sodium dodecyl sulfate could efficiently shorten the settling time of the mushroom sample solutions by eliminating the emulsification of two-phase solvent systems. Moreover, we found that sodium dodecyl sulfate could play a new "salting-in" role and made the partition coefficients of the solutes decrease with the increased concentrations. Thus, a sodium dodecyl sulfate based salting-in countercurrent chromatography method has been successfully established for the first time for preparative isolation of a cytotoxic principle of the mushroom. The active component was identified as isosuillin. Whole results indicated that sodium dodecyl sulfate could be used as an efficient salting-in reagent for two-phase solvent system selection and targeted countercurrent chromatography isolation. It is very useful for current natural products isolation and drug discovery. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Validation of a Mechanistic Model for Non-Invasive Study of Ecological Energetics in an Endangered Wading Bird with Counter-Current Heat Exchange in its Legs.

PubMed

Fitzpatrick, Megan J; Mathewson, Paul D; Porter, Warren P

2015-01-01

Mechanistic models provide a powerful, minimally invasive tool for gaining a deeper understanding of the ecology of animals across geographic space and time. In this paper, we modified and validated the accuracy of the mechanistic model Niche Mapper for simulating heat exchanges of animals with counter-current heat exchange mechanisms in their legs and animals that wade in water. We then used Niche Mapper to explore the effects of wading and counter-current heat exchange on the energy expenditures of Whooping Cranes, a long-legged wading bird. We validated model accuracy against the energy expenditure of two captive Whooping Cranes measured using the doubly-labeled water method and time energy budgets. Energy expenditure values modeled by Niche Mapper were similar to values measured by the doubly-labeled water method and values estimated from time-energy budgets. Future studies will be able to use Niche Mapper as a non-invasive tool to explore energy-based limits to the fundamental niche of Whooping Cranes and apply this knowledge to management decisions. Basic questions about the importance of counter-current exchange and wading to animal physiological tolerances can also now be explored with the model.

Validation of a Mechanistic Model for Non-Invasive Study of Ecological Energetics in an Endangered Wading Bird with Counter-Current Heat Exchange in its Legs

PubMed Central

Fitzpatrick, Megan J.; Mathewson, Paul D.; Porter, Warren P.

2015-01-01

Mechanistic models provide a powerful, minimally invasive tool for gaining a deeper understanding of the ecology of animals across geographic space and time. In this paper, we modified and validated the accuracy of the mechanistic model Niche Mapper for simulating heat exchanges of animals with counter-current heat exchange mechanisms in their legs and animals that wade in water. We then used Niche Mapper to explore the effects of wading and counter-current heat exchange on the energy expenditures of Whooping Cranes, a long-legged wading bird. We validated model accuracy against the energy expenditure of two captive Whooping Cranes measured using the doubly-labeled water method and time energy budgets. Energy expenditure values modeled by Niche Mapper were similar to values measured by the doubly-labeled water method and values estimated from time-energy budgets. Future studies will be able to use Niche Mapper as a non-invasive tool to explore energy-based limits to the fundamental niche of Whooping Cranes and apply this knowledge to management decisions. Basic questions about the importance of counter-current exchange and wading to animal physiological tolerances can also now be explored with the model. PMID:26308207

Countercurrent flow absorber and desorber

DOEpatents

Wilkinson, William H.

1984-01-01

Countercurrent flow absorber and desorber devices are provided for use in absorption cycle refrigeration systems and thermal boosting systems. The devices have increased residence time and surface area resulting in improved heat and mass transfer characteristics. The apparatuses may be incorporated into open cycle thermal boosting systems in which steam serves both as the refrigerant vapor which is supplied to the absorber section and as the supply of heat to drive the desorber section of the system.

Countercurrent heat exchange and thermoregulation during blood-feeding in kissing bugs

PubMed Central

Lahondère, Chloé; Insausti, Teresita C; Belev, George; Pereira, Marcos H

2017-01-01

Blood-sucking insects experience thermal stress at each feeding event on endothermic vertebrates. We used thermography to examine how kissing-bugs Rhodnius prolixus actively protect themselves from overheating. During feeding, these bugs sequester and dissipate the excess heat in their heads while maintaining an abdominal temperature close to ambient. We employed a functional-morphological approach, combining histology, µCT and X-ray-synchrotron imaging to shed light on the way these insects manage the flow of heat across their bodies. The close alignment of the circulatory and ingestion systems, as well as other morphological characteristics, support the existence of a countercurrent heat exchanger in the head of R. prolixus, which decreases the temperature of the ingested blood before it reaches the abdomen. This kind of system has never been described before in the head of an insect. For the first time, we show that countercurrent heat exchange is associated to thermoregulation during blood-feeding. PMID:29157359

Countercurrent Separation of Natural Products: An Update

PubMed Central

2015-01-01

This work assesses the current instrumentation, method development, and applications in countercurrent chromatography (CCC) and centrifugal partition chromatography (CPC), collectively referred to as countercurrent separation (CCS). The article provides a critical review of the CCS literature from 2007 since our last review (J. Nat. Prod.2008, 71, 1489–1508), with a special emphasis on the applications of CCS in natural products research. The current state of CCS is reviewed in regard to three continuing topics (instrumentation, solvent system development, theory) and three new topics (optimization of parameters, workflow, bioactivity applications). The goals of this review are to deliver the necessary background with references for an up-to-date perspective of CCS, to point out its potential for the natural product scientist, and thereby to induce new applications in natural product chemistry, metabolome, and drug discovery research involving organisms from terrestrial and marine sources. PMID:26177360

Application of an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum.

PubMed

Chen, Tao; Liu, Yongling; Zou, Denglang; Chen, Chen; You, Jinmao; Zhou, Guoying; Sun, Jing; Li, Yulin

2014-01-01

This study presents an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum. A new solvent system composed of petroleum ether/ethyl acetate/water (4:2:1, v/v/v) was developed for the liquid-liquid extraction of the crude extract from R. tanguticum. As a result, emodin, aloe-emodin, physcion, and chrysophanol were greatly enriched in the organic layer. In addition, an efficient method was successfully established to separate and purify the above anthraquinones by high-speed counter-current chromatography and preparative HPLC. This study supplies a new alternative method for the rapid enrichment, separation, and purification of emodin, aloe-emodin, physcione, and chrysophanol. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Separation of alkaloids in tea by high-speed counter-current chromatography].

PubMed

Yuan, L; Fu, R; Zhang, T; Deng, J; Li, X

1998-07-01

Alkaloids extracted from the green tea were separated by high-speed counter-current chromatography. A series of experiments have been performed to investigate effects of different solvent system. A system of CHCl3-CH3OH-NaH2PO4(23 mmol/L) = (4:3:2) was selected, in which the upper phase was used as the stationary phase, and the lower phase as mobile phase. When acidity of solvent system is pH 5.6, three chemical components are very efficiently isolated by one injection of 50 mg sample mixture. Analyzing the eluted fractions by TLC, we know that one is caffeine, and the other is theophylline. In comparing the separation results by high-speed counter-current chromatography with those by TLC, the advantages of this method is verified. It should find wide applications of this technology for the separation of crude mixture of plant components.

Extraction of manganese by alkyl monocarboxylic acid in a mixed extractant from a leaching solution of spent lithium-ion battery ternary cathodic material

NASA Astrophysics Data System (ADS)

Joo, Sung-Ho; Shin, Dongju; Oh, ChangHyun; Wang, Jei-Pil; Shin, Shun Myung

2016-02-01

We investigate the separation of manganese by an antagonistic effect from a leaching solution of ternary cathodic material of spent lithium-ion batteries that contain 11,400 mg L-1 Co, 11,700 mg L-1 Mn, 12,200 mg L-1 Ni, and 5300 mg L-1 Li using a mixture of alkyl monocarboxylic acid and di-(2-ethylhexyl)phosphoric acid extractants. pH isotherm, distribution coefficient, separation factor, McCabe-Thiele diagram, selective scrubbing, and countercurrent extraction tests are carried out to prove an antagonistic effect and to recover manganese using alkyl monocarboxylic in the mixed extractant. Slope analysis is used to determine the extraction mechanism between a mixture of extractants and valuable metals. An increasing concentration of alkyl monocarboxylic acid in the mixture of extractants results in a decrease in distribution coefficient of cobalt and manganese, however, the separation factor value (β(Mn/Co)) increases at pH 4.5. This is caused by slope analysis where alkyl monocarboxylic acid disrupts the extraction mechanism between di-(2-ethylhexyl)phosphoric acid and cobalt. Finally, continuous countercurrent extraction in a mini-plant test demonstrate the feasibility of manganese recovery from cobalt, nickel, and lithium.

Allogeneic cell therapy bioprocess economics and optimization: downstream processing decisions.

PubMed

Hassan, Sally; Simaria, Ana S; Varadaraju, Hemanthram; Gupta, Siddharth; Warren, Kim; Farid, Suzanne S

2015-01-01

To develop a decisional tool to identify the most cost effective process flowsheets for allogeneic cell therapies across a range of production scales. A bioprocess economics and optimization tool was built to assess competing cell expansion and downstream processing (DSP) technologies. Tangential flow filtration was generally more cost-effective for the lower cells/lot achieved in planar technologies and fluidized bed centrifugation became the only feasible option for handling large bioreactor outputs. DSP bottlenecks were observed at large commercial lot sizes requiring multiple large bioreactors. The DSP contribution to the cost of goods/dose ranged between 20-55%, and 50-80% for planar and bioreactor flowsheets, respectively. This analysis can facilitate early decision-making during process development.

THE IMPACT OF THE MCU LIFE EXTENSION SOLVENT ON DWPF GLASS FORMULATION EFFORTS

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

Peeler, D; Edwards, T

2011-03-24

As a part of the Actinide Removal Process (ARP)/Modular Caustic Side Solvent Extraction Unit (MCU) Life Extension Project, a next generation solvent (NG-CSSX), a new strip acid, and modified monosodium titanate (mMST) will be deployed. The strip acid will be changed from dilute nitric acid to dilute boric acid (0.01 M). Because of these changes, experimental testing with the next generation solvent and mMST is required to determine the impact of these changes in 512-S operations as well as Chemical Process Cell (CPC), Defense Waste Processing Facility (DWPF) glass formulation activities, and melter operations at DWPF. To support programmatic objectives,more » the downstream impacts of the boric acid strip effluent (SE) to the glass formulation activities and melter operations are considered in this study. More specifically, the impacts of boric acid additions to the projected SB7b operating windows, potential impacts to frit production temperatures, and the potential impact of boron volatility are evaluated. Although various boric acid molarities have been reported and discussed, the baseline flowsheet used to support this assessment was 0.01M boric acid. The results of the paper study assessment indicate that Frit 418 and Frit 418-7D are robust to the implementation of the 0.01M boric acid SE into the SB7b flowsheet (sludge-only or ARP-added). More specifically, the projected operating windows for the nominal SB7b projections remain essentially constant (i.e., 25-43 or 25-44% waste loading (WL)) regardless of the flowsheet options (sludge-only, ARP added, and/or the presence of the new SE). These results indicate that even if SE is not transferred to the Sludge Receipt and Adjustment Tank (SRAT), there would be no need to add boric acid (from a trim tank) to compositionally compensate for the absence of the boric acid SE in either a sludge-only or ARP-added SB7b flowsheet. With respect to boron volatility, the Measurement Acceptability Region (MAR) assessments also suggest that Slurry Mix Evaporator (SME) acceptability decisions would not be different assuming either 100% of the B{sub 2}O{sub 3} from the SE were retained or volatilized. More specifically, the 0.84 wt% B{sub 2}O{sub 3} in the SE is so minor that its presence in the SME analysis does not influence SME acceptability decisions. In fact, using the 100% retention and 100% volatilization composition projections, only minor differences in the predicted properties of the glass product occur with all of the glasses being acceptable over a WL interval of 32-42%. Based on the 0.01M boric acid flowsheet, there is very little difference between Frit 418 and Frit 418-7D (a frit that was compositionally altered to account for the 0.84 wt% B{sub 2}O{sub 3} in the SE) with respect to melt temperature. In fact, when one evaluates the composition of Frit 418-7D, it lies within the current Frit 418 vendor specifications and therefore could have been produced by the vendor targeting the nominal composition of Frit 418.« less

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

Bundy, R.D.; Alderfer, R.B.

Bench-scale tests of the direct calcination process for Portsmouth were conducted using batch pot calcination of simulated and actual raffinate wastes. These studies included investigation of the evaporation step needed to concentrate the raffinate before calcination. Tests were conducted at calcination temperatures of 600, 700, 1000, and 1200/sup 0/F with two levels of evaporative concentration before calcination at 1000/sup 0/F. Evaporation only tests were also made. Performance of the bench-scale system was excellent. A calcination temperature of 715/sup 0/F indicated that 80 to 100% of the Tc was retained in the calcined solids, while all of the nitrates were decomposedmore » to oxides. With calcination temperatures of greater than or equal to 1000/sup 0/F, part of the Tc escaped from the calcination pot to the scrubber. Below 700/sup 0/F, not all of the nitrates were decomposed to oxides. Most of the U remained in the calcined solids for calcination temperatures of less than or equal to 1000/sup 0/F. The mass of solids remaining after calcination was 4 to 5% of the original raffinate for calcination temperatures from 700 to 1000/sup 0/F. Flow rate through the off-gas treatment system was variable. The water scrubber had a good removal efficiency for nitrate and most metals, but not for uranium. The trapping efficiency of the limestone trap for nitrate was low. Flowsheet studies indicate that enough U would pass through the scrubber and chemical traps to cause an unacceptably high release of radioactivity if the assay of the uranium exceeded 33%. A small HEPA filter after the limestone chemical traps is recommended to reduce U emissions. A flowsheet was developed for a full-scale process for the direct calcination of raffinate waste.« less

Pretreatment Engineering Platform Phase 1 Final Test Report

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

Kurath, Dean E.; Hanson, Brady D.; Minette, Michael J.

2009-12-23

Pacific Northwest National Laboratory (PNNL) was tasked by Bechtel National Inc. (BNI) on the River Protection Project, Hanford Tank Waste Treatment and Immobilization Plant (RPP-WTP) project to conduct testing to demonstrate the performance of the WTP Pretreatment Facility (PTF) leaching and ultrafiltration processes at an engineering-scale. In addition to the demonstration, the testing was to address specific technical issues identified in Issue Response Plan for Implementation of External Flowsheet Review Team (EFRT) Recommendations - M12, Undemonstrated Leaching Processes.( ) Testing was conducted in a 1/4.5-scale mock-up of the PTF ultrafiltration system, the Pretreatment Engineering Platform (PEP). Parallel laboratory testing wasmore » conducted in various PNNL laboratories to allow direct comparison of process performance at an engineering-scale and a laboratory-scale. This report presents and discusses the results of those tests.« less

Countercurrent flow absorber and desorber

DOEpatents

Wilkinson, W.H.

1984-10-16

Countercurrent flow absorber and desorber devices are provided for use in absorption cycle refrigeration systems and thermal boosting systems. The devices have increased residence time and surface area resulting in improved heat and mass transfer characteristics. The apparatuses may be incorporated into open cycle thermal boosting systems in which steam serves both as the refrigerant vapor which is supplied to the absorber section and as the supply of heat to drive the desorber section of the system. 9 figs.

Separation of phenolic acids from sugarcane rind by online solid-phase extraction with high-speed counter-current chromatography.

PubMed

Geng, Ping; Fang, Yingtong; Xie, Ronglong; Hu, Weilun; Xi, Xingjun; Chu, Qiao; Dong, Genlai; Shaheen, Nusrat; Wei, Yun

2017-02-01

Sugarcane rind contains some functional phenolic acids. The separation of these compounds from sugarcane rind is able to realize the integrated utilization of the crop and reduce environment pollution. In this paper, a novel protocol based on interfacing online solid-phase extraction with high-speed counter-current chromatography (HSCCC) was established, aiming at improving and simplifying the process of phenolic acids separation from sugarcane rind. The conditions of online solid-phase extraction with HSCCC involving solvent system, flow rate of mobile phase as well as saturated extent of absorption of solid-phase extraction were optimized to improve extraction efficiency and reduce separation time. The separation of phenolic acids was performed with a two-phase solvent system composed of butanol/acetic acid/water at a volume ratio of 4:1:5, and the developed online solid-phase extraction with HSCCC method was validated and successfully applied for sugarcane rind, and three phenolic acids including 6.73 mg of gallic acid, 10.85 mg of p-coumaric acid, and 2.78 mg of ferulic acid with purities of 60.2, 95.4, and 84%, respectively, were obtained from 150 mg sugarcane rind crude extracts. In addition, the three different elution methods of phenolic acids purification including HSCCC, elution-extrusion counter-current chromatography and back-extrusion counter-current chromatography were compared. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Gradient x Isocratic Elution CCC on the Isolation of Verbascoside and Other Phenylethanoids: Influence of the Complexity of the Matrix.

PubMed

Leitão, Gilda Guimarães; Pinto, Shaft Correa; de Oliveira, Danilo Ribeiro; Timoteo, Patrícia; Guimarães, Michelle Guedes; Cordova, Wilmer H Perera; Leitão, Suzana Guimarães

2015-11-01

Verbascoside is a phenylethanoid glycoside widely distributed in nature, especially among the order Lamiales, occurring in numerous plants that are constituents of folk medicine preparations. This natural compound, previously isolated by our group from the ethyl acetate extract of Lantana trifolia using the gradient approach in countercurrent chromatography, was now isolated from the butanol extract of the same plant and from Lippia alba f. intermedia (Verbenaceae) using countercurrent chromatography in either gradient or isocratic elution modes. The ethyl acetate extract of L. alba, rich in phenylethanoids and flavonoids, was fractionated using countercurrent chromatography in the step-gradient elution approach. The four-step solvent system was composed of n-hexane-ethyl acetate-n-butanol-water (4 : 10 : X : 10), where X = 1 (solvent system A), 3 (solvent system B), 5 (solvent system C), and 7 (solvent system D), and allowed for the isolation of verbascoside along with other phenylethanoids and flavonoids from both plants. Verbascoside and 2'-O-β-apiosylverbascoside were further isolated from the n-butanol extract of L. trifolia using the solvent system ethyl acetate-n-butanol-water 10 : 2 : 10 on an isocratic run. The difference in the complexity of the two plant extracts demanded different purification steps, which included a second high-speed countercurrent chromatography purification using the isocratic elution mode. Georg Thieme Verlag KG Stuttgart · New York.

Preparative separation of six rhynchophylla alkaloids from Uncaria macrophylla wall by pH-zone refining counter-current chromatography.

PubMed

Zhang, Qinghai; Lin, Changhu; Duan, Wenjuan; Wang, Xiao; Luo, Aiqin

2013-12-12

pH-Zone refining counter-current chromatography was successfully applied to the preparative isolation and purification of six alkaloids from the ethanol extracts of Uncaria macrophylla Wall. Because of the low content of alkaloids (about 0.2%, w/w) in U. macrophylla Wall, the target compounds were enriched by pH-zone refining counter-current chromatography using a two-phase solvent system composed of petroleum ether-ethyl acetate-isopropanol-water (2:6:3:9, v/v), adding 10 mM triethylamine in organic stationary phase and 5 mM hydrochloric acid in aqueous mobile phase. Then pH-zone refining counter-current chromatography using the other two-phase solvent system was used for final purification. Six target compounds were finally isolated and purified by following two-phase solvent system composed of methyl tert-butyl ether (MTBE)-acetonitrile-water (4:0.5:5, v/v), adding triethylamine (TEA) (10 mM) to the organic phase and HCl (5 mM) to aqueous mobile phase. The separation of 2.8 g enriched total alkaloids yielded 36 mg hirsutine, 48 mg hirsuteine, 82 mg uncarine C, 73 mg uncarine E, 163 mg rhynchophylline, and 149 mg corynoxeine, all with purities above 96% as verified by HPLC Their structures were identified by electrospray ionization-mass spectrometry (ESI-MS) and 1H-NMR spectroscopy.

Improved separation with the intermittently pressed tubing of multilayer coil in type-I counter-current chromatography.

PubMed

Yang, Yi; Yang, Jiao; Fang, Chen; Wang, Jihui; Gu, Dongyu; Tian, Jing; Ito, Yoichiro

2018-05-25

The intermittently pressed tubing was introduced in type-I counter-current chromatographic system as the separation column to improve the separation performance in the present study. The separations were performed with two different solvent systems composed of 1-butanol-acetic acid-water (4:1:5, v/v) (BAW) and hexane-ethyl acetate-methanol-0.1 M HCl (1:1:1:1, v/v) (HEMW) using dipeptides and DNP-amino acids as test samples, respectively. The chromatographic performance was evaluated in terms of retention of the stationary phase (Sf), theoretical plate (N) and peak resolution (Rs). In general, the type-I planetary motion with the multilayer coil of non-modified standard tubing can yield the best separation at a low revolution speed of 200 rpm with lower flow rate. The present results with intermittently pressed tubing indicated that the performance was also optimal at the revolution speed of 200 rpm where the lower flow rate was more beneficial to retention of stationary phase and resolution. In the moderately hydrophobic two-phase solvent system composed of hexane-ethyl acetate-metanol-0.1 M hydrochloric acid (1:1:1:1, v/v), DNP-amino acids were separated with Rs at 1.67 and 1.47, respectively, with 12.66% of stationary phase retention at a flow rate of 0.25 ml/min. In the polar solvent system composed of 1-butanol-acetic acid-water (4:1:5, v/v), dipeptide samples were resolved with Rs at 2.18 and 18.75% of stationary phase retention at a flow rate of 0.25 ml/min. These results indicate that the present system substantially improves the separation efficiency of type-I counter-current chromatographic system. Published by Elsevier B.V.

Use of Inert Gases and Carbon Monoxide to Study the Possible Influence of Countercurrent Exchange on Passive Absorption from the Small Bowel

PubMed Central

Bond, John H.; Levitt, David G.; Levitt, Michael D.

1974-01-01

The purpose of the present study was to quantitate the influence of countercurrent exchange on passive absorption of highly diffusible substances from the small intestine of the rabbit. The absorption of carbon monoxide, which is tightly bound to hemoglobin and therefore cannot exchange, was compared to the absorption of four unbound gases (H2, He, CH4, and 133Xe), which should exchange freely. The degree to which the observed absorption of the unbound gases falls below that predicted from CO absorption should provide a quantitative measure of countercurrent exchange. CO uptake at high luminal Pco is flow-limited and, assuming that villus and central hemoglobin concentrations are equal, the flow that equilibrates with CO (Fco) was calculated to equal 7.24 ml/min/100 g. The observed absorption rate of the unbound gases was from two to four times greater than would have been predicted had their entire uptake been accounted for by equilibration with Fco. This is the opposite of what would occur if countercurrent exchange retarded absorption of the unbound gases. The unbound gases have both flow- and diffusion-limited components, and Fco should account for only the fraction of absorption that is flow limited. A simple model of perfusion and diffusion made it possible to calculate the fraction of the total uptake of unbound gases that was flow limited. This fraction of the total observed absorption rate was still about 1.8 times greater than predicted by CO absorption. A possible explanation for this discrepancy is that plasma skimming reduces the hemoglobin of villus blood to about 60% of that of central blood. Thus, Fco is actually about 1.7 times greater than initially calculated, and with this correction, there is close agreement between the predicted and observed rates of absorption of each of the unbound gases. We conclude that countercurrent exchange does not influence passive absorption under the conditions of this study. PMID:4436431

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

Jain, V.; Shah, H.; Bannochie, C. J.

Mercury (Hg) in the Savannah River Site Liquid Waste System (LWS) originated from decades of canyon processing where it was used as a catalyst for dissolving the aluminum cladding of reactor fuel. Approximately 60 metric tons of mercury is currently present throughout the LWS. Mercury has long been a consideration in the LWS, from both hazard and processing perspectives. In February 2015, a Mercury Program Team was established at the request of the Department of Energy to develop a comprehensive action plan for long-term management and removal of mercury. Evaluation was focused in two Phases. Phase I activities assessed themore » Liquid Waste inventory and chemical processing behavior using a system-by-system review methodology, and determined the speciation of the different mercury forms (Hg+, Hg++, elemental Hg, organomercury, and soluble versus insoluble mercury) within the LWS. Phase II activities are building on the Phase I activities, and results of the LWS flowsheet evaluations will be summarized in three reports: Mercury Behavior in the Salt Processing Flowsheet (i.e. this report); Mercury Behavior in the Defense Waste Processing Facility (DWPF) Flowsheet; and Mercury behavior in the Tank Farm Flowsheet (Evaporator Operations). The evaluation of the mercury behavior in the salt processing flowsheet indicates, inter alia, the following: (1) In the assembled Salt Batches 7, 8 and 9 in Tank 21, the total mercury is mostly soluble with methylmercury (MHg) contributing over 50% of the total mercury. Based on the analyses of samples from 2H Evaporator feed and drop tanks (Tanks 38/43), the source of MHg in Salt Batches 7, 8 and 9 can be attributed to the 2H evaporator concentrate used in assembling the salt batches. The 2H Evaporator is used to evaporate DWPF recycle water. (2) Comparison of data between Tank 21/49, Salt Solution Feed Tank (SSFT), Decontaminated Salt Solution Hold Tank (DSSHT), and Tank 50 samples suggests that the total mercury as well as speciated forms in the assembled salt batches in Tanks 21/49 pass through the Actinide Removal Process (ARP) / Modular Caustic Side Solvent Extraction Unit (MCU) process to Tank 50 with no significant change in the mercury chemistry. (3) In Tank 50, Decontaminated Salt Solution (DSS) from ARP/MCU is the major contributor to the total mercury including MHg. (4) Speciation analyses of TCLP leached solutions of the grout samples prepared from Tank 21, as well as Tank 50 samples, show the majority of the mercury released in the solution is MHg.« less

Separation of Calcium Isotopes by Counter-Current Electro-Migration in Molten Salts; SEPARATION DES ISOTOPES DU CALCIUM PAR ELECTRO-MIGRATION A CONTRECOURANT EN SELS FONDUS

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

Menes, F.; Dirian, G.; Roth, E.

1962-01-01

The method of counter-current electromigration in molten salts was applied to CaBr/sub 2/ with an alkali metal bromide added to the cathode compartment. Enrichments on Ca/sup 46/ greater than a factor of two were obtained at the anode. The mass effect was found to be about 0.06. An estimation of the cost of energy for a process based on this method was made. (auth)

Hybrid indirect/direct contactor for thermal management of counter-current processes

DOEpatents

Hornbostel, Marc D.; Krishnan, Gopala N.; Sanjurjo, Angel

2018-03-20

The invention relates to contactors suitable for use, for example, in manufacturing and chemical refinement processes. In an aspect is a hybrid indirect/direct contactor for thermal management of counter-current processes, the contactor comprising a vertical reactor column, an array of interconnected heat transfer tubes within the reactor column, and a plurality of stream path diverters, wherein the tubes and diverters are configured to block all straight-line paths from the top to bottom ends of the reactor column.

Low temperature dissolution flowsheet for Pu metal

DOE PAGES

Daniel, Jr., William E.; Almond, Philip M.; Rudisill, Tracy S.

2017-06-30

The Savannah River National Laboratory was requested to develop a Pu metal dissolution flowsheet at two reduced temperature ranges for implementation in the Savannah River Site H-Canyon facility. The dissolution and H 2 generation rates during Pu metal dissolution were investigated using a dissolving solution at ambient temperature (20–30°C) and for an intermediate temperature of 50–60°C. The Pu metal dissolution rate measured at 57°C was approximately 20 times slower than at boiling (112–116°C). As a result, the dissolution rate at ambient temperature (24°C) was approximately 80 times slower than the dissolution rate at boiling. Hydrogen concentrations were less than detectablemore » (<0.1 vol%).« less

Simultaneous separation of three isomeric sennosides from senna leaf (Cassia acutifolia) using counter-current chromatography.

PubMed

Park, Sait Byul; Kim, Yeong Shik

2015-10-01

Senna leaf is widely consumed as tea to treat constipation or to aid in weight loss. Sennoside A, A1 , and B are dirheinanthrone glucosides that are abundant and the bioactive constituents in the plant. They are isomers that refer to the (R*R*), (S*S*), and (R*S*) forms of protons on C-10 and C-10' centers and it is difficult to refine them individually due to their structural similarities. The new separation method using counter-current chromatography successfully purified sennoside A, A1 , and B from senna leaf (Cassia acutifolia) while reversed-phase medium-pressure liquid chromatography yielded sennoside A only. n-Butanol/isopropanol/water (5:1:6, v/v/v) was selected as the solvent system for counter-current chromatography operation, and the partition coefficients were carefully determined by adding different concentrations of formic acid. High-resolution mass spectrometry and NMR spectroscopy were performed to verify the chemical properties of the compounds. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation of five compounds from leaves of Andrographis paniculata (Burm. f.) Nees by off-line two-dimensional high-speed counter-current chromatography combined with gradient and recycling elution.

PubMed

Zhang, Li; Liu, Qi; Yu, Jingang; Zeng, Hualiang; Jiang, Shujing; Chen, Xiaoqing

2015-05-01

An off-line two-dimensional high-speed counter-current chromatography method combined with gradient and recycling elution mode was established to isolate terpenoids and flavones from the leaves of Andrographis paniculata (Burm. f.) Nees. By using the solvent systems composed of n-hexane/ethyl acetate/methanol/water with different volume ratios, five compounds including roseooside, 5,4'-dihydroxyflavonoid-7-O-β-d-pyranglucuronatebutylester, 7,8-dimethoxy-2'-hydroxy-5-O-β-d-glucopyranosyloxyflavon, 14-deoxyandrographiside, and andrographolide were successfully isolated. Purities of these isolated compounds were all over 95% as determined by high-performance liquid chromatography. Their structures were identified by UV, mass spectrometry, and (1) H NMR spectroscopy. It has been demonstrated that the combination of off-line two-dimensional high-speed counter-current chromatography with different elution modes is an efficient technique to isolate compounds from complex natural product extracts. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Online hyphenation of extraction, Sephadex LH-20 column chromatography, and high-speed countercurrent chromatography: A highly efficient strategy for the preparative separation of andrographolide from Andrographis paniculata in a single step.

PubMed

Zhang, Ying-Qi; Wang, Shan-Shan; Han, Chao; Xu, Jin-Fang; Luo, Jian-Guang; Kong, Ling-Yi

2017-12-01

A novel isolation strategy, online hyphenation of ultrasonic extraction, Sephadex LH-20 column chromatography combined with high-speed countercurrent chromatography, was developed for pure compounds extraction and purification. Andrographolide from Andrographis paniculata was achieved only in a single step purification protocol via the present strategy. The crude powder was ultrasonic extracted and extraction was pumped into Sephadex LH-20 column directly to cut the nontarget fractions followed by the second-dimensional high-speed countercurrent chromatography, hyphenated by a six-port valve equipped at the post-end of Sephadex LH-20 column, for the final purification. The results yielded andrographolide with the amount of 1.02 mg and a purity of 98.5% in a single step, indicating that the present method is effective to harvest target compound from medicinal plant. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A simple tool for tubing modification to improve spiral high-speed counter-current chromatography for protein purification

PubMed Central

Ito, Yoichiro; Ma, Xiaofeng; Clary, Robert

2016-01-01

A simple tool is introduced which can modify the shape of tubing to enhance the partition efficiency in high-speed countercurrent chromatography. It consists of a pair of interlocking identical gears, each coaxially holding a pressing wheel to intermittently compress plastic tubing in 0 – 10 mm length at every 1 cm interval. The performance of the processed tubing is examined in protein separation with 1.6 mm ID PTFE tubing intermittently pressed in 3 mm and 10 mm width both at 10 mm intervals at various flow rates and revolution speeds. A series of experiments was performed with a polymer phase system composed of polyethylene glycol and dibasic potassium phosphate each at 12.5% (w/w) in deionized water using three protein samples. Overall results clearly demonstrate that the compressed tubing can yield substantially higher peak resolution than the non-processed tubing. The simple tubing modifier is very useful for separation of proteins with high-speed countercurrent chromatography. PMID:27818942

Purification of α-glucosidase from mouse intestine by countercurrent chromatography coupled with a reverse micelle solvent system.

PubMed

He, Kai; Zou, Zongyao; Hu, Yinran; Yang, Yong; Xiao, Yubo; Gao, Pincao; Li, Xuegang; Ye, Xiaoli

2016-02-01

Countercurrent chromatography coupled with a reverse micelle solvent was applied to separate α-glucosidase, which is stable at pH 6.0-8.8, 15-50°C. The separation conditions are as follows: stationary phase: pH 4.0 Tris-HCl buffer phase containing 50 mM Tris-HCl and 50 mM KCl; mobile phase A: isooctane containing 50 mM anionic surfactant sodium di(2-ethylhexyl)sulfosuccinate; mobile phase B: 50 mM Tris-HCl buffer containing 500 mM KCl (pH 8.0); In total, 25 mL (23.9 mg) crude enzyme was injected through the injection valve, the enzymatic reaction and sodium dodecylsulfate polyacrylamide gel electrophoresis results imply that the activity of purified α-glucosidase is 6.63-fold higher than that of the crude enzyme. Therefore, countercurrent chromatography coupled with a reverse micelle solvent is capable for protein separation and enrichment. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A simple tool for tubing modification to improve spiral high-speed counter-current chromatography for protein purification.

PubMed

Ito, Yoichiro; Ma, Xiaofeng; Clary, Robert

2016-01-01

A simple tool is introduced which can modify the shape of tubing to enhance the partition efficiency in high-speed countercurrent chromatography. It consists of a pair of interlocking identical gears, each coaxially holding a pressing wheel to intermittently compress plastic tubing in 0 - 10 mm length at every 1 cm interval. The performance of the processed tubing is examined in protein separation with 1.6 mm ID PTFE tubing intermittently pressed in 3 mm and 10 mm width both at 10 mm intervals at various flow rates and revolution speeds. A series of experiments was performed with a polymer phase system composed of polyethylene glycol and dibasic potassium phosphate each at 12.5% (w/w) in deionized water using three protein samples. Overall results clearly demonstrate that the compressed tubing can yield substantially higher peak resolution than the non-processed tubing. The simple tubing modifier is very useful for separation of proteins with high-speed countercurrent chromatography.

Flow enhancement of deformable self-driven objects by countercurrent

NASA Astrophysics Data System (ADS)

Mashiko, Takashi; Fujiwara, Takashi

2016-10-01

We report numerical simulations of the mixed flows of two groups of deformable self-driven objects. The objects belonging to the group A (B) have drift coefficient D =DA (DB), where a positive (negative) value of D denotes the rightward (leftward) driving force. For co-current flows (DA ,DB > 0), the result is rather intuitive: the net flow of one group (QA) increases if the driving force of the other group is stronger than its own driving force (i.e., DB >DA), and decreases otherwise (DB

Separation of three phenolic high-molecular-weight compounds from the crude extract of Terminalia Chebula Retz. by ultrasound-assisted extraction and high-speed counter-current chromatography.

PubMed

Zou, Deng-lang; Chen, Tao; Li, Hong-mei; Chen, Chen; Zhao, Jing-yang; Li, Yu-lin

2016-04-01

This study presents an efficient strategy for separation of three phenolic compounds with high molecular weight from the crude extract of Terminalia chebula Retz. by ultrasound-assisted extraction and high-speed counter-current chromatography. The ultrasound-assisted extraction conditions were optimized by response surface methodology and the results showed the target compounds could be well enriched under the optimized extraction conditions. Then the crude extract was directly separated by high-speed counter-current chromatography without any pretreatment using n-hexane/ethyl acetate/methanol/water (1:7:0.5:3, v/v/v/v) as the solvent system. In 180 min, 13 mg of A, 18 mg of B, and 9 mg of C were obtained from 200 mg of crude sample. Their structures were identified as Chebulagic acid (A, 954 Da), Chebulinic acid (B, 956 Da), and Ellagic acid (C) by (1) H NMR spectroscopy. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Heat production in depth up to 2500m via in situ combustion of methane using a counter-current heat-exchange reactor

NASA Astrophysics Data System (ADS)

Schicks, Judith Maria; Spangenberg, Erik; Giese, Ronny; Heeschen, Katja; Priegnitz, Mike; Luzi-Helbing, Manja; Thaler, Jan; Abendroth, Sven; Klump, Jens

2014-05-01

In situ combustion is a well-known method used for exploitation of unconventional oil deposits such as heavy oil/bitumen reservoirs where the required heat is produced directly within the oil reservoir by combustion of a small percentage of the oil. A new application of in situ combustion for the production of methane from hydrate-bearing sediments was tested at pilot plant scale within the first phase of the German national gas hydrate project SUGAR. The applied method of in situ combustion was a flameless, catalytic oxidation of CH4 in a counter-current heat-exchange reactor with no direct contact between the catalytic reaction zone and the reservoir. The catalyst permitted a flameless combustion of CH4 with air to CO2 and H2O below the auto-ignition temperature of CH4 in air (868 K) and outside the flammability limits. This led to a double secured application of the reactor. The relatively low reaction temperature allowed the use of cost-effective standard materials for the reactor and prevented NOx formation. Preliminary results were promising and showed that only 15% of the produced CH4 was needed to be catalytically burned to provide enough heat to dissociate the hydrates in the environment and release CH4. The location of the heat source right within the hydrate-bearing sediment is a major advantage for the gas production from natural gas hydrates as the heat is generated where it is needed without loss of energy due to transportation. As part of the second period of the SUGAR project the reactor prototype of the first project phase was developed further to a borehole tool. The dimensions of this counter-current heat-exchange reactor are about 540 cm in length and 9 cm in diameter. It is designed for applications up to depths of 2500 m. A functionality test and a pressure test of the reactor were successfully carried out in October 2013 at the continental deep drilling site (KTB) in Windischeschenbach, Germany, in 600 m depth and 2000 m depth, respectively. In this study we present technical details of the reactor, the catalyst and potential fields of application beside the production of natural gas from hydrate bearing sediments.

Preparative enantioseparation of loxoprofen precursor by recycling countercurrent chromatography with hydroxypropyl-β-cyclodextrin as a chiral selector.

PubMed

Zhang, Hui; Qiu, Xujun; Lv, Liqiong; Sun, Wenyu; Wang, Chaoyue; Yan, Jizhong; Tong, Shengqiang

2018-04-17

Recycling countercurrent chromatography was successfully applied to the resolution of 2-(4-bromomethylphenyl)propionic acid, a key synthetic intermediate for synthesis of nonsteroidal anti-inflammatory drug loxoprofen, using hydroxypropyl-β-cyclodextrin as chiral selector. The two-phase solvent system composed of n-hexane/n-butyl acetate/0.1 mol/L citrate buffer solution with pH 2.4 (8:2:10, v/v/v) was selected. Influence factors for the enantioseparation were optimized, including type of substituted β-cyclodextrin, concentration of hydroxypropyl-β-cyclodextrin, separation temperature, and pH of aqueous phase. Under optimized separation conditions, 50 mg of 2-(4-bromomethylphenyl)propionic acid was enantioseparated using preparative recycling countercurrent chromatography. Technical details for recycling elution mode were discussed. The purities of both the S and R enantiomers were over 99.0% as determined by high-performance liquid chromatography. The enantiomeric excess of the S and R enantiomers reached 98.0%. The recovery of the enantiomers from eluted fractions was 40.8-65.6%, yielding 16.4 mg of the S enantiomer and 10.2 mg of the R enantiomer. At the same time, we attempted to enantioseparate the anti-inflammatory drug loxoprofen by countercurrent chromatography and high-performance liquid chromatography using a chiral mobile phase additive. However, no successful enantioseparation was achieved so far. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Schinus terebinthifolius scale-up countercurrent chromatography (Part I): High performance countercurrent chromatography fractionation of triterpene acids with off-line detection using atmospheric pressure chemical ionization mass spectrometry.

PubMed

Vieira, Mariana Neves; Costa, Fernanda das Neves; Leitão, Gilda Guimarães; Garrard, Ian; Hewitson, Peter; Ignatova, Svetlana; Winterhalter, Peter; Jerz, Gerold

2015-04-10

'Countercurrent chromatography' (CCC) is an ideal technique for the recovery, purification and isolation of bioactive natural products, due to the liquid nature of the stationary phase, process predictability and the possibility of scale-up from analytical to preparative scale. In this work, a method developed for the fractionation of Schinus terebinthifolius Raddi berries dichloromethane extract was thoroughly optimized to achieve maximal throughput with minimal solvent and time consumption per gram of processed crude extract, using analytical, semi-preparative and preparative 'high performance countercurrent chromatography' (HPCCC) instruments. The method using the biphasic solvent system composed of n-heptane-ethyl acetate-methanol-water (6:1:6:1, v/v/v/v) was volumetrically scaled up to increase sample throughput up to 120 times, while maintaining separation efficiency and time. As a fast and specific detection alternative, the fractions collected from the CCC-separations were injected to an 'atmospheric pressure chemical ionization mass-spectrometer' (APCI-MS/MS) and reconstituted molecular weight MS-chromatograms of the APCI-ionizable compounds from S. terebinthifolius were obtained. This procedure led to the direct isolation of tirucallane type triterpenes such as masticadienonic and 3β-masticadienolic acids. Also oleanonic and moronic acids have been identified for the first time in the species. In summary, this approach can be used for other CCC scale-up processes, enabling MS-target-guided isolation procedures. Copyright © 2015 Elsevier B.V. All rights reserved.

Scale-up protein separation on stainless steel wide bore toroidal columns in the type-J counter-current chromatography.

PubMed

Guan, Yue Hugh; Hewitson, Peter; van den Heuvel, Remco N A M; Zhao, Yan; Siebers, Rick P G; Zhuang, Ying-Ping; Sutherland, Ian

2015-12-11

Manufacturing high-value added biotech biopharmaceutical products (e.g. therapeutic proteins) requires quick-to-develop, GMP-compliant, easy-to-scale and cost effective preparatory chromatography technologies. In this work, we describe the construction and testing of a set of 5-mm inner diameter stainless steel toroidal columns for use on commercially available preparatory scale synchronous J-type counter-current chromatography (CCC) machinery. We used a 20.2m long column with an aqueous two-phase system containing 14% (w/w) PEG1000 and 14% (w/w) potassium phosphate at pH 7, and tested a sample loading of 5% column volume and a mobile phase flow rate of 20ml/min. We then satisfactorily demonstrated the potential for a weekly protein separation and preparation throughput of ca. 11g based on a normal weekly routine for separating a pair of model proteins by making five stacked injections on a single portion of stationary phase with no stripping. Compared to our previous 1.6mm bore PTFE toroidal column, the present columns enlarged the nominal column processing throughput by nearly 10. For an ideal model protein injection modality, we observed a scaling up factor of at least 21. The 2 scales of protein separation and purification steps were realized on the same commercial CCC device. Copyright © 2015 Elsevier B.V. All rights reserved.

Consolidated fuel reprocessing program

NASA Astrophysics Data System (ADS)

1985-02-01

Improved processes and components for the Breeder Reprocessing Engineering Test (BRET) were identified and developed as well as the design, procurement and development of prototypic equipment. The integrated testing of process equipment and flowsheets prototypical of a pilot scale full reprocessing plant, and also for testing prototypical remote features of specific complex components in the system are provided. Information to guide the long range activities of the Consolidated Fuel Reprocessing Program (CERP), a focal point for foreign exchange activities, and support in specialized technical areas are described. Research and development activities in HTGR fuel treatment technology are being conducted. Head-end process and laboratory scale development efforts, as well as studies specific to HTGR fuel, are reported. The development of off-gas treatment processes has generic application to fuel reprocessing, progress in this work is also reported.

RESULTS OF INITIAL AMMONIA OXIDATION TESTING

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

Nash, C.; Fowley, M.

This memo presents an experimental survey of aqueous phase chemical processes to remove aqueous ammonia from waste process streams. Ammonia is generated in both the current Hanford waste flowsheet and in future waste processing. Much ammonia will be generated in the Low Activity Waste (LAW) melters.i Testing with simulants in glass melters at Catholic University has demonstrated the significant ammonia production.ii The primary reaction there is the reducing action of sugar on nitrate in the melter cold cap. Ammonia has been found to be a problem in secondary waste stabilization. Ammonia vapors are noxious and destruction of ammonia could reducemore » hazards to waste treatment process personnel. It is easily evolved especially when ammonia-bearing solutions are adjusted to high pH.« less

Wall pressure measurements of flooding in vertical countercurrent annular air–water flow

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

Choutapalli, I., Vierow, K.

2010-01-01

An experimental study of flooding in countercurrent air-water annular flow in a large diameter vertical tube using wall pressure measurements is described in this paper. Axial pressure profiles along the length of the test section were measured up to and after flooding using fast response pressure transducers for three representative liquid flow rates representing a wide range of liquid Reynolds numbers (ReL = 4Γ/μ; Γ is the liquid mass flow rate per unit perimeter; μ is the dynamic viscosity) from 3341 to 19,048. The results show that flooding in large diameter tubes cannot be initiated near the air outlet andmore » is only initiated near the air inlet. Fourier analysis of the wall pressure measurements shows that up to the point of flooding, there is no dominant wave frequency but rather a band of frequencies encompassing both the low frequency and the broad band that are responsible for flooding. The data indicates that flooding in large diameter vertical tubes may be caused by the constructive superposition of a plurality of waves rather than the action of a single large-amplitude wave.« less

Fractionation of Gallotannins from mango (Mangifera indica L.) kernels by high-speed counter-current chromatography and determination of their antibacterial activity.

PubMed

Engels, Christina; Gänzle, Michael G; Schieber, Andreas

2010-01-27

High-speed counter-current chromatography was applied to the separation of gallotannins from mango (Mangifera indica L.) kernels. The kernels were defatted and subsequently extracted with aqueous acetone [80% (v/v)]. The crude extract was purified by being partitioned against ethyl acetate. A hexane/ethyl acetate/methanol/water solvent system [0.5:5:1:5 (v/v/v/v)] was used in the head-to-tail mode to elute tannins according to their degree of galloylation (tetra-O-galloylglucose to deca-O-galloylglucose). The compounds were characterized using liquid chromatography and mass spectrometry in the negative ionization mode. Purities ranged from 72% (tetra-O-galloylglucose) to 100% (octa-O-galloylglucose). The iron binding capacity of gallotannins was dependent on the number of galloyl groups in the molecule, with a larger capacity at lower degrees of galloylation. The minimum inhibitory concentration against Bacillus subtilis did not change among the different gallotannins tested and was in the range of 0.05-0.1 g/L in Luria-Bertani broth but up to 20 times higher in media containing more iron and divalent cations.

A mixture theory approach to model co- and counter-current two-phase flow in porous media accounting for viscous coupling

NASA Astrophysics Data System (ADS)

Qiao, Y.; Andersen, P. Ø.; Evje, S.; Standnes, D. C.

2018-02-01

It is well known that relative permeabilities can depend on the flow configuration and they are commonly lower during counter-current flow as compared to co-current flow. Conventional models must deal with this by manually changing the relative permeability curves depending on the observed flow regime. In this paper we use a novel two-phase momentum-equation-approach based on general mixture theory to generate effective relative permeabilities where this dependence (and others) is automatically captured. In particular, this formulation includes two viscous coupling effects: (i) Viscous drag between the flowing phases and the stagnant porous rock; (ii) viscous drag caused by momentum transfer between the flowing phases. The resulting generalized model will predict that during co-current flow the faster moving fluid accelerates the slow fluid, but is itself decelerated, while for counter-current flow they are both decelerated. The implications of these mechanisms are demonstrated by investigating recovery of oil from a matrix block surrounded by water due to a combination of gravity drainage and spontaneous imbibition, a situation highly relevant for naturally fractured reservoirs. We implement relative permeability data obtained experimentally through co-current flooding experiments and then explore the model behavior for different flow cases ranging from counter-current dominated to co-current dominated. In particular, it is demonstrated how the proposed model seems to offer some possible interesting improvements over conventional modeling by providing generalized mobility functions that automatically are able to capture more correctly different flow regimes for one and the same parameter set.

Flooding Experiments and Modeling for Improved Reactor Safety

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

Solmos, M.; Hogan, K. J.; Vierow, K.

2008-09-14

Countercurrent two-phase flow and “flooding” phenomena in light water reactor systems are being investigated experimentally and analytically to improve reactor safety of current and future reactors. The aspects that will be better clarified are the effects of condensation and tube inclination on flooding in large diameter tubes. The current project aims to improve the level of understanding of flooding mechanisms and to develop an analysis model for more accurate evaluations of flooding in the pressurizer surge line of a Pressurized Water Reactor (PWR). Interest in flooding has recently increased because Countercurrent Flow Limitation (CCFL) in the AP600 pressurizer surge linemore » can affect the vessel refill rate following a small break LOCA and because analysis of hypothetical severe accidents with the current flooding models in reactor safety codes shows that these models represent the largest uncertainty in analysis of steam generator tube creep rupture. During a hypothetical station blackout without auxiliary feedwater recovery, should the hot leg become voided, the pressurizer liquid will drain to the hot leg and flooding may occur in the surge line. The flooding model heavily influences the pressurizer emptying rate and the potential for surge line structural failure due to overheating and creep rupture. The air-water test results in vertical tubes are presented in this paper along with a semi-empirical correlation for the onset of flooding. The unique aspects of the study include careful experimentation on large-diameter tubes and an integrated program in which air-water testing provides benchmark knowledge and visualization data from which to conduct steam-water testing.« less

Fundamental Chemical Kinetic And Thermodynamic Data For Purex Process Models

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

Taylor, R.J.; Fox, O.D.; Sarsfield, M.J.

2007-07-01

To support either the continued operations of current reprocessing plants or the development of future fuel processing using hydrometallurgical processes, such as Advanced Purex or UREX type flowsheets, the accurate simulation of Purex solvent extraction is required. In recent years we have developed advanced process modeling capabilities that utilize modern software platforms such as Aspen Custom Modeler and can be run in steady state and dynamic simulations. However, such advanced models of the Purex process require a wide range of fundamental data including all relevant basic chemical kinetic and thermodynamic data for the major species present in the process. Thismore » paper will summarize some of these recent process chemistry studies that underpin our simulation, design and testing of Purex solvent extraction flowsheets. Whilst much kinetic data for actinide redox reactions in nitric acid exists in the literature, the data on reactions in the diluted TBP solvent phase is much rarer. This inhibits the accurate modelization of the Purex process particularly when species show a significant extractability in to the solvent phase or when cycling between solvent and aqueous phases occurs, for example in the reductive stripping of Pu(IV) by ferrous sulfamate in the Magnox reprocessing plant. To support current oxide reprocessing, we have investigated a range of solvent phase reactions: - U(IV)+HNO{sub 3}; - U(IV)+HNO{sub 2}; - U(IV)+HNO{sub 3} (Pu catalysis); - U(IV)+HNO{sub 3} (Tc catalysis); - U(IV)+ Np(VI); - U(IV)+Np(V); - Np(IV)+HNO{sub 3}; - Np(V)+Np(V); Rate equations have been determined for all these reactions and kinetic rate constants and activation energies are now available. Specific features of these reactions in the TBP phase include the roles of water and hydrolyzed intermediates in the reaction mechanisms. In reactions involving Np(V), cation-cation complex formation, which is much more favourable in TBP than in HNO{sub 3}, also occurs and complicates the redox chemistry. Whilst some features of the redox chemistry in TBP appear similar to the corresponding reactions in aqueous HNO{sub 3}, there are notable differences in rates, the forms of the rate equations and mechanisms. Secondly, to underpin the development of advanced single cycle flowsheets using the complexant aceto-hydroxamic acid, we have also characterised in some detail its redox chemistry and solvent extraction behaviour with both Np and Pu ions. We find that simple hydroxamic acids are remarkably rapid reducing agents for Np(VI). They also reduce Pu(VI) and cause a much slower reduction of Pu(IV) through a complex mechanism involving acid hydrolysis of the ligand. AHA is a strong hydrophilic and selective complexant for the tetravalent actinide ions as evidenced by stability constant and solvent extraction data for An(IV), M(III) and U(VI) ions. This has allowed the successful design of U/Pu+Np separation flowsheets suitable for advanced fuel cycles. (authors)« less

Counter-current acid leaching process for the removal of Cu, Pb, Sb and Zn from shooting range soil.

PubMed

Lafond, Stéphanie; Blais, Jean-François; Mercier, Guy; Martel, Richard

2013-01-01

This research explores the performance of a counter-current leaching process (CCLP) for Cu, Pb, Sb and Zn extraction in a polluted shooting range soil. The initial metal concentrations in the soil were 1790 mg Cu/kg, 48,300 mg Pb/kg, 840 mg Sb/kg and 368 mg Zn/kg. The leaching process consisted of five one-hour acid leaching steps, which used 1 M H2SO4 + 4 M NaCl (20 degrees C, soil suspension = 100 g/L) followed by two water rinsing steps. Ten counter-current remediation cycles were completed and the average metal removal yields were 98.3 +/- 0.3% of Cu, 99.5 +/- 0.1% of Pb, 75.5 +/- 5.1% of Sb and 29.1 +/- 27.2% of Zn. The quality of metal leaching did not deteriorate throughout the 10 remediation cycles completed for this study. The CCLP reduced acid and salt use by approximately 68% and reduced water consumption by approximately 60%, exceeding reductions achieved by a standard acid leaching process.

Counter-current thermocapillary migration of bubbles in self-rewetting liquids

NASA Astrophysics Data System (ADS)

Nazareth, R.; Saenz, P.; Sefiane, K.; Kim, J.; Valluri, P.

2016-11-01

In this work, we study the counter-current thermocapillary propulsion of a suspended bubble in the fluid flowing inside a channel subject to an axial temperature gradient when the surface tension dependence on temperature is non-monotonic. We use direct numerical simulations to address the two-phase conservation of mass, momentum and energy with a volume-of-fluid method to resolve the deformable interface. Two distinct regimes of counter-current bubble migration are characterized: i) "exponential decay" where the bubble decelerates rapidly until it comes to a halt at the spatial position corresponding to the minimum surface tension and ii) "sustained oscillations" where the bubble oscillates about the point of minimum surface tension. We illustrate how these sustained oscillations arise at low capillary number O(10-5) and moderate Reynolds number O(10) and, they are dampened by viscosity at lower Reynolds number. These results are in agreement with the experiments by Shanahan and Sefiane (Sci. Rep. 4, 2014). The work was supported by the Science without Borders program from CAPES agency of Brazilian Ministry of Education and the European Commission's Thermapower Project (294905).

Schinus terebinthifolius countercurrent chromatography (Part III): Method transfer from small countercurrent chromatography column to preparative centrifugal partition chromatography ones as a part of method development.

PubMed

das Neves Costa, Fernanda; Hubert, Jane; Borie, Nicolas; Kotland, Alexis; Hewitson, Peter; Ignatova, Svetlana; Renault, Jean-Hugues

2017-03-03

Countercurrent chromatography (CCC) and centrifugal partition chromatography (CPC) are support free liquid-liquid chromatography techniques sharing the same basic principles and features. Method transfer has previously been demonstrated for both techniques but never from one to another. This study aimed to show such a feasibility using fractionation of Schinus terebinthifolius berries dichloromethane extract as a case study. Heptane - ethyl acetate - methanol -water (6:1:6:1, v/v/v/v) was used as solvent system with masticadienonic and 3β-masticadienolic acids as target compounds. The optimized separation methodology previously described in Part I and II, was scaled up from an analytical hydrodynamic CCC column (17.4mL) to preparative hydrostatic CPC instruments (250mL and 303mL) as a part of method development. Flow-rate and sample loading were further optimized on CPC. Mobile phase linear velocity is suggested as a transfer invariant parameter if the CPC column contains sufficient number of partition cells. Copyright © 2017 Elsevier B.V. All rights reserved.

Purification of semiconducting single-walled carbon nanotubes by spiral counter-current chromatography.

PubMed

Knight, Martha; Lazo-Portugal, Rodrigo; Ahn, Saeyoung Nate; Stefansson, Steingrimur

2017-02-03

Over the last decade man-made carbon nanostructures have shown great promise in electronic applications, but they are produced as very heterogeneous mixtures with different properties so the achievement of a significant commercial application has been elusive. The dimensions of single-wall carbon nanotubes are generally a nanometer wide, up to hundreds of microns long and the carbon nanotubes have anisotropic structures. They are processed to have shorter lengths but they need to be sorted by diameter and chirality. Thus counter-current chromatography methods developed for large molecules are applied to separate these compounds. A modified mixer-settler spiral CCC rotor made with 3 D printed disks was used with a polyethylene glycol-dextran 2-phase solvent system and a surfactant gradient to purify the major species in a commercial preparation. We isolated the semi-conducting single walled carbon nanotube chiral species identified by UV spectral analysis. The further development of spiral counter-current chromatography instrumentation and methods will enable the scalable purification of carbon nanotubes useful for the next generation electronics. Copyright © 2016 Elsevier B.V. All rights reserved.

Isolation and purification of arctigenin from Fructus Arctii by enzymatic hydrolysis combined with high-speed counter-current chromatography.

PubMed

Liu, Feng; Xi, Xingjun; Wang, Mei; Fan, Li; Geng, Yanling; Wang, Xiao

2014-02-01

Enzymatic hydrolysis pretreatment combined with high-speed counter-current chromatography for the transformation and isolation of arctigenin from Fructus Arctii was successfully developed. In the first step, the extract solution of Fructus Arctii was enzymatic hydrolyzed by β-glucosidase. The optimal hydrolysis conditions were 40°C, pH 5.0, 24 h of hydrolysis time, and 1.25 mg/mL β-glucosidase concentration. Under these conditions, the content of arctigenin was transformed from 2.60 to 12.59 mg/g. In the second step, arctigenin in the hydrolysis products was separated and purified by high-speed counter-current chromatography with a two-phase solvent system composed of petroleum ether/ethyl acetate/methanol/water (10:25:15:20, v/v), and the fraction was analyzed by HPLC, ESI-MS, and (1)H NMR spectroscopy. Finally, 102 mg of arctigenin with a purity of 98.9% was obtained in a one-step separation from 200 mg of hydrolyzed sample. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ionic Liquid-Liquid Chromatography: A New General Purpose Separation Methodology.

PubMed

Brown, Leslie; Earle, Martyn J; Gîlea, Manuela A; Plechkova, Natalia V; Seddon, Kenneth R

2017-08-10

Ionic liquids can form biphasic solvent systems with many organic solvents and water, and these solvent systems can be used in liquid-liquid separations and countercurrent chromatography. The wide range of ionic liquids that can by synthesised, with specifically tailored properties, represents a new philosophy for the separation of organic, inorganic and bio-based materials. A customised countercurrent chromatograph has been designed and constructed specifically to allow the more viscous character of ionic liquid-based solvent systems to be used in a wide variety of separations (including transition metal salts, arenes, alkenes, alkanes, bio-oils and sugars).

VALIDATION FOR THE PERMANGANATE DIGESTION OF REILLEX HPQ ANION RESIN

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

Kyser, E.

2009-09-23

The flowsheet for the digestion of Reillex{trademark} HPQ was validated both under the traditional alkaline conditions and under strongly acidic conditions. Due to difficulty in performing a pH adjustment in the large tank where this flowsheet must be performed, the recommended digestion conditions were changed from pH 8-10 to 8 M HNO{sub 3}. Thus, no pH adjustment of the solution is required prior to performing the permanganate addition and digestion and the need to sample the digestion tank to confirm appropriate pH range for digestion may be avoided. Neutralization of the acidic digestion solution will be performed after completion ofmore » the resin digestion cycle. The amount of permanganate required for this type of resin (Reillex{trademark} HPQ) was increased from 1 kg/L resin to 4 kg/L resin to reduce the amount of residual resin solids to a minimal amount (<5%). The length of digestion time at 70 C remains unchanged at 15 hours. These parameters are not optimized but are expected to be adequate for the conditions. The flowsheet generates a significant amount of fine manganese dioxide (MnO{sub 2}) solids (1.71 kg/L resin) and involves the generation of a significant liquid volume due to the low solubility of permanganate. However, since only two batches of resin (40 L each) are expected to be digested, the total waste generated is limited.« less

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

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

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

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

High Throughput Method of Extracting and Counting Strontium-90 in Urine

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

Shkrob, I.; Kaminski, M.; Mertz, C.

2016-03-01

A method has been developed for the rapid extraction of Sr-90 from the urine of individuals exposed to radiation in a terrorist attack. The method employs two chromatographic ion-exchange materials: Diphonix resin and Sr resin, both of which are commercially available. The Diphonix resin reduces the alkali ion concentrations below 10 mM, and the Sr resin concentrates and decontaminates strontium-90. Experimental and calculational data are given for a variety of test conditions. On the basis of these results, a flowsheet has been developed for the rapid concentration and extraction of Sr-90 from human urine samples for subsequent beta-counting.

Qualitative and quantitative evaluation of solvent systems for countercurrent separation.

PubMed

Friesen, J Brent; Ahmed, Sana; Pauli, Guido F

2015-01-16

Rational solvent system selection for countercurrent chromatography and centrifugal partition chromatography technology (collectively known as countercurrent separation) studies continues to be a scientific challenge as the fundamental questions of comparing polarity range and selectivity within a solvent system family and between putative orthogonal solvent systems remain unanswered. The current emphasis on metabolomic investigations and analysis of complex mixtures necessitates the use of successive orthogonal countercurrent separation (CS) steps as part of complex fractionation protocols. Addressing the broad range of metabolite polarities demands development of new CS solvent systems with appropriate composition, polarity (π), selectivity (σ), and suitability. In this study, a mixture of twenty commercially available natural products, called the GUESSmix, was utilized to evaluate both solvent system polarity and selectively characteristics. Comparisons of GUESSmix analyte partition coefficient (K) values give rise to a measure of solvent system polarity range called the GUESSmix polarity index (GUPI). Solvatochromic dye and electrical permittivity measurements were also evaluated in quantitatively assessing solvent system polarity. The relative selectivity of solvent systems were evaluated with the GUESSmix by calculating the pairwise resolution (αip), the number of analytes found in the sweet spot (Nsw), and the pairwise resolution of those sweet spot analytes (αsw). The combination of these parameters allowed for both intra- and inter-family comparison of solvent system selectivity. Finally, 2-dimensional reciprocal shifted symmetry plots (ReSS(2)) were created to visually compare both the polarities and selectivities of solvent system pairs. This study helps to pave the way to the development of new solvent systems that are amenable to successive orthogonal CS protocols employed in metabolomic studies. Copyright © 2014 Elsevier B.V. All rights reserved.

Dynamic pH junction high-speed counter-current chromatography coupled with microwave-assisted extraction for online separation and purification of alkaloids from Stephania cepharantha.

PubMed

Yuan, Zhiquan; Xiao, Xiaohua; Li, Gongke

2013-11-22

A simple and efficient dynamic pH junction high-speed counter-current chromatography method was developed and further applied to the online extraction, separation and purification of alkaloids from Stephania cepharantha by coupling with microwave-assisted extraction. Mineral acid and organic base were added into the mobile phase and the sample solution, respectively, leading to the formation of a dynamic pH junction in the column and causing focus of alkaloids. Selective focus of analytes can be achieved on the basis of velocity changes of the pH junction through appropriate selection of solvent systems and optimization of additive concentrations. The extract can be directly introduced into the HSCCC for the online extraction, separation and purification of alkaloids from S. cepharantha. Continuous separation can be easily achieved with the same solvent system. Under the optimum conditions, 6.0 g original sample was extracted with 60 mL of the upper phase of hexane-ethyl acetate-methanol-water (1:1:1:1, v/v/v/v) containing 10% triethylamine under 50 °C and 400 W irradiation power for 10 min, the extracts were directly separated and purified by high-speed counter-current chromatography. A total of 5.7 mg sinomenine, 8.3mg 6,7-di-O-acetylsinococuline, 17.9 mg berbamine, 12.7 mg isotetrandrine and 14.6 mg cepharanthine were obtained with purities of 96.7%, 93.7%, 98.7%, 97.3% and 99.3%, respectively. The online method provides good selectivity to ionizable compounds and improves the separation and purification efficiency of the high-speed counter-current chromatography technique. It has good potential for separation and purification of effective compounds from natural products. Copyright © 2013 Elsevier B.V. All rights reserved.

Development of Crystallizer for Advanced Aqueous Reprocessing Process

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

Tadahiro Washiya; Atsuhiro Shibata; Toshiaki Kikuchi

2006-07-01

Crystallization is one of the remarkable technologies for future fuel reprocessing process that has safety and economical advantages. Japan Atomic Energy Agency (JAEA) (former Japan Nuclear Cycle Development Institute), Mitsubishi Material Corporation and Saitama University have been developing the crystallization process. In previous study, we carried out experimental studies with uranium, MOX and spent fuel conditions, and flowsheet analysis was considered. In association with these studies, an innovative continuous crystallizer and its system was developed to ensure high process performance. From the design study, an annular type continuous crystallizer was selected as the most promising design, and performance was confirmedmore » by small-scale test and engineering scale demonstration at uranium crystallization conditions. In this paper, the design study and the demonstration test results are described. (authors)« less

Spiral Countercurrent Chromatography

PubMed Central

Ito, Yoichiro; Knight, Martha; Finn, Thomas M.

2013-01-01

For many years, high-speed countercurrent chromatography conducted in open tubing coils has been widely used for the separation of natural and synthetic compounds. In this method, the retention of the stationary phase is solely provided by the Archimedean screw effect by rotating the coiled column in the centrifugal force field. However, the system fails to retain enough of the stationary phase for polar solvent systems such as the aqueous–aqueous polymer phase systems. To address this problem, the geometry of the coiled channel was modified to a spiral configuration so that the system could utilize the radially acting centrifugal force. This successfully improved the retention of the stationary phase. Two different types of spiral columns were fabricated: the spiral disk assembly, made by stacking multiple plastic disks with single or four interwoven spiral channels connected in series, and the spiral tube assembly, made by inserting the tetrafluoroethylene tubing into a spiral frame (spiral tube support). The capabilities of these column assemblies were successfully demonstrated by separations of peptides and proteins with polar two-phase solvent systems whose stationary phases had not been well retained in the earlier multilayer coil separation column for high-speed countercurrent chromatography. PMID:23833207

An easy-to-use calculating machine to simulate steady state and non-steady-state preparative separations by multiple dual mode counter-current chromatography with semi-continuous loading of feed mixtures.

PubMed

Kostanyan, Artak E; Shishilov, Oleg N

2018-06-01

Multiple dual mode counter-current chromatography (MDM CCC) separation processes with semi-continuous large sample loading consist of a succession of two counter-current steps: with "x" phase (first step) and "y" phase (second step) flow periods. A feed mixture dissolved in the "x" phase is continuously loaded into a CCC machine at the beginning of the first step of each cycle over a constant time with the volumetric rate equal to the flow rate of the pure "x" phase. An easy-to-use calculating machine is developed to simulate the chromatograms and the amounts of solutes eluted with the phases at each cycle for steady-state (the duration of the flow periods of the phases is kept constant for all the cycles) and non-steady-state (with variable duration of alternating phase elution steps) separations. Using the calculating machine, the separation of mixtures containing up to five components can be simulated and designed. Examples of the application of the calculating machine for the simulation of MDM CCC processes are discussed. Copyright © 2018 Elsevier B.V. All rights reserved.

Proposal for a new CAPE-OPEN Object Model

EPA Science Inventory

Process simulation applications require the exchange of significant amounts of data between the flowsheet environment, unit operation model, and thermodynamic server. Packing and unpacking various data types and exchanging data using structured text-based architectures, including...

Chemical Dissolution of Simulant FCA Cladding and Plates

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

Daniel, G.; Pierce, R.; O'Rourke, P.

The Savannah River Site (SRS) has received some fast critical assembly (FCA) fuel from the Japan Atomic Energy Agency (JAEA) for disposition. Among the JAEA FCA fuel are approximately 7090 rectangular Stainless Steel clad fuel elements. Each element has an internal Pu-10.6Al alloy metal wafer. The thickness of each element is either 1/16 inch or 1/32 inch. The dimensions of each element ranges from 2 inches x 1 inch to 2 inches x 4 inches. This report discusses the potential chemical dissolution of the FCA clad material or stainless steel. This technology uses nitric acid-potassium fluoride (HNO 3-KF) flowsheets ofmore » H-Canyon to dissolve the FCA elements from a rack of materials. Historically, dissolution flowsheets have aimed to maximize Pu dissolution rates while minimizing stainless steel dissolution (corrosion) rates. Because the FCA cladding is made of stainless steel, this work sought to accelerate stainless steel dissolution.« less

Evolution of an Implementation-Ready Interprofessional Pain Assessment Reference Model

PubMed Central

Collins, Sarah A; Bavuso, Karen; Swenson, Mary; Suchecki, Christine; Mar, Perry; Rocha, Roberto A.

2017-01-01

Standards to increase consistency of comprehensive pain assessments are important for safety, quality, and analytics activities, including meeting Joint Commission requirements and learning the best management strategies and interventions for the current prescription Opioid epidemic. In this study we describe the development and validation of a Pain Assessment Reference Model ready for implementation on EHR forms and flowsheets. Our process resulted in 5 successive revisions of the reference model, which more than doubled the number of data elements to 47. The organization of the model evolved during validation sessions with panels totaling 48 subject matter experts (SMEs) to include 9 sets of data elements, with one set recommended as a minimal data set. The reference model also evolved when implemented into EHR forms and flowsheets, indicating specifications such as cascading logic that are important to inform secondary use of data. PMID:29854125

Process feasibility study in support of silicon material task 1

NASA Technical Reports Server (NTRS)

Fang, C. S.; Hansen, K. C.; Miller, J. W., Jr.; Yaws, C. L.

1978-01-01

Initial results for gas thermal conductivity of silicon tetrafluoride and trichlorosilane are reported in respective temperature ranges of 25 to 400 C and 50 to 400 C. For chemical engineering analyses, the preliminary process design for the original silane process of Union Carbide was completed for Cases A and B, Regular and Minimum Process Storage. Included are raw material usage, utility requirements, major process equipment lists, and production labor requirements. Because of the large differences in surge tankage between major unit operations the fixed capital investment varied from $19,094,000 to $11,138,000 for Cases A and B, respectively. For the silane process the original flowsheet was revised for a more optimum arrangement of major equipment, raw materials and operating conditions. The initial issue of the revised flowsheet (Case C) for the silane process indicated favorable cost benefits over the original scheme.

Sample selection and testing of separation processes

NASA Technical Reports Server (NTRS)

Karr, L. J.

1985-01-01

Phase partitioning, which has become an important tool for the separation and purification of biological materials, was studied. Instruments available for this technique were researched and a countercurrent distribution apparatus, the Biosheff MK2N, was purchased. Various proteins, polysaccharides and cells were studied as models to determine operating procedures and conditions for this piece of equipment. Results were compared with those obtained from other similar equipment, including a nonsynchronous coil planet centrifuge device. Additionally, work was done with affinity ligands attached to PEG, which can further enhance the separation capabilities of phase partitioning.

Isolation of a polysaccharide with anticancer activity from Auricularia polytricha using high-speed countercurrent chromatography with an aqueous two-phase system.

PubMed

Song, Guanglei; Du, Qizhen

2010-09-17

Polysaccharides from a crude extract of Auricularia polytricha were separated by high-speed countercurrent chromatography (HSCCC). The separation was performed with an aqueous two-phase system of PEG1000-K2HPO4-KH2PO4-H2O (0.5:1.25:1.25:7.0, w/w). The crude sample (2.0 g) was successfully separated into three polysaccharide components of AAPS-1 (192 mg), AAPS-2 (137 mg), and AAPS-3 (98 mg) with molecular weights of 162, 259, and 483 kDa, respectively. These compounds were tested for growth inhibition of transplanted S180 sarcoma in mice. AAPS-2 had an inhibition rate of 40.4%. The structure of AAPS-2 was elucidated from partial hydrolysis, periodate oxidation, acetylation, methylation analysis, and NMR spectroscopy (1H, 13C). These results showed AAPS-2 is a polysaccharide with a backbone of (1-->3)-linked-beta-d-glucopyranosyl and (1-->3, 6)-linked-beta-D-glucopyranosyl residues in a 2:1 ratio, and has one terminal (1-->)-beta-D-glucopyranosyl at the O-6 position of (1-->3, 6)-linked-beta-D-glucopyranosyl of the main chain. 2010 Elsevier B.V. All rights reserved.

Isolation of Flavonoids From Wild Aquilaria sinensis Leaves by an Improved Preparative High-Speed Counter-Current Chromatography Apparatus.

PubMed

Yang, Mao-Xun; Liang, Yao-Guang; Chen, He-Ru; Huang, Yong-Fang; Gong, Hai-Guang; Zhang, Tian-You; Ito, Yoichiro

2018-01-01

Four flavonoids including apigenin-7,4'-dimethylether, genkwanin, quercetin, and kaempferol were isolated in a preparative or semi-preparative scale from the leaves of wild Aquilaria sinensis using an improved preparative high-speed counter-current chromatography apparatus. The separations were performed with a two-phase solvent system composed of hexane-ethyl acetate, methanol-water at suitable volume ratios. The obtained fractions were analyzed by HPLC, and the identification of each target compound was carried out by ESI-MS and NMR. The yields of the above four target flavonoids were 4.7, 10.0, 11.0 and 4.4%, respectively. All these four flavonoids exhibited nitrite scavenging activities with the clearance rate of 12.40 ± 0.20%, 5.84 ± 0.03%, 28.10 ± 0.17% and 5.19 ± 0.11%, respectively. Quercetin was originally isolated from the Thymelaeaceae family, while kaempferol was isolated from the Aquilaria genus for the first time. In cytotoxicity test these two flavonoids exhibited moderate inhibitory activities against HepG2 cells with the IC50 values of 12.54 ± 1.37 and 38.63 ± 4.05 μM, respectively. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

OPTIMIZATION OF COUNTERCURRENT STAGED PROCESSES.

DTIC Science & Technology

CHEMICAL ENGINEERING , OPTIMIZATION), (*DISTILLATION, OPTIMIZATION), INDUSTRIAL PRODUCTION, INDUSTRIAL EQUIPMENT, MATHEMATICAL MODELS, DIFFERENCE EQUATIONS, NONLINEAR PROGRAMMING, BOUNDARY VALUE PROBLEMS, NUMERICAL INTEGRATION

Use of Electronic Health Record Tools to Facilitate and Audit Infliximab Prescribing.

PubMed

Sharpless, Bethany R; Del Rosario, Fernando; Molle-Rios, Zarela; Hilmas, Elora

2018-01-01

The objective of this project was to assess a pediatric institution's use of infliximab and develop and evaluate electronic health record tools to improve safety and efficiency of infliximab ordering through auditing and improved communication. Best use of infliximab was defined through a literature review, analysis of baseline use of infliximab at our institution, and distribution and analysis of a national survey. Auditing and order communication were optimized through implementation of mandatory indications in the infliximab orderable and creation of an interactive flowsheet that collects discrete and free-text data. The value of the implemented electronic health record tools was assessed at the conclusion of the project. Baseline analysis determined that 93.8% of orders were dosed appropriately according to the findings of a literature review. After implementation of the flowsheet and indications, the time to perform an audit of use was reduced from 60 minutes to 5 minutes per month. Four months post implementation, data were entered by 60% of the pediatric gastroenterologists at our institution on 15.3% of all encounters for infliximab. Users were surveyed on the value of the tools, with 100% planning to continue using the workflow, and 82% stating the tools frequently improve the efficiency and safety of infliximab prescribing. Creation of a standard workflow by using an interactive flowsheet has improved auditing ability and facilitated the communication of important order information surrounding infliximab. Providers and pharmacists feel these tools improve the safety and efficiency of infliximab ordering, and auditing data reveal that the tools are being used.

Investigation of different ethylenediamine-N,N'-disuccinic acid-enhanced washing configurations for remediation of a Cu-contaminated soil: process kinetics and efficiency comparison between single-stage and multi-stage configurations.

PubMed

Ferraro, Alberto; Fabbricino, Massimiliano; van Hullebusch, Eric D; Esposito, Giovanni

2017-09-01

A comparison of Cu extraction yields for three different ethylenediamine-N,N'-disuccinic acid (EDDS)-enhanced washing configurations was performed on a Cu-contaminated soil. Batch experiments were used to simulate a single-stage continuous stirred tank reactor (CSTR) and a multi-stage (side feeding and counter-current) reactor. Single-stage CSTR conditions were simulated for various EDDS:(Cu + Cd + Pb + Co + Ni + Zn) molar ratio (EDDS:M ratio) (from 1 to 30) and liquid to soil (L/S) ratio (from 15 to 45). The highest Cu extraction yield (≃56%) was achieved with EDDS:M = 30. In contrast, a Cu extraction yield decrease was observed with increasing L/S ratio with highest extracted Cu achievement (≃48%) for L/S = 15. Side feeding configuration was tested in four experimental conditions through different fractionation mode of EDDS dose and treatment time at each washing step. Results from the four tests showed all enhanced Cu extraction (maximum values from ≃43 to ≃51%) achieved at lower treatment time and lower EDDS:M molar ratio compared to CSTR configuration with L/S = 25 and EDDS:M = 10. The counter-current washing was carried out through two washing flows achieving a process performance enhancement with 27% increase of extracted Cu compared to single-stage CSTR configuration. Higher Cu extraction percentage (36.8%) was observed in the first washing phase than in the second one (24.7%).

Separation of chlorogenic acid and concentration of trace caffeic acid from natural products by pH-zone-refining countercurrent chromatography.

PubMed

Lu, Yuanyuan; Dong, Genlai; Gu, Yanxiang; Ito, Yoichiro; Wei, Yun

2013-07-01

Chlorogenic acid and caffeic acid were selected as test samples for separation by the pH-zone-refining countercurrent chromatography (CCC). The separation of these test samples was performed with a two-phase solvent system composed of methyl-tert-butyl-ether/acetonitrile/water at a volume ratio of 4:1:5 v/v/v where trifluoroacetic acid (TFA; 8 mM) was added to the organic stationary phase as a retainer and NH4 OH (10 mM) to the aqueous mobile phase as an eluter. Chlorogenic acid was successfully separated from Flaveria bidentis (L.) Kuntze (F. bidentis) and Lonicerae Flos by pH-zone-refining CCC, a slightly polar two-phase solvent system composed of methyl-tert-butyl-ether/acetonitrile/n-butanol/water at a volume ratio of 4:1:1:5 v/v/v/v was selected where TFA (3 mM) was added to the organic stationary phase as a retainer and NH4 OH (3 mM) to the aqueous mobile phase as an eluter. A 16.2 mg amount of chlorogenic acid with the purity of 92% from 1.4 g of F. bidentis, and 134 mg of chlorogenic acid at the purity of 99% from 1.3 g of crude extract of Lonicerae Flos have been obtained. These results suggest that pH-zone-refining CCC is suitable for the isolation of the chlorogenic acid from the crude extracts of F. bidentis and Lonicerae Flos. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparative isolation and purification of indigo and indirubin from Folium isatidis by high-speed counter-current chromatography.

PubMed

Lü, Hai-tao; Liu, Jing; Deng, Rui; Song, Ji-ying

2012-01-01

Indigo and indirubin are the main active ingredients found in traditional Chinese herbal medicine Folium isatidis. An effective method for the isolation and purification of indigo and indirubin from Folium isatidis is needed. Compared with the conventional column chromatographic techniques, high-speed counter-current chromatography (HSCCC) is a suitable alternative for the enrichment and purification of these target compounds, and eliminates the complications resulting from a solid support matrix. To develop a reliable HSCCC method for isolation and identification of indigo and indirubin in a one-step separation from Folium isatidis. The optimum extracting conditions of indigo and indirubin from Folium isatidis were investigated by orthogonal test L(16) (4(5)). The target compounds were isolated and purified with a solvent system of n-hexane:ethyl acetate:ethanol:water (1:1:1:1, v/v) and the lower phase was used as the mobile phase in the head-to-tail elution mode. The purities of target compounds were tested by HPLC and their structures were identified by UV, IR, electrospray ion source (ESI)-MS, (1) H-NMR and (13) C-NMR analyses. From 165 mg of the crude extract, 5.65 mg of indigo and 1.00 mg of indirubin were obtained by HPLC analysis with purities of 98.4% and 99.0% respectively, and their mean recoveries were 91.0% and 90.7%, respectively. The HSCCC method is effective for the preparative separation and purification of indigo and indirubin in a one-step separation from Folium isatidis. Copyright © 2012 John Wiley & Sons, Ltd.

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

Stoltzfus-Dueck, T.; Scott, B.

An often-neglected portion of the radialmore » $$\\boldsymbol{E}\\times \\boldsymbol{B}$$ drift is shown to drive an outward flux of co-current momentum when free energy is transferred from the electrostatic potential to ion parallel flows. This symmetry breaking is fully nonlinear, not quasilinear, necessitated simply by free-energy balance in parameter regimes for which significant energy is dissipated via ion parallel flows. The resulting rotation peaking is counter-current and has a scaling and order of magnitude that are comparable with experimental observations. Finally, the residual stress becomes inactive when frequencies are much higher than the ion transit frequency, which may explain the observed relation of density peaking and counter-current rotation peaking in the core.« less

Preparative high-speed counter-current chromatography for purification of shikonin from the Chinese medicinal plant Lithospermum erythrorhizon.

PubMed

Lu, Hai-Tao; Jiang, Yue; Chen, Feng

2004-01-09

The bioactive compound shikonin was successfully isolated and purified from the crude extract of the traditional Chinese medicinal plant Lithospermum erythrorhizon Sieb. et Zucc. by preparative high-speed counter-current chromatography (HSCCC). The preparative HSCCC was performed using a two-phase solvent system composed of n-hexane-ethylacetate-ethanol-water (16:14:14:5 (v/v)). A total amount of 19.6 mg of shikonin at 98.9% purity was obtained from 52 mg of the crude extract (containing 38.9% shikonin) with 96.9% recovery. The preparative isolation and purification of shikonin by HSCCC was completed in 200 min in a one-step separation.

Evaluating Process Sustainability Using Flowsheet Monitoring

EPA Science Inventory

Environmental metric software can be used to evaluate the sustainability of a chemical based on data from the chemical process that is used to manufacture it. One problem in developing environmental metric software is that chemical process simulation packages typically do not rea...

The Medical Gopher — A Microcomputer Based Physician Work Station

PubMed Central

McDonald, Clement J.

1984-01-01

We've developed a microcomputer medical work station intended to reduce the physician's “gopher” work of fetching, reviewing, organizing and writing that consumes his day. The system requires extensive physician interaction; so we have developed a fast and consistent menu-oriented user interface. It provides facilities for entering prescriptions, orders, problems and other medical record information and for generating flowsheets, executing reminder rules, providing ad hoc retrievals and reporting facts about drugs, tests and differential diagnoses. Each work station is connected to a central server (currently a VAX 117/80) in a network configuration, but carries all of its own programs, tables and medical records for a few hundred patients, locally. This system is tested but not yet tried. Questions remain about physician's acceptance and the true usefullness of such a work station.

Intracellular Calcium Release Channels Mediate Their Own Countercurrent: The Ryanodine Receptor Case Study

PubMed Central

Gillespie, Dirk; Fill, Michael

2008-01-01

Intracellular calcium release channels like ryanodine receptors (RyRs) and inositol trisphosphate receptors (IP3Rs) mediate large Ca2+ release events from Ca2+ storage organelles lasting >5 ms. To have such long-lasting Ca2+ efflux, a countercurrent of other ions is necessary to prevent the membrane potential from becoming the Ca2+ Nernst potential in <1 ms. A recent model of ion permeation through a single, open RyR channel is used here to show that the vast majority of this countercurrent is conducted by the RyR itself. Consequently, changes in membrane potential are minimized locally and instantly, assuring maintenance of a Ca2+-driving force. This RyR autocountercurrent is possible because of the poor Ca2+ selectivity and high conductance for both monovalent and divalent cations of these channels. The model shows that, under physiological conditions, the autocountercurrent clamps the membrane potential near 0 mV within ∼150 μs. Consistent with experiments, the model shows how RyR unit Ca2+ current is defined by luminal [Ca2+], permeable ion composition and concentration, and pore selectivity and conductance. This very likely is true of the highly homologous pore of the IP3R channel. PMID:18621826

Separation and purification of four flavonol diglucosides from the flower of Meconopsis integrifolia by high-speed counter-current chromatography.

PubMed

Huang, Yanfei; Han, Yatao; Chen, Keli; Huang, Bisheng; Liu, Yuan

2015-12-01

Flavonoids are the main components of Meconopsis integrifolia (Maxim.) Franch, which is a traditional Tibetan medicine. However, traditional chromatography separation requires a large quantity of raw M. integrifolia and is very time consuming. Herein, we applied high-speed counter-current chromatography in the separation and purification of flavonoids from the ethanol extracts of M. integrifolia flower. Ethyl acetate/n-butanol/water (2:3:5, v/v/v) was selected as the optimum solvent system to purify the four components, namely quercetin-3-O-β-d-glucopyrannosy-(1→6)-β-d-glucopyranoside (compound 1, 60 mg), quercetin 3-O-[2'''-O-acetyl-β-d-glucopyranosyl-(1→6)-β-d-glucopyranoside (compound 2, 40 mg), quercetin 3-O-[3'''-O-acetyl-β-d-glucopyranosyl-(1→6)-β-d-glucopyranoside (compound 3, 11 mg), and quercetin 3-O-[6'''-O-acetyl-β-d-glucopyranosyl-(1→6)-β-d-glucopyranoside (compound 4, 16 mg). Among the four compounds, 3 and 4 were new acetylated flavonol diglucosides. After the high-speed counter-current chromatography separation, the purities of the four flavonol diglucosides were 98, 95, 90, and 92%, respectively. The structures of these compounds were identified by mass spectrometry and NMR spectroscopy. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effects of dialysate flow configurations in continuous renal replacement therapy on solute removal: computational modeling.

PubMed

Kim, Jeong Chul; Cruz, Dinna; Garzotto, Francesco; Kaushik, Manish; Teixeria, Catarina; Baldwin, Marie; Baldwin, Ian; Nalesso, Federico; Kim, Ji Hyun; Kang, Eungtaek; Kim, Hee Chan; Ronco, Claudio

2013-01-01

Continuous renal replacement therapy (CRRT) is commonly used for critically ill patients with acute kidney injury. During treatment, a slow dialysate flow rate can be applied to enhance diffusive solute removal. However, due to the lack of the rationale of the dialysate flow configuration (countercurrent or concurrent to blood flow), in clinical practice, the connection settings of a hemodiafilter are done depending on nurse preference or at random. In this study, we investigated the effects of flow configurations in a hemodiafilter during continuous venovenous hemodialysis on solute removal and fluid transport using computational fluid dynamic modeling. We solved the momentum equation coupling solute transport to predict quantitative diffusion and convection phenomena in a simplified hemodiafilter model. Computational modeling results showed superior solute removal (clearance of urea: 67.8 vs. 45.1 ml/min) and convection (filtration volume: 29.0 vs. 25.7 ml/min) performances for the countercurrent flow configuration. Countercurrent flow configuration enhances convection and diffusion compared to concurrent flow configuration by increasing filtration volume and equilibrium concentration in the proximal part of a hemodiafilter and backfiltration of pure dialysate in the distal part. In clinical practice, the countercurrent dialysate flow configuration of a hemodiafilter could increase solute removal in CRRT. Nevertheless, while this configuration may become mandatory for high-efficiency treatments, the impact of differences in solute removal observed in slow continuous therapies may be less important. Under these circumstances, if continuous therapies are prescribed, some of the advantages of the concurrent configuration in terms of simpler circuit layout and simpler machine design may overcome the advantages in terms of solute clearance. Different dialysate flow configurations influence solute clearance and change major solute removal mechanisms in the proximal and distal parts of a hemodiafilter. Advantages of each configuration should be balanced against the overall performance of the treatment and its simplicity in terms of treatment delivery and circuit handling procedures. Copyright © 2013 S. Karger AG, Basel.

Evaluating Process Sustainability Using Flowsheet Monitoring (Abstract)

EPA Science Inventory

Environmental metric software can be used to evaluate the sustainability of a chemical based upon data from the chemical process that is used to manufacture it. One problem in developing environmental metric software is that chemical process simulation packages typically do not p...

Quality improvement tools for chronic disease care--more effective processes are less likely to be implemented in developing countries.

PubMed

Hashim, Muhammad Jawad; Prinsloo, Adrianna; Mirza, Deen M

2013-01-01

Chronic disease services may be improved if care management processes (CMPs), such as disease-specific flowsheets and chronic disease registries, are used. The newly industrialized Gulf state health service has underdeveloped primary care but higher diabetes prevalence. This paper's aim is to investigate care management processes in United Arab Emirates (UAE) primary care clinics to explore these issues. A cross-sectional survey using self-administered questionnaires given to family physicians and nurses attending a UAE University workshop was used to collect data. All 38 participants completed the questionnaire: 68 per cent were women and 81 per cent physicians. Care management processes in use included: medical records, 76 per cent; clinical guidelines, 74 per cent; chronic disease care rooms, 74 per cent; disease-specific flowsheets, 61 per cent; medical record audits, 57 per cent; chronic disease nurse-educators, 58 per cent; electronic medical records (EMR), 34 per cent; and incentive plans based on clinical performance, 21 per cent. Only 62 per cent and 48 per cent reported that flowsheets and problem lists, respectively, were completed by physicians. Responses to the open-ended question included using traditional quality improvement (QI) approaches such as continuing education and staff meetings, but not proactive systems such as disease registries and self-management. The study used a small, non-random sample and the survey instrument's psychometric properties were not collected. Chronic disease care CMPs are present in UAE clinics but use is limited. Quality improvement should include disease registries, reminder-tracking systems, patient self-management support and quality incentives. This report highlights the lag regarding adopting more effective CMPs in developing countries.

Momentum flux parasitic to free-energy transfer

DOE PAGES

Stoltzfus-Dueck, T.; Scott, B.

2017-05-11

An often-neglected portion of the radialmore » $$\\boldsymbol{E}\\times \\boldsymbol{B}$$ drift is shown to drive an outward flux of co-current momentum when free energy is transferred from the electrostatic potential to ion parallel flows. This symmetry breaking is fully nonlinear, not quasilinear, necessitated simply by free-energy balance in parameter regimes for which significant energy is dissipated via ion parallel flows. The resulting rotation peaking is counter-current and has a scaling and order of magnitude that are comparable with experimental observations. Finally, the residual stress becomes inactive when frequencies are much higher than the ion transit frequency, which may explain the observed relation of density peaking and counter-current rotation peaking in the core.« less

Preparative isolation and purification of three sesquiterpenoid lactones from Eupatorium lindleyanum DC. by high-speed counter-current chromatography.

PubMed

Yan, Guilong; Ji, Lilian; Luo, Yuming; Hu, Yonghong

2012-07-27

A high-speed counter-current chromatography (HSCCC) method was established for the preparative separation of three sesquiterpenoid lactones from Eupatorium lindleyanum DC. The two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:4:2:3, v/v/v/v) was selected. From 540 mg of the n-butanol fraction of Eupatorium lindleyanum DC., 10.8 mg of 3β-hydroxy-8β-[4'-hydroxytigloyloxy]-costunolide, 17.9 mg of eupalinolide A and 19.3 mg of eupalinolide B were obtained in a one-step HSCCC separation, with purities of 91.8%, 97.9% and 97.1%, respectively, as determined by HPLC. Their structures were further identified by ESI-MS and ¹H-NMR.

Effect of magnetic field configuration on the multiply charged ion and plume characteristics in Hall thruster plasmas

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

Kim, Holak; Lim, Youbong; Choe, Wonho, E-mail: wchoe@kaist.ac.kr

2015-04-13

Multiply charged ions and plume characteristics in Hall thruster plasmas are investigated with regard to magnetic field configuration. Differences in the plume shape and the fraction of ions with different charge states are demonstrated by the counter-current and co-current magnetic field configurations, respectively. The significantly larger number of multiply charged and higher charge state ions including Xe{sup 4+} are observed in the co-current configuration than in the counter-current configuration. The large fraction of multiply charged ions and high ion currents in this experiment may be related to the strong electron confinement, which is due to the strong magnetic mirror effectmore » in the co-current magnetic field configuration.« less

Electric field-driven, magnetically-stabilized ferro-emulsion phase contactor

DOEpatents

Scott, T.C.

1990-07-17

Methods and systems are disclosed for interfacial surface area contact between a dispersed phase liquid and a continuous phase liquid in counter-current flow for purposes such as solvent extraction. Initial droplets of a dispersed phase liquid material containing ferromagnetic particles functioning as a packing'' are introduced to a counter-current flow of the continuous phase. A high intensity pulsed electric field is applied so as to shatter the initial droplets into a ferromagnetic emulsion comprising many smaller daughter droplets having a greater combined total surface area than that of the initial droplets in contact with the continuous phase material. A magnetic field is applied to control the position of the ferromagnetic emulsion for enhanced coalescence of the daughter droplets into larger reformed droplets. 2 figs.

Electric field-driven, magnetically-stabilized ferro-emulsion phase contactor

DOEpatents

Scott, Timothy C.

1990-01-01

Methods and systems for interfacial surface area contact between a dispersed phase liquid and a continuous phase liquid in counter-current flow for purposes such as solvent extraction. Initial droplets of a dispersed phase liquid material containing ferromagnetic particles functioning as a "packing" are introduced to a counter-current flow of the continuous phase. A high intensity pulsed electric field is applied so as to shatter the initial droplets into a ferromagnetic emulsion comprising many smaller daughter droplets having a greater combined total surface area than that of the initial droplets in contact with the continuous phase material. A magnetic field is applied to control the position of the ferromagnetic emulsion for enhanced coalescence of the daughter droplets into larger reformed droplets.

Two-step purification of scutellarin from Erigeron breviscapus (vant.) Hand. Mazz. by high-speed counter-current chromatography.

PubMed

Gao, Min; Gu, Ming; Liu, Chun-Zhao

2006-07-11

Scutellarin, a flavone glycoside, popularly applied for the treatment of cardiopathy, has been purified in two-step purification by high-speed counter-current chromatography (HSCCC) from Erigeron breviscapus (vant.) Hand. Mazz. (Deng-zhan-hua in Chinese), a well-known traditional Chinese medicinal plant for heart disease. Two solvent systems, n-hexane-ethyl acetate-methanol-acetic acid-water (1:6:1.5:1:4, v/v/v/v/v) and ethyl acetate-n-butanol-acetonitrile-0.1% HCl (5:2:5:10, v/v/v/v) were used for the two-step purification. The purity of the collected fraction of scutellarin was 95.6%. This study supplies a new alternative method for purification of scutellarin.

Recovery of magnetite from low grade banded magnetite quartzite (BMQ) ore

NASA Astrophysics Data System (ADS)

Tripathy, Alok; Bagchi, Subhankar; Rao, Danda Srinivas; Nayak, Bijaya Ketana; Rout, Prashanta Kumar; Biswal, Surendra Kumar

2018-04-01

There has been a steady increase of iron ore demand in the last few decades. This growing demand could be countered by use of low grade iron ore after beneficiation. Banded iron formations (BIF) are one of the resources of such low grade iron ores. Banded magnetite quartzite (BMQ) is one such BIF and a source of iron phase mineral in the form of magnetite. In the present study a low grade BMQ ore containing around 25.47% Fe was beneficiated for recovery of magnetite. XRD study shows that quartz, magnetite, hematite, and goethite are the major minerals phases present in the low grade BMQ sample. Unit operations such as crushing, scrubbing, grinding, and magnetic separations were used for recovering magnetite. Based on the large scale beneficiation studies the process flowsheet has been developed for enrichment of magnetite. It was found that with the help of developed process flowsheet it is possible to enrich Fe value up to 65.14% in the concentrate with a yield of 24.59%.

Defense Waste Processing Facility Nitric- Glycolic Flowsheet Chemical Process Cell Chemistry: Part 2

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

Zamecnik, J.; Edwards, T.

The conversions of nitrite to nitrate, the destruction of glycolate, and the conversion of glycolate to formate and oxalate were modeled for the Nitric-Glycolic flowsheet using data from Chemical Process Cell (CPC) simulant runs conducted by Savannah River National Laboratory (SRNL) from 2011 to 2016. The goal of this work was to develop empirical correlation models to predict these values from measureable variables from the chemical process so that these quantities could be predicted a-priori from the sludge or simulant composition and measurable processing variables. The need for these predictions arises from the need to predict the REDuction/OXidation (REDOX) statemore » of the glass from the Defense Waste Processing Facility (DWPF) melter. This report summarizes the work on these correlations based on the aforementioned data. Previous work on these correlations was documented in a technical report covering data from 2011-2015. This current report supersedes this previous report. Further refinement of the models as additional data are collected is recommended.« less

[The comparative assessment of the practical value of the currently employed methods for the recognition and species specificity of the blood].

PubMed

Grezina, N Iu; Suleĭmenova, G M

2011-01-01

The objective of the present study was to evaluate sensitivity and specificity of the HemDirect method on test-plates (Seratec) for detecting human hemoglobin (HHb). These characteristics were compared with those of other widely used methods designed for the detection of blood traces, viz. thin layer chromatography, hemotest, spectrofluorimetry, and identification of blood species specificity (by countercurrent immunoelectrophoresis in agar and on the acetate-cellulose film). It was shown that the HemDirect test is highly specific and far more sensitive than other techniques used for the same purpose in the practical work. It can be recommended as the method of choice for the detection of blood microtraces.

The effects of surface tension on flooding in counter-current two-phase flow in an inclined tube

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

Deendarlianto; Forschungszentrum Dresden-Rossendorf e.V., Institute of Safety Research, P.O. Box 510 119, D-01314 Dresden; Ousaka, Akiharu

2010-10-15

The purpose of the present study is to investigate the effects of surface tension on flooding phenomena in counter-current two-phase flow in an inclined tube. Previous studies by other researchers have shown that surface tension has a stabilizing effect on the falling liquid film under certain conditions and a destabilizing or unclear trend under other conditions. Experimental results are reported herein for air-water systems in which a surfactant has been added to vary the liquid surface tension without altering other liquid properties. The flooding section is a tube of 16 mm in inner diameter and 1.1 m length, inclined atmore » 30-60 from horizontal. The flooding mechanisms were observed by using two high-speed video cameras and by measuring the time variation of liquid hold-up along the test tube. The results show that effects of surface tension are significant. The gas velocity needed to induce flooding is lower for a lower surface tension. There was no upward motion of the air-water interfacial waves upon flooding occurrence, even for lower a surface tension. Observations on the liquid film behavior after flooding occurred suggest that the entrainment of liquid droplets plays an important role in the upward transport of liquid. Finally, an empirical correlation for flooding velocities is proposed that includes functional dependencies on surface tension and tube inclination. (author)« less

An Efficient Method for the Preparative Isolation and Purification of Flavonoid Glycosides and Caffeoylquinic Acid Derivatives from Leaves of Lonicera japonica Thunb. Using High Speed Counter-Current Chromatography (HSCCC) and Prep-HPLC Guided by DPPH-HPLC Experiments.

PubMed

Wang, Daijie; Du, Ning; Wen, Lei; Zhu, Heng; Liu, Feng; Wang, Xiao; Du, Jinhua; Li, Shengbo

2017-02-02

In this work, the n-butanol extract from leaves of Lonicera japonica Thunb. (L. japonica) was reacted with DPPH and subjected to a HPLC analysis for the guided screening antioxidants (DPPH-HPLC experiments). Then, nine antioxidants, including flavonoid glycosides and caffeoylquinic acid derivatives, were isolated and purified from leaves of L. japonica using high speed counter-current chromatography (HSCCC) and prep-HPLC. The n-butanol extract was firstly isolated by HSCCC using methyl tert-butyl ether/n-butanol/acetonitrile/water (0.5% acetic acid) (2:2:1:5, v/v), yielding five fractions F1, F2 (rhoifolin), F3 (luteoloside), F4 and F5 (collected from the column after the separation). The sub-fractions F1, F4 and F5 were successfully separated by prep-HPLC. Finally, nine compounds, including chlorogenic acid (1), lonicerin (2), rutin (3), rhoifolin (4), luteoloside (5), 3,4-Odicaffeoylquinic acid (6), hyperoside (7), 3,5-O-dicaffeoylquinic acid (8), and 4,5-O-dicaffeoylquinic acid (9) were obtained, respectively, with the purities over 94% as determined by HPLC. The structures were identified by electrospray ionization mass spectrometry (ESI-MS), 1H- and 13C-NMR. Antioxidant activities were tested, and the isolated compounds showed strong antioxidant activities.

DWPF SIMULANT CPC STUDIES FOR SB7B

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

Koopman, D.

2011-11-01

Lab-scale DWPF simulations of Sludge Batch 7b (SB7b) processing were performed. Testing was performed at the Savannah River National Laboratory - Aiken County Technology Laboratory (SRNL-ACTL). The primary goal of the simulations was to define a likely operating window for acid stoichiometry for the DWPF Sludge Receipt and Adjustment Tank (SRAT). In addition, the testing established conditions for the SRNL Shielded Cells qualification simulation of SB7b-Tank 40 blend, supported validation of the current glass redox model, and validated the coupled process flowsheet at the nominal acid stoichiometry. An acid window of 105-140% by the Koopman minimum acid (KMA) equation (107-142%more » DWPF Hsu equation) worked for the sludge-only flowsheet. Nitrite was present in the SRAT product for the 105% KMA run at 366 mg/kg, while SME cycle hydrogen reached 94% of the DWPF Slurry Mix Evaporator (SME) cycle limit in the 140% KMA run. The window was determined for sludge with added caustic (0.28M additional base, or roughly 12,000 gallons 50% NaOH to 820,000 gallons waste slurry). A suitable processing window appears to be 107-130% DWPF acid equation for sludge-only processing allowing some conservatism for the mapping of lab-scale simulant data to full-scale real waste processing including potentially non-conservative noble metal and mercury concentrations. This window should be usable with or without the addition of up to 7,000 gallons of caustic to the batch. The window could potentially be wider if caustic is not added to SB7b. It is recommended that DWPF begin processing SB7b at 115% stoichiometry using the current DWPF equation. The factor could be increased if necessary, but changes should be made with caution and in small increments. DWPF should not concentrate past 48 wt.% total solids in the SME cycle if moderate hydrogen generation is occurring simultaneously. The coupled flowsheet simulation made more hydrogen in the SRAT and SME cycles than the sludge-only run with the same acid stoichiometric factor. The slow acid addition in MCU seemed to alter the reactions that consumed the small excess acid present such that hydrogen generation was promoted relative to sludge-only processing. The coupled test reached higher wt.% total solids, and this likely contributed to the SME cycle hydrogen limit being exceeded at 110% KMA. It is clear from the trends in the SME processing GC data, however, that the frit slurry formic acid contributed to driving the hydrogen generation rate above the SME cycle limit. Hydrogen generation rates after the second frit addition generally exceeded those after the first frit addition. SRAT formate loss increased with increasing acid stoichiometry (15% to 35%). A substantial nitrate gain which was observed to have occurred after acid addition (and nitrite destruction) was reversed to a net nitrate loss in runs with higher acid stoichiometry (nitrate in SRAT product less than sum of sludge nitrate and added nitric acid). Increased ammonium ion formation was also indicated in the runs with nitrate loss. Oxalate loss on the order 20% was indicated in three of the four acid stoichiometry runs and in the coupled flowsheet run. The minimum acid stoichiometry run had no indicated loss. The losses were of the same order as the official analytical uncertainty of the oxalate concentration measurement, but were not randomly distributed about zero loss, so some actual loss was likely occurring. Based on the entire set of SB7b test data, it is recommended that DWPF avoid concentrating additional sludge solids in single SRAT batches to limit the concentrations of noble metals to SB7a processing levels (on a grams noble metal per SRAT batch basis). It is also recommended that DWPF drop the formic acid addition that accompanies the process frit 418 additions, since SME cycle data showed considerable catalytic activity for hydrogen generation from this additional acid (about 5% increase in stoichiometry occurred from the frit formic acid). Frit 418 also does not appear to need formic acid addition to prevent gel formation in the frit slurry. Simulant processing was successful using 100 ppm of 747 antifoam added prior to nitric acid instead of 200 ppm. This is a potential area for DWPF to cut antifoam usage in any future test program. An additional 100 ppm was added before formic acid addition. Foaming during formic acid addition was not observed. No build-up of oily or waxy material was observed in the off-gas equipment. Lab-scale mercury stripping behavior was similar to SB6 and SB7a. More mercury was unaccounted for as the acid stoichiometry increased.« less

The Impact Of The MCU Life Extension Solvent On Sludge Batch 8 Projected Operating Windows

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

Peeler, D. K.; Edwards, T. B.

2013-06-26

As a part of the Actinide Removal Process (ARP)/Modular Caustic Side Solvent Extraction Unit (MCU) Life Extension Project, a next generation solvent (NGS) and a new strip acid will be deployed. The strip acid will be changed from dilute nitric acid to dilute boric acid (0.01 M). Because of these changes, experimental testing or evaluations with the next generation solvent are required to determine the impact of these changes (if any) to Chemical Process Cell (CPC) activities, glass formulation strategies, and melter operations at the Defense Waste Processing Facility (DWPF). The introduction of the dilute (0.01 M) boric acid streammore » into the DWPF flowsheet has a potential impact on glass formulation and frit development efforts since B203 is a major oxide in frits developed for DWPF. Prior knowledge of this stream can be accounted for during frit development efforts but that was not the case for Sludge Batch 8 (SB8). Frit 803 has already been recommended and procured for SB8 processing; altering the frit to account for the incoming boron from the strip effluent (SE) is not an option for SB8. Therefore, the operational robustness of Frit 803 to the introduction of SE including its compositional tolerances (i.e., up to 0.0125M boric acid) is of interest and was the focus of this study. The primary question to be addressed in the current study was: What is the impact (if any) on the projected operating windows for the Frit 803 - SB8 flowsheet to additions of B203 from the SE in the Sludge Receipt and Adjustment Tank (SRAT)? More specifically, will Frit 803 be robust to the potential compositional changes occurring in the SRAT due to sludge variation, varying additions of ARP and/or the introduction of SE by providing access to waste loadings (WLs) of interest to DWPF? The Measurement Acceptability Region (MAR) results indicate there is very little, if any, impact on the projected operating windows for the Frit 803 - SB8 system regardless of the presence or absence of ARP and SE (up to 2 wt% B203 contained in the SRAT and up to 2000 gallons of ARP). It should be noted that 0.95 wt% B203 is the nominal projected concentration in the SRAT based on a 0.0125M boric acid flowsheet with 70,000 liters of SE being added to the SRAT.« less

Countercurrent flow afterburner

DOEpatents

Leggett, Ronald L.; Presse, Donald E.; Smith, Carl J.; Teter, Alton R.

1976-01-01

Afterburner apparatus for receiving from an incinerator products of combustion and distributing them through a domed distributor in counterflow manner throughout a housing, in opposition to a stream of combustible gas.

Isolation of four phenolic compounds from Mangifera indica L. flowers by using normal phase combined with elution extrusion two-step high speed countercurrent chromatography.

PubMed

Shaheen, Nusrat; Lu, Yanzhen; Geng, Ping; Shao, Qian; Wei, Yun

2017-03-01

Two-step high speed countercurrent chromatography method, following normal phase and elution-extrusion mode of operation by using selected solvent systems, was introduced for phenolic compounds separation. Phenolic compounds including gallic acid, ethyl gallate, ethyl digallate and ellagic acid were separated from the ethanol extract of mango (Mangifera indica L.) flowers for the first time. In the first step, gallic acid of 3.7mg and ethyl gallate of 3.9mg with the purities of 98.87% and 99.55%, respectively, were isolated by using hexane-ethylacetate-methanol-water (4:6:4:6, v/v) in normal phase high speed countercurrent chromatography from 200mg of crude extract, while ethyl digallate and ellagic acid were collected in the form of mixture fraction. In the second step, further purification of the mixture was carried out with the help of another selected solvent system of dichloromethane-methanol-water (4:3:2, v/v) following elusion-extrusion mode of operation. Ethyl digallate of 3.8mg and ellagic acid of 5.7mg were separated well with high purities of 98.68% and 99.71%, respectively. The separated phenolic compounds were identified and confirmed by HPLC, UPLC-QTOF/ESI-MS, 1 H and 13 C NMR spectrometric analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparative isolation and purification of antioxidative diarylheptanoid derivatives from Alnus japonica by high-speed counter-current chromatography.

PubMed

Lim, Soon Sung; Lee, Min Young; Ahn, Hong Ryul; Choi, Soon Jung; Lee, Jae-Yong; Jung, Sang Hoon

2011-12-01

This study employed the online HPLC-2,2'-azino-bis(3-ethylbenzthiazoline-6-sulphonic acid) (ABTS)(+) bioassay to rapidly determine the antioxidant compounds occurring in the crude extract of Alnus japonica. The negative peaks of the ABTS(+) radical scavenging detection system, which indicated the presence of antioxidant activity, were monitored by measuring the decrease in absorbance at 734 nm. The ABTS(+)-based antioxidant activity profile showed that three negative peaks exhibited antioxidant activity. High-speed counter-current chromatography (HSCCC) was used for preparative scale separation of the three active peaks from the extract. The purity of the isolated compounds was analyzed by HPLC and their structures were identified by (1)H- and (13)C-nuclear magnetic resonance spectrometry (NMR), heteronuclear multiple bond correlation (HMBC), and heteronuclear single quantum correlation (HSQC). Two solvent systems composed of n-hexane/ethylacetate/methanol/water (4:6:4:6, v/v) and of ethyl acetate/methanol/water (1:0.1:1, v/v) were performed in high-speed counter-current chromatography. Consequently, a total of 527 mg of hirsutanonol 5-O-β-D-glucopyranoside, 80.04 mg of 3-deoxohirsutenonol 5-O-β-D-glucopyranoside, and 91.0 mg of hirsutenone were obtained with purity of 94.7, 90.5, and 98.6%, respectively. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Purification of monoclonal antibodies from clarified cell culture fluid using Protein A capture continuous countercurrent tangential chromatography

PubMed Central

Dutta, Amit K.; Tran, Travis; Napadensky, Boris; Teella, Achyuta; Brookhart, Gary; Ropp, Philip A.; Zhang, Ada W.; Tustian, Andrew D.; Zydney, Andrew L.; Shinkazh, Oleg

2015-01-01

Recent studies using simple model systems have demonstrated that Continuous Countercurrent Tangential Chromatography (CCTC) has the potential to overcome many of the limitations of conventional Protein A chromatography using packed columns. The objective of this work was to optimize and implement a CCTC system for monoclonal antibody purification from clarified Chinese Hamster Ovary (CHO) cell culture fluid using a commercial Protein A resin. Several improvements were introduced to the previous CCTC system including the use of retentate pumps to maintain stable resin concentrations in the flowing slurry, the elimination of a slurry holding tank to improve productivity, and the introduction of an “after binder” to the binding step to increase antibody recovery. A kinetic binding model was developed to estimate the required residence times in the multi-stage binding step to optimize yield and productivity. Data were obtained by purifying two commercial antibodies from two different manufactures, one with low titer (~0.67 g/L) and one with high titer (~6.9 g/L), demonstrating the versatility of the CCTC system. Host cell protein removal, antibody yields and purities were similar to that obtained with conventional column chromatography; however, the CCTC system showed much higher productivity. These results clearly demonstrate the capabilities of continuous countercurrent tangential chromatography for the commercial purification of monoclonal antibody products. PMID:25747172

Purification of monoclonal antibodies from clarified cell culture fluid using Protein A capture continuous countercurrent tangential chromatography.

PubMed

Dutta, Amit K; Tran, Travis; Napadensky, Boris; Teella, Achyuta; Brookhart, Gary; Ropp, Philip A; Zhang, Ada W; Tustian, Andrew D; Zydney, Andrew L; Shinkazh, Oleg

2015-11-10

Recent studies using simple model systems have demonstrated that continuous countercurrent tangential chromatography (CCTC) has the potential to overcome many of the limitations of conventional Protein A chromatography using packed columns. The objective of this work was to optimize and implement a CCTC system for monoclonal antibody purification from clarified Chinese Hamster Ovary (CHO) cell culture fluid using a commercial Protein A resin. Several improvements were introduced to the previous CCTC system including the use of retentate pumps to maintain stable resin concentrations in the flowing slurry, the elimination of a slurry holding tank to improve productivity, and the introduction of an "after binder" to the binding step to increase antibody recovery. A kinetic binding model was developed to estimate the required residence times in the multi-stage binding step to optimize yield and productivity. Data were obtained by purifying two commercial antibodies from two different manufactures, one with low titer (∼ 0.67 g/L) and one with high titer (∼ 6.9 g/L), demonstrating the versatility of the CCTC system. Host cell protein removal, antibody yields and purities were similar to those obtained with conventional column chromatography; however, the CCTC system showed much higher productivity. These results clearly demonstrate the capabilities of continuous countercurrent tangential chromatography for the commercial purification of monoclonal antibody products. Copyright © 2015 Elsevier B.V. All rights reserved.

Effect of gas-liquid flow pattern and microbial diversity analysis of a pilot-scale biotrickling filter for anoxic biogas desulfurization.

PubMed

Almenglo, Fernando; Bezerra, Tercia; Lafuente, Javier; Gabriel, David; Ramírez, Martín; Cantero, Domingo

2016-08-01

Hydrogen sulfide removal from biogas was studied under anoxic conditions in a pilot-scale biotrickling filter operated under counter- and co-current gas-liquid flow patterns. The best performance was found under counter-current conditions (maximum elimination capacity of 140 gS m(-3) h(-1)). Nevertheless, switching conditions between co- and counter-current flow lead to a favorable redistribution of biomass and elemental sulfur along the bed height. Moreover, elemental sulfur was oxidized to sulfate when the feeding biogas was disconnected and the supply of nitrate (electron acceptor) was maintained. Removal of elemental sulfur was important to prevent clogging in the packed bed and, thereby, to increase the lifespan of the packed bed between maintenance episodes. The larger elemental sulfur removal rate during shutdowns was 59.1 gS m(-3) h(-1). Tag-encoded FLX amplicon pyrosequencing was used to study the diversity of bacteria under co-current flow pattern with liquid recirculation and counter-current mode with a single-pass flow of the liquid phase. The main desulfurizing bacteria were Sedimenticola while significant role of heterotrophic, opportunistic species was envisaged. Remarkable differences between communities were found when a single-pass flow of industrial water was fed to the biotrickling filter. Copyright © 2016 Elsevier Ltd. All rights reserved.

Separation of catechin constituents from five tea cultivars using high-speed counter-current chromatography.

PubMed

Kumar, N Savitri; Rajapaksha, Maheshinie

2005-08-12

Catechins were extracted from five different tea (Camellia sinensis L.) cultivars. High-speed counter-current chromatography was found to be an efficient method for the separation of seven catechins from the catechin extracts. High-performance liquid chromatography was used to assess the purity of the catechins isolated. Epigallocatechin gallate (EGCG), epicatechin gallate (ECG) and epigallocatechin (EGC) of high purity (91-99%) were isolated in high yield after a single high-speed counter-current chromatography run. The two-phase solvent mixtures used for the separation of the catechin extracts were hexane:ethyl acetate:methanol:water (1:6:1:6 for TRI 2023); (1:7:1:7 for TRI 2025 and TRI 2043); (1:5:1:5 for TRI 3079) and (1:6.5:1:6.5 for TRI 4006). Fresh tea shoots from the tea cultivar TRI 2023 (150 g) gave 440 mg of 96% pure EGCG while TRI 2025 (235 g) gave 347 mg of 99% pure EGCG and 40 mg of 97% ECG, and TRI 3079 (225 g) gave 432 mg of 97% pure EGCG and 32 mg of 96% pure ECG. Tea cultivar TRI 4006 (160 g) gave EGCG (272 mg, 96% pure) and EGC (104 mg, 90% pure). 1H and 13C NMR chemical shifts for catechin gallate (CG), EGC, ECG, EGCG and epigallocatechin 3,5-di-O-gallate (EGCDG) in CD3OD were also recorded.

Separation and purification of five alkaloids from Aconitum duclouxii by counter-current chromatography.

PubMed

Wang, Yarong; Cai, Shining; Chen, Yang; Deng, Liang; Zhou, Xumei; Liu, Jia; Xu, Xin; Xia, Qiang; Lin, Mao; Zhang, Jili; Huang, Weili; Wang, Wenjun; Xiang, Canhui; Cui, Guozhen; Du, Lianfeng; He, Huan; Qi, Baohui

2015-07-01

C19 -diterpenoid alkaloids are the main components of Aconitum duclouxii Levl. The process of separation and purification of these compounds in previous studies was tedious and time consuming, requiring multiple chromatographic steps, thus resulted in low recovery and high cost. In the present work, five C19 -diterpenoid alkaloids, namely, benzoylaconine (1), N-deethylaconitine (2), aconitine (3), deoxyaconitine (4), and ducloudine A (5), were efficiently prepared from A. duclouxii Levl (Aconitum L.) by ethyl acetate extraction followed with counter-current chromatography. In the process of separation, the critical conditions of counter-current chromatography were optimized. The two-phase solvent system composed of n-hexane/ethyl acetate/methanol/water/NH3 ·H2 O (25%) (1:1:1:1:0.1, v/v) was selected and 148.2 mg of 1, 24.1 mg of 2, 250.6 mg of 3, 73.9 mg of 4, and 31.4 mg of 5 were obtained from 1 g total Aconitum alkaloids extract, respectively, in a single run within 4 h. Their purities were found to be 98.4, 97.2, 98.2, 96.8, and 96.6%, respectively, by ultra-high performance liquid chromatography analysis. The presented separation and purification method was simple, fast, and efficient, and the obtained highly pure alkaloids are suitable for biochemical and toxicological investigation. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparative separation of bioactive compounds from essential oil of Flaveria bidentis (L.) Kuntze using steam distillation extraction and one step high-speed counter-current chromatography.

PubMed

Wei, Yun; Du, Jilin; Lu, Yuanyuan

2012-10-01

In order to utilize and control the invasive weed, bioactive compounds from essential oil of Flaveria bidentis (L.) Kuntze were studied. Steam distillation extraction and one step high-speed counter-current chromatography were applied to separate and purify the caryophyllene oxide, 7,11-dimethyl-3-methylene-1,6,10-dodecatriene, and caryophyllene from essential oil of Flaveria bidentis (L.) Kuntze. The two-phase solvent system containing n-hexane/acetonitrile/ethanol (5:4:3, v/v/v) was selected for the one step separation mode according to the partition coefficient values (K) of the target compounds and the separation factor (α). The purity of each isolated fraction after a single high-speed counter-current chromatography run was determined by high performance liquid chromatography. A 3.2 mg of caryophyllene oxide at a purity of 92.6%, 10.4 mg of 7,11-dimethyl-3-methylene-1,6,10-dodecatriene at a purity of 99.1% and 5.7 mg of caryophyllene at a purity of 98.8% were obtained from 200 mg essential oil of Flaveria bidentis (L.) Kuntze. The chemical structures of these components were identified by GC-MS, (1) H-NMR, and (13) C-NMR. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Integrated Bioprocess Design: A Case Study for Undergraduates.

ERIC Educational Resources Information Center

Titchener-Hooker, Nigel; Zhou, Yu-Hong

2000-01-01

Presents a case study for use in the teaching of bioprocess design. Taking the production and isolation of the intracellular protein s. cerevisae, demonstrates how undergraduates can use a range of data to construct and then investigate the range of processes flowsheet options available for a process duty. (Author/SAH)

Isolation and purification of orientin and vitexin from Trollius chinensis Bunge by high-speed counter-current chromatography.

PubMed

Yu, Xiao-Xue; Huang, Jie-Yun; Xu, Dan; Xie, Zhi-Yong; Xie, Zhi-Sheng; Xu, Xin-Jun

2014-01-01

Orientin and vitexin are the two main bioactive compounds in Trollius chinensis Bunge. In this study, a rapid method was established for the isolation and purification of orientin and vitexin from T. chinensis Bunge using high-speed counter-current chromatography in one step, with a solvent system of ethyl acetate-ethanol-water (4:1:5, v/v/v). A total of 9.8 mg orientin and 2.1 mg vitexin were obtained from 100 mg of the ethyl acetate extract, with purities of 99.2% and 96.0%, respectively. Their structures were identified by UV, MS and NMR. The method was efficient and convenient, which could be used for the preparative separation of orientin and vitexin from T. chinensis Bunge.

Preparative isolation and purification of harpagoside and angroside C from the root of Scrophularia ningpoensis Hemsley by high-speed counter-current chromatography.

PubMed

Tian, Jinfeng; Ye, Xiaoli; Shang, Yuanhong; Deng, Yafei; He, Kai; Li, Xuegang

2012-10-01

In this study, the bioactive component harpagoside and angroside C in the root of Scrophularia ningpoensis Hemsley was simultaneously separated by high-speed counter-current chromatography (HSCCC). A two-phase solvent system containing chloroform/n-butanol/methanol/water (4:1:3:2, v/v/v/v) was selected following consideration of the partition coefficient of the target compound. The crude extract (200 mg) was loaded onto a 280-mL HSCCC column and yielded 22 mg harpagoside and 31 mg angroside C with the purity of higher than 98 and 98.5%, respectively. It is feasible to isolate active compounds harpagoside and angroside C from S. ningpoensis using HSCCC. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation and purification of astaxanthin from Phaffia rhodozyma by preparative high-speed counter-current chromatography.

PubMed

Du, Xiping; Dong, Congcong; Wang, Kai; Jiang, Zedong; Chen, Yanhong; Yang, Yuanfan; Chen, Feng; Ni, Hui

2016-09-01

An effective high-speed counter-current chromatography (HSCCC) method was established for the preparative isolation and purification of astaxanthin from Phaffia rhodozyma. With a two-phase solvent system composed of n-hexane-acetone-ethanol-water (1:1:1:1, v/v/v/v), 100mg crude extract of P. rhodozyma was separated to yield 20.6mg of astaxanthin at 92.0% purity. By further one step silica gel column chromatography, the purity reached 99.0%. The chemical structure of astaxanthin was confirmed by thin layer chromatography (TLC), UV spectroscopy scanning, high performance liquid chromatography with a ZORBAX SB-C18 column and a Waters Nova-pak C18 column, and ESI/MS/MS. Copyright © 2016 Elsevier B.V. All rights reserved.

Method for enhancing selectivity and recovery in the fractional flotation of particles in a flotation column

DOEpatents

Klunder, Edgar B [Bethel Park, PA

2011-08-09

The method relates to particle separation from a feed stream. The feed stream is injected directly into the froth zone of a vertical flotation column in the presence of a counter-current reflux stream. A froth breaker generates a reflux stream and a concentrate stream, and the reflux stream is injected into the froth zone to mix with the interstitial liquid between bubbles in the froth zone. Counter-current flow between the plurality of bubbles and the interstitial liquid facilitates the attachment of higher hydrophobicity particles to bubble surfaces as lower hydrophobicity particles detach. The height of the feed stream injection and the reflux ratio may be varied in order to optimize the concentrate or tailing stream recoveries desired based on existing operating conditions.

Alkaline-side extraction of technetium from tank waste using crown ethers and other extractants

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

Bonnesen, P.V.; Moyer, B.A.; Presley, D.J.

The chemical development of a new crown-ether-based solvent-extraction process for the separation of (Tc) from alkaline tank-waste supernate is ready for counter-current testing. The process addresses a priority need in the proposed cleanup of Hanford and other tank wastes. This need has arisen from concerns due to the volatility of Tc during vitrification, as well as {sup 99}Tc`s long half-life and environmental mobility. The new process offers several key advantages that direct treatability--no adjustment of the waste composition is needed; economical stripping with water; high efficiency--few stages needed; non-RCRA chemicals--no generation of hazardous or mixed wastes; co-extraction of {sup 90}Sr;more » and optional concentration on a resin. A key concept advanced in this work entails the use of tandem techniques: solvent extraction offers high selectivity, while a subsequent column sorption process on the aqueous stripping solution serves to greatly concentrate the Tc. Optionally, the stripping solution can be evaporated to a small volume. Batch tests of the solvent-extraction and stripping components of the process have been conducted on actual melton Valley Storage Tank (MVST) waste as well as simulants of MVST and Hanford waste. The tandem process was demonstrated on MVST waste simulants using the three solvents that were selected the final candidates for the process. The solvents are 0.04 M bis-4,4{prime}(5{prime})[(tert-butyl)cyclohexano]-18-crown-6 (abbreviated di-t-BuCH18C6) in a 1:1 vol/vol blend of tributyl phosphate and Isopar{reg_sign} M (an isoparaffinic kerosene); 0.02 M di-t-BuCH18C6 in 2:1 vol/vol TBP/Isopar M and pure TBP. The process is now ready for counter-current testing on actual Hanford tank supernates.« less

Development of solvent systems with room temperature ionic liquids for the countercurrent chromatographic separation of very nonpolar lipid compounds.

PubMed

Müller, Marco; Englert, Michael; Earle, Martyn J; Vetter, Walter

2017-03-10

Solvent systems are not readily available for the separation of very nonpolar compounds by countercurrent chromatography (CCC). In this study we therefore evaluated the suitability of room temperature ionic liquids (IL) in organic solvents for the CCC separation of the extremely nonpolar lipid compounds tripalmitin (PPP) and cholesteryl stearate (CS). The four IL tested were [C 10 mim][OTf], [C 2 mim][NTf 2 ], [P66614][NTf 2 ], and [P66614][Cl]. Search for a CCC-suited solvent system started with solubility studies with fourteen organic solvents. Following this, combinations were made with one organic solvent miscible and one organic solvent immiscible with IL (147 combinations). Twenty-four initially monophasic mixtures of two organic solvents became biphasic by adding IL. Several unexpected results could be observed. For instance, n-hexane and n-heptane became biphasic with [P66614][Cl]. Further nine systems became biphasic although the IL was not miscible in any of the two components. These 33 solvent systems were investigated with regard to phase ratio, settling time, share of IL in the upper phase and last not least the K U/L values of PPP and CS, which were 8.1 and 7.7 respectively. The most promising system, n-heptane/chloroform/[C 10 mim][OTf] (3:3:1, v/v/v) allowed a partial separation of PPP and CS by CCC which was not achieved beforehand. Copyright © 2017 Elsevier B.V. All rights reserved.

Chiral ligand exchange high-speed countercurrent chromatography: mechanism, application and comparison with conventional liquid chromatography in enantioseparation of aromatic α-hydroxyl acids

PubMed Central

Tong, Shengqiang; Shen, Mangmang; Cheng, Dongping; Ito, Yoichiro; Yan, Jizhong

2014-01-01

This work concentrates on the separation mechanism and application of chiral ligand exchange high-speed countercurrent chromatography (HSCCC) in enantioseparations, and comparison with traditional chiral ligand exchange high performance liquid chromatography (HPLC). The enantioseparation of ten aromatic α-hydroxyl acids were performed by these two chromatographic methods. Results showed that five of the racemates were successfully enantioseparated by HSCCC while only three of the racemates could be enantioseparated by HPLC using a suitable chiral ligand mobile phase additive. For HSCCC, the two-phase solvent system was composed of butanol-water (1:1, v/v), to which N-n-dodecyl-L-proline was added in the organic phase as chiral ligand and cupric acetate was added in the aqueous phase as a transition metal ion. Various operation parameters in HSCCC were optimized by enantioselective liquid-liquid extraction. Based on the results of the present studies the separation mechanism for HSCCC was proposed. For HPLC, the optimized mobile phase composed of aqueous solution containing 6 mmol L−1 L-phenylalanine and 3 mmol L−1 cupric sulfate and methanol was used for enantioseparation. Among three ligands tested on a conventional reverse stationary phase column, only one was found to be effective. In the present studies HSCCC presented unique advantages due to its high versatility of two-phase solvent systems and it could be used as an alternative method for enantioseparations. PMID:25087742

Countercurrent Chromatographic Separation of Proteins Using an Eccentric Coiled Column with Synchronous and Nonsynchronous Type-J Planetary Motions

PubMed Central

SHINOMIYA, Kazufusa; YOSHIDA, Kazunori; TOKURA, Koji; TSUKIDATE, Etsuhiro; YANAGIDAIRA, Kazuhiro; ITO, Yoichiro

2015-01-01

Protein separation was performed using the high-speed counter-current chromatograph (HSCCC) at both synchronous and nonsynchronous type-J planetary motions. The partition efficiency was evaluated with two different column configurations, eccentric coil and toroidal coil, on the separation of a set of stable protein samples including cytochrome C, myoglobin and lysozyme with a polymer phase system composed of 12.5% (w/w) polyethylene glycol 1000 and 12.5% (w/w) dibasic potassium phosphate. Better peak resolution was obtained by the eccentric coil than by the toroidal coil using either lower or upper phase as the mobile phase. The peak resolution was further improved using the eccentric coil by the nonsynchronous type-J planetary motion with the combination of 1066 rpm of column rotation and 1000 rpm of revolution. PMID:25765276

Countercurrent chromatographic separation of proteins using an eccentric coiled column with synchronous and nonsynchronous type-J planetary motions.

PubMed

Shinomiya, Kazufusa; Yoshida, Kazunori; Tokura, Koji; Tsukidate, Etsuhiro; Yanagidaira, Kazuhiro; Ito, Yoichiro

2015-01-01

Protein separation was performed using the high-speed countercurrent chromatograph (HSCCC) at both synchronous and nonsynchronous type-J planetary motions. The partition efficiency was evaluated with two different column configurations, eccentric coil and toroidal coil, on the separation of a set of stable protein samples including cytochrome C, myoglobin and lysozyme with a polymer phase system composed of 12.5% (w/w) polyethylene glycol 1000 and 12.5% (w/w) dibasic potassium phosphate. Better peak resolution was obtained by the eccentric coil than by the toroidal coil using either lower or upper phase as the mobile phase. The peak resolution was further improved using the eccentric coil by the nonsynchronous type-J planetary motion with the combination of 1066 rpm of column rotation and 1000 rpm of revolution.

Isolation of cyanidin 3-glucoside from blue honeysuckle fruits by high-speed counter-current chromatography.

PubMed

Chen, Liang; Xin, Xiulan; Lan, Rong; Yuan, Qipeng; Wang, Xiaojie; Li, Ye

2014-01-01

Blue honeysuckle fruits are rich in anthocyanins with many beneficial effects such as reduction of the risk of cardiovascular diseases, diabetes and cancers. High-speed counter-current chromatography (HSCCC) was used for the separation of anthocyanin on a preparative scale from blue honeysuckle fruit crude extract with a biphasic solvent system composed of tert-butyl methyl ether/n-butanol/acetonitrile/water/trifluoroacetic acid (2:2:1:5:0.01, v/v) for the first time in this paper. Each injection of 100 mg crude extract yielded 22.8 mg of cyanidin 3-glucoside (C3G) at 98.1% purity. The compound was identified by means of electro-spray ionisation mass (ESI/MS) and (1)H and (13)C nuclear magnetic resonance (NMR) spectra. Copyright © 2013 Elsevier Ltd. All rights reserved.

Countercurrent flow of supercritical anti-solvent in the production of pure xanthophylls from Nannochloropsis oculata.

PubMed

Cho, Yueh-Cheng; Wang, Yuan-Chuen; Shieh, Chwen-Jen; Lin, Justin Chun-Te; Chang, Chieh-Ming J; Han, Esther

2012-08-10

This study examined pilot scaled elution chromatography coupled with supercritical anti-solvent precipitation (using countercurrent flow) in generating zeaxanthin-rich particulates from a micro-algal species. Ultrasonic agitated acetone extract subjected to column fractionation successfully yielded a fraction containing 349.4 mg/g of zeaxanthin with a recovery of 85%. Subsequently, supercritical anti-solvent (SAS) precipitation of the column fraction at 150 bar and 343 K produced submicron-sized particulates with a concentration of 845.5mg/g of zeaxanthin with a recovery of 90%. Experimental results from a two-factor response surface method SAS precipitation indicated that purity, mean size and morphology of the precipitates were significantly affected by the flow type configuration, feed flow rate and injection time. Copyright © 2012 Elsevier B.V. All rights reserved.

Isolation of sutherlandins A, B, C and D from Sutherlandia frutescens (L.) R. Br. by counter-current chromatography using spiral tubing support rotors.

PubMed

Chen, Cuiping; Folk, William R; Lazo-Portugal, Rodrigo; Finn, Thomas M; Knight, Martha

2017-07-28

Spiral countercurrent-chromatography has great potential for improving the capacity and efficiency of purification of secondary metabolites, and here we describe applications useful for the isolation of flavonoids from the widely used South African medicinal plant, Sutherlandia frutescens (L.) R. Br. In the spiral tubing support rotor, STS-4 for high-speed counter-current chromatography, several polar butanol aqueous solvent systems were selected using a logK plot, and the novel flavonol glycosides (sutherlandins A-D) were well separated by the optimized solvent system (ethyl acetate:n-butanol:acetic acid:water; 5:1:0.3:6 by vol.). The yield of purified flavonoids from 0.9g extract varied from 8.6mg to 54mg of the sutherlandins for a total of 85.3mg. The same extract was fractionated in the new STS-12 rotor of the same outside dimensions but with more radial channels forming 12 loops of the tubing instead of 4. The rotor holds more layers and increased length of tubing. From 0.9g extract the STS-12 rotor yielded more recovery of 110.4mg total with amounts varying from 11.2mg to 64mg of the sutherlandins and apparent increased separation efficiency as noted by less volume of each fraction peak. Thus from 1-g amounts of extract, good recovery of the flavonoids was achieved in the butanol aqueous solvent system. Copyright © 2017 Elsevier B.V. All rights reserved.

Isolation and purification of two antioxidant isomers of resveratrol dimer from the wine grape by counter-current chromatography.

PubMed

Kong, Qingjun; Ren, Xueyan; Hu, Ruilin; Yin, Xuefeng; Jiang, Guoshan; Pan, Yuanjiang

2016-06-01

Resveratrol dimers belong to a group of compounds called stilbenes, which along with proanthocyanidins, anthocyanins, catechins, and flavonols are natural phenolic compounds found in grapes and red wine. Stilbenes have a variety of structural isomers, all of which exhibit various biological properties. Counter-current chromatography with a two-phase solvent system composed of n-hexane/ethyl acetate/methanol/water (2:5:4:5, v/v/v/v) was applied to isolate and purify stilbene from the stems of wine grape. Two isomers of resveratrol dimers trans-ε-viniferin and trans-δ-viniferin were obtained from the crude sample in a one-step separation, with purities of 93.2 and 97.5%, respectively, as determined by high-performance liquid chromatography. The structures of these two compounds were identified by (1) H and (13) C NMR spectroscopy. In addition, their antioxidant activities were assessed by 1,1-diphenyl-2-picrylhydrazyl (DPPH) assay. The antioxidant activities of trans-δ-viniferin were higher than that of trans-ε-viniferin in this model. This work demonstrated that counter-current chromatography is a powerful and effective method for the isolation and purification of polyphenols from wine grape. Additionally, the DPPH radical assay showed that the isolated component trans-δ-viniferin exhibited stronger antioxidant activities than trans-ε-viniferin and a little bit weaker than vitamin E at the same concentration. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Technical Basis of Scaling Relationships for the Pretreatment Engineering Platform

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

Kuhn, William L.; Arm, Stuart T.; Huckaby, James L.

Pacific Northwest National Laboratory has been tasked by Bechtel National Inc. (BNI) on the River Protection Project-Waste Treatment Plant (RPP-WTP) project to perform research and development activities. The Pretreatment Engineering Platform (PEP) is being designed and constructed as part of a plan to respond to an issue raised by the WTP External Flowsheet Review Team (EFRT) entitled “Undemonstrated Leaching Processes” and numbered M12. The PEP replicates the WTP leaching process using prototypic equipment and control strategies. The approach for scaling PEP performance data to predict WTP performance is critical to the successful resolution of the EFRT issue. This report describesmore » the recommended PEP scaling approach, PEP data interpretation and provides recommendations on test conduct and data requirements.« less

Impact of scaling on the nitric-glycolic acid flowsheet

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

Lambert, D.

Savannah River Remediation (SRR) is considering using glycolic acid as a replacement for formic acid in Sludge Receipt and Adjustment Tank (SRAT) processing in the Defense Waste Processing Facility (DWPF). Catalytic decomposition of formic acid is responsible for the generation of hydrogen, a potentially flammable gas, during processing. To prevent the formation of a flammable mixture in the offgas, an air purge is used to dilute the hydrogen concentration below the 60% of the Composite Lower Flammability Limit (CLFL). The offgas is continuously monitored for hydrogen using Gas Chromatographs (GCs). Since formic acid is much more volatile and toxic thanmore » glycolic acid, a formic acid spill would lead to the release of much larger quantities to the environment. Switching from formic acid to glycolic acid is expected to eliminate the hydrogen flammability hazard leading to lower air purges, thus downgrading of Safety Significant GCs to Process Support GCs, and minimizing the consequence of a glycolic acid tank leak in DWPF. Overall this leads to a reduction in process operation costs and an increase in safety margin. Experiments were completed at three different scales to demonstrate that the nitric-glycolic acid flowsheet scales from the 4-L lab scale to the 22-L bench scale and 220-L engineering scale. Ten process demonstrations of the sludge-only flowsheet for SRAT and Slurry Mix Evaporator (SME) cycles were performed using Sludge Batch 8 (SB8)-Tank 40 simulant. No Actinide Removal Process (ARP) product or strip effluent was added during the runs. Six experiments were completed at the 4-L scale, two experiments were completed at the 22-L scale, and two experiments were completed at the 220-L scale. Experiments completed at the 4-L scale (100 and 110% acid stoichiometry) were repeated at the 22-L and 220-L scale for scale comparisons.« less

Hybrid upwind discretization of nonlinear two-phase flow with gravity

NASA Astrophysics Data System (ADS)

Lee, S. H.; Efendiev, Y.; Tchelepi, H. A.

2015-08-01

Multiphase flow in porous media is described by coupled nonlinear mass conservation laws. For immiscible Darcy flow of multiple fluid phases, whereby capillary effects are negligible, the transport equations in the presence of viscous and buoyancy forces are highly nonlinear and hyperbolic. Numerical simulation of multiphase flow processes in heterogeneous formations requires the development of discretization and solution schemes that are able to handle the complex nonlinear dynamics, especially of the saturation evolution, in a reliable and computationally efficient manner. In reservoir simulation practice, single-point upwinding of the flux across an interface between two control volumes (cells) is performed for each fluid phase, whereby the upstream direction is based on the gradient of the phase-potential (pressure plus gravity head). This upwinding scheme, which we refer to as Phase-Potential Upwinding (PPU), is combined with implicit (backward-Euler) time discretization to obtain a Fully Implicit Method (FIM). Even though FIM suffers from numerical dispersion effects, it is widely used in practice. This is because of its unconditional stability and because it yields conservative, monotone numerical solutions. However, FIM is not unconditionally convergent. The convergence difficulties are particularly pronounced when the different immiscible fluid phases switch between co-current and counter-current states as a function of time, or (Newton) iteration. Whether the multiphase flow across an interface (between two control-volumes) is co-current, or counter-current, depends on the local balance between the viscous and buoyancy forces, and how the balance evolves in time. The sensitivity of PPU to small changes in the (local) pressure distribution exacerbates the problem. The common strategy to deal with these difficulties is to cut the timestep and try again. Here, we propose a Hybrid-Upwinding (HU) scheme for the phase fluxes, then HU is combined with implicit time discretization to yield a fully implicit method. In the HU scheme, the phase flux is divided into two parts based on the driving force. The viscous-driven and buoyancy-driven phase fluxes are upwinded differently. Specifically, the viscous flux, which is always co-current, is upwinded based on the direction of the total-velocity. The buoyancy-driven flux across an interface is always counter-current and is upwinded such that the heavier fluid goes downward and the lighter fluid goes upward. We analyze the properties of the Implicit Hybrid Upwinding (IHU) scheme. It is shown that IHU is locally conservative and produces monotone, physically-consistent numerical solutions. The IHU solutions show numerical diffusion levels that are slightly higher than those for standard FIM (i.e., implicit PPU). The primary advantage of the IHU scheme is that the numerical overall-flux of a fluid phase remains continuous and differentiable as the flow regime changes between co-current and counter-current conditions. This is in contrast to the standard phase-potential upwinding scheme, in which the overall fractional-flow (flux) function is non-differentiable across the boundary between co-current and counter-current flows.

Cross-axis synchronous flow-through coil planet centrifuge for large-scale preparative counter-current chromatography. III. Performance of large-bore coils in slow planetary motion.

PubMed

Ito, Y; Zhang, T Y

1988-11-25

A preparative capability of the present cross-axis synchronous flow-through coil planet centrifuge was demonstrated with 0.5 cm I.D. multilayer coils. Results of the model studies with short coils indicated that the optimal separations are obtained at low revolutional speeds of 100-200 rpm in both central and lateral coil positions. Preparative separations were successfully performed on 2.5-10 g quantities of test samples in a pair of multilayer coils connected in series with a total capacity of 2.5 l. The sample loading capacity will be scaled up in several folds by increasing the column width.

Membrane Specifications for Multi-Configuration Membrane Distillation Model

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

Villa, Daniel; Vanneste, Johan; Cath, Tzahi

The data includes the membrane properties and specifications used for multi-configuration membrane distillation desalination. In this study, membranes from CLARCOR, 3M, and Aquastill are tested in counter-current, co-current and air-gap configurations at Colorado School of Mines (CSM), Advanced Water technology Center ( Aqwatech) laboratories. In the data sheets: The "theoretical" worksheet, contains steady-state values of the experimental runs and also provides several calculated values. The "Specifications" worksheet contains the inputs to the experiment. The "Data" spreadsheet contains the entire set of data and the rest of the sheets "20-40", "20-45", ...etc., contain individual portions of the data with variation ofmore » feed temperatures.« less

Changes in glycolytic enzyme activities in aging erythrocytes fractionated by counter-current distribution in aqueous polymer two-phase systems.

PubMed Central

Jimeno, P; Garcia-Perez, A I; Luque, J; Pinilla, M

1991-01-01

Human and rat erythrocytes were fractionated by counter-current distribution in charge-sensitive dextran/poly(ethylene glycol) two-phase systems. The specific activities of the key glycolytic enzymes (hexokinase, phosphofructokinase and pyruvate kinase) declined along the distribution profiles, although the relative positions of the activity profiles were reversed in the two species. These enzymes maintained their normal response to specific regulatory effectors in all cell fractions. No variations were observed for phosphoglycerate kinase and bisphosphoglycerate mutase activities. Some correlations between enzyme activities (pyruvate kinase/hexokinase, pyruvate kinase/phosphofructokinase, pyruvate kinase/pyruvate kinase plus phosphoglycerate kinase, pyruvate kinase/bisphosphoglycerate mutase and phosphoglycerate kinase/bisphosphoglycerate mutase ratios) were studied in whole erythrocyte populations as well as in cell fractions. These results strongly support the fractionation of human erythrocytes according to cell age, as occurs with rat erythrocytes. PMID:1656939

Preparative isolation and purification of anti-tumor agent ansamitocin P-3 from fermentation broth of Actinosynnema pretiosum using high-performance counter-current chromatography.

PubMed

Yao, Yuqin; Cheng, Zhihui; Ye, Haoyu; Xie, Yongmei; He, Jing; Tang, Minghai; Shen, Tao; Wang, Jiangman; Zhou, Yan; Lu, Zejun; Luo, Feng; Chen, Lijuan; Yu, Luoting; Yang, Jin-Liang; Peng, Aihua; Wei, Yuquan

2010-05-01

Ansamitocin P-3 is a potent anti-tumor maytansinoid found in Actinosynnema pretiosum. However, due to the complexity of the fermentation broth of Actinomycete, how to effectively separate ansamitocin P-3 is still a challenge. In this study, both analytical and preparative high-performance counter-current chromatography were successfully used to separate and purify ansamitocin P-3 from fermentation broth. A total of 28.8 mg ansamitocin P-3 with purity of 98.4% was separated from 160 mg crude sample of fermentation broth in less than 80 min with the two-phase solvent system of hexane-ethyl acetate-methanol-water (0.6:1:0.6:1, v/v/v/v). The purity and structural identification were determined by HPLC, (1)H NMR, (13)C NMR and mass spectroscopy.

Separation of three anthraquinone glycosides including two isomers by preparative high-performance liquid chromatography and high-speed countercurrent chromatography from Rheum tanguticum Maxim. ex Balf.

PubMed

Chen, Tao; Li, Hongmei; Zou, Denglang; Liu, Yongling; Chen, Chen; Zhou, Guoying; Li, Yulin

2016-08-01

Anthraquinone glycosides, such as chrysophanol 1-O-β-d-glucoside, chrysophanol 8-O-β-d-glucoside, and physion 8-O-β-d-glucoside, are the accepted important active components of Rheum tanguticum Maxim. ex Balf. due to their pharmacological properties: antifungal, antimicrobial, cytotoxic, and antioxidant activities. However, an effective method for the separation of the above-mentioned anthraquinone glycosides from this herb is not currently available. Especially, greater difficulty existed in the separation of the two isomers chrysophanol 1-O-β-d-glucoside and chrysophanol 8-O-β-d-glucoside. This study demonstrated an efficient strategy based on preparative high-performance liquid chromatography and high-speed countercurrent chromatography for the separation of the above-mentioned anthraquinone glycosides from Rheum tanguticum Maxim.ex Balf. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

ELM-free and inter-ELM divertor heat flux broadening induced by edge harmonics oscillation in NSTX

DOE PAGES

Gan, K. F.; Ahn, J. -W.; Gray, T. K.; ...

2017-10-26

A new n =1 dominated edge harmonic oscillation (EHO) has been found in NSTX. The new EHO, rotating toroidally in the counter-current direction and the opposite direction of the neutral beam, was observed during certain inter-ELM and ELM-free periods of H-mode operation. This EHO is associated with a significant broadening of the integral heat flux width (more » $${{\\lambda}_{\\operatorname{int}}}$$ ) by up to 150%, and a decrease in the divertor peak heat flux by >60%. An EHO induced filament was also observed by the gas puff imaging diagnostic. The toroidal rotating filaments could change the edge magnetic topology resulting in toroidal rotating strike point splitting and heat flux broadening. Finally, experimental result of the counter current rotation of strike points splitting is consistent with the counter-current EHO.« less

Separation of two major chalcones from Angelica keiskei by high-speed counter-current chromatography.

PubMed

Kil, Yun-Seo; Nam, Joo-Won; Lee, Jun; Seo, Eun Kyoung

2015-08-01

Angelica keiskei (Shin-sun cho) is an edible higher plant with the beneficial preventive effects on cancer, hypertension, and coronary heart disease. Two bioactive chalcones of Shin-sun cho, xanthoangelol (1) and 4-hydroxyderricin (2), were separated simultaneously by using high-speed counter-current chromatography with a two-phase solvent system composed of n-hexane-EtOAc-MeOH-H2O (9:5:9:4). Only nonconsuming processes, solvent fractionations and Sephadex LH-20 column chromatography, were conducted as presteps. Xanthoangelol (1, 35.9 mg, 99.9 % purity at 254 and 365 nm) and 4-hydroxyderricin (2, 4.4 mg, 98.7 % purity at 254 nm and 98.8 % purity at 365 nm) were successfully purified from 70 mg of the processed extract from A. keiskei. The structures of two compounds were confirmed by (1)H- and (13)C-NMR analysis.

An interesting two-phase solvent system and its use in preparative isolation of aconitines from aconite roots by counter-current chromatography.

PubMed

Han, Quan-Bin; Tang, Wai-Lun; Dong, Cai-Xia; Xu, Hong-Xi; Jiang, Zhi-Hong

2013-04-01

Two-phase solvent system plays crucial role in successful separation of organic compounds using counter-current chromatography (CCC). An interesting two-phase solvent system, composed of chloroform/ethyl acetate/methanol/water, is reported here, in which both phases contain sufficient organic solvents to balance their dissolving capacities. Adjusting the solvent system to get satisfactory partition coefficients (K values) for target compounds becomes relatively simple. This solvent system succeeded in sample preparation of aconitine (8.07 mg, 93.69%), hypaconitine (7.74 mg, 93.17%), mesaconitine (1.95 mg, 94.52%) from raw aconite roots (102.24 mg, crude extract), benzoylmesaconine (34.79 mg, 98.67%) from processed aconite roots (400.01 mg, crude extract), and yunaconitine (253.59 mg, 98.65%) from a crude extract of Aconitum forrestii (326.69 mg, crude extract). © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

ISOLATION OF GLYCOSIDES FROM THE BARKS OF ILEX ROTUNDA BY HIGH-SPEED COUNTER-CURRENT CHROMATOGRAPHY.

PubMed

Wang, Chun; Chao, Zhimao; Sun, Wen; Wu, Xiaoyi; Ito, Yoichiro

2014-04-01

Semi-preparative and preparative high-speed counter-current chromatography (HSCCC) were successfully used for isolation of glycosides from 50% ethanol extract of the dried barks of Ilex rotunda Thunb. (Aquifoliaceae) by using a two-phase solvent system composed of ethyl acetate-n-butanol-water (1:6:7, v/v/v). From 1.0 g of the extract, syringaresinol 4',4"-di-o-β-d-glucopyranoside ( I , 20.2 mg),, syringin ( II , 56.8 mg), sinapaldehyde glucoside ( III , 26.2 mg),, syringaresinol 4'-o-β-d-glucopyranoside ( IV , 20.4 mg), and pedunculoside ( V , 45.1 mg) were obtained by one run of TBE-1000A HSCCC instrument with 1000 mL of column volume. Their structures were identified by IR, MS, and 1 H and 13 C NMR studies. Glycoside I was isolated from this plant for the first time.

ISOLATION OF GLYCOSIDES FROM THE BARKS OF ILEX ROTUNDA BY HIGH-SPEED COUNTER-CURRENT CHROMATOGRAPHY

PubMed Central

Wang, Chun; Chao, Zhimao; Sun, Wen; Wu, Xiaoyi; Ito, Yoichiro

2013-01-01

Semi-preparative and preparative high-speed counter-current chromatography (HSCCC) were successfully used for isolation of glycosides from 50% ethanol extract of the dried barks of Ilex rotunda Thunb. (Aquifoliaceae) by using a two-phase solvent system composed of ethyl acetate-n-butanol-water (1:6:7, v/v/v). From 1.0 g of the extract, syringaresinol 4',4"-di-o-β-d-glucopyranoside (I, 20.2 mg),, syringin (II, 56.8 mg), sinapaldehyde glucoside (III, 26.2 mg),, syringaresinol 4'-o-β-d-glucopyranoside (IV, 20.4 mg), and pedunculoside (V, 45.1 mg) were obtained by one run of TBE-1000A HSCCC instrument with 1000 mL of column volume. Their structures were identified by IR, MS, and 1H and 13C NMR studies. Glycoside I was isolated from this plant for the first time. PMID:25132792

Countercurrent direct contact heat exchange process and system

DOEpatents

Wahl, III, Edward F.; Boucher, Frederic B.

1979-01-01

Recovery of energy from geothermal brines and other hot water sources by direct contact heat exchange with a working fluid, such as a hydrocarbon working fluid, e.g. isobutane. The process and system consists of a plurality of stages, each stage including mixing and settling units. In the first stage, hot brine and arm working fluid are intimately mixed and passed into a settler wherein the brine settles to the bottom of the settler and the hot working fluid rises to the top. The hot working fluid is passed to a heat engine or turbine to produce work and the working fluid is then recycled back into the system. The system is comprised of a series of stages each containing a settler and mixer, and wherein the working fluid and the brine flow in a countercurrent manner through the stages to recover the heat from the brine in increments and raise the temperature of the working fluid in increments.

Application of silver ion in the separation of macrolide antibiotic components by high-speed counter-current chromatography.

PubMed

Wen, Yaoming; Wang, Jiaoyan; Chen, Xiuming; Le, Zhanxian; Chen, Yuxiang; Zheng, Wei

2009-05-29

Three macrolide antibiotic components - ascomycin, tacrolimus and dihydrotacrolimus - were separated and purified by silver ion high-speed counter-current chromatography (HSCCC). The solvent system consisted of n-hexane-tert-butyl methyl ether-methanol-water (1:3:6:5, v/v) and silver nitrate (0.10mol/l). The silver ion acted as a pi-complexing agent with tacrolimus because of its extra side double bond compared with ascomycin and dihydrotacrolimus. This complexation modified the partition coefficient values and the separation factors of the three components. As a result, ascomycin, tacrolimus and dihydrotacrolimus were purified from 150mg extracted crude sample with purities of 97.6%, 98.7% and 96.5%, respectively, and yields over 80% (including their tautomers). These results cannot be achieved with the same solvent system but without the addition of silver ion.

Preparative isolation and purification of chemical constituents from the root of Adenophora tetraphlla by high-speed counter-current chromatography with evaporative light scattering detection.

PubMed

Yao, Shun; Liu, Renming; Huang, Xuefeng; Kong, Lingyi

2007-01-19

Preparative high-speed counter-current chromatography (HSCCC), as a continuous liquid-liquid partition chromatography with no solid support matrix, combined with evaporative light scattering detection (ELSD) was employed for systematic separation and purification of non-chromophoric chemical components from Chinese medicinal herb Adenophora tetraphlla (Thunb.), Fisch. Nine compounds, including alpha-spinasterol, beta-sitosterol, nonacosan-10-ol, 24-methylene cycloartanol, lupenone, 3-O-palmitoyl-beta-sitosterol, 3-O-beta-d-glucose-beta-sitosterol, eicosanoic acid and an unknown compound, were obtained. The compounds were all above 95% determined by high-performance liquid chromatography (HPLC)-ELSD, and their structures were identified by (1)H NMR and chemical ionization mass spectroscopy (CI-MS). The results demonstrate that HSCCC coupled with ELSD is a feasible and efficient technique for systematic isolation of non-chromophoric components from traditional medicinal herbs.

Isolation and Purification of Two Isoflavones from Hericium erinaceum Mycelium by High-Speed Counter-Current Chromatography.

PubMed

He, Jinzhe; Fan, Peng; Feng, Simin; Shao, Ping; Sun, Peilong

2018-03-02

High-speed counter-current chromatography (HSCCC) was used to separate and purify two isoflavones for the first time from Hericium erinaceum ( H. erinaceum ) mycelium using a two-phase solvent system composed of chloroform-dichloromethane-methanol-water (4:2:3:2, v / v / v / v ). These two isoflavones were identified as genistein (4',5,7-trihydroxyisoflavone, C 15 H 10 O₅) and daidzein (4',7-dihydroxyisoflavone, C 15 H 10 O₄), using infrared spectroscopy (IR), electro-spary ionisation mass (ESI-MS), ¹H-nuclear magnetic resonance (NMR) and 13 C-NMR spectra. About 23 mg genistein with 95.7% purity and 18 mg daidzein with 97.3% purity were isolated from 150 mg ethanolic extract of H. erinaceum mycelium. The results demonstrated that HSCCC was a feasible method to separate and purify genistein and daidzein from H. erinaceum mycelium.

Glycolic acid physical properties and impurities assessment

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

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

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

PH-zone-refining counter-current chromatography with a hydrophilic organic/salt-containing two-phase solvent system for preparative separation of polar alkaloids from natural products.

PubMed

Zou, Denglang; Du, Yurong; Kuang, Jianyuan; Sun, Shihao; Ma, Jianbin; Jiang, Renwang

2018-06-08

This study presents an efficient strategy based on pH-zone-refining counter-current chromatography with a hydrophilic organic/salt-containing two-phase system composed of acetonitrile, sodium chloride and water for preparative separation of polar alkaloids from natural products. Acetonitrile-sodium chloride-water system provides a wider range of polarity for polar alkaloids than classical aqueous two-phase systems. It gets rid of the effect of free hydrogen ion, strong ionic strength, hold low viscosity and the sharp retainer border could be formed easily. So acetonitrile-sodium chloride-water system showed great advantages to pH-zone-refining counter-current chromatography for polar alkaloids. The separation of polar indole alkaloids from toad venom was selected as an example to show the advantage and practicability of this strategy. An optimized acetonitrile-sodium chloride-water (54%:5%:41%, w%) system was applied in this study, where 10 mM triethylamine (TEA) as the retainer and 15 mM hydrochloric acid (HCl) as the eluter were added. As a result, three polar indole alkaloids, including 19 mg of serotonin, 45 mg of 5-Hydroxy-N'-methyl tryptamine, 33 mg of bufotenine were simultaneously separated from 500 mg of 5% ethanol elution fraction of toad venom on macroporous resin chromatography, with the purity of 91.3%, 97.5% and 89.4%, respectively. Their structures were identified by spectroscopic analysis. Copyright © 2018 Elsevier B.V. All rights reserved.

Magnetic nanoparticles and high-speed countercurrent chromatography coupled in-line and using the same solvent system for separation of quercetin-3-O-rutinoside, luteoloside and astragalin from a Mikania micrantha extract.

PubMed

Wang, Juanqiang; Geng, Shan; Wang, Binghai; Shao, Qian; Fang, Yingtong; Wei, Yun

2017-07-28

A new in-line method of magnetic nanoparticles (MNPs) coupled with high-speed countercurrent chromatography (HSCCC) using a same solvent system during the whole separation process was established to achieve the rapid separation of flavonoids from Mikania micrantha. The adsorption and desorption capacities of five different MNPs for flavonoid standards and Mikania micrantha crude extract were compared and the most suitable magnetic nanoparticle Fe 3 O 4 @SiO 2 @DIH@EMIMLpro was selected as the in-line MNP column. An in-line separation system was established by combining this MNP column with HSCCC through a six-way valve. The comparison between two solvent systems n-hexane-ethyl acetate-methanol-water (3:5:3:5, v/v) and ethyl acetate-methanol-water (25:1:25, v/v) showed that the latter solvent system was more suitable for simultaneously in-line separating three flavonoids quercetin-3-O-rutinoside, luteoloside and astragalin from Mikania micrantha. The purities of these three compounds with the ethyl acetate-methanol-water solvent system were 95.13%, 98.54% and 98.19% respectively. Results showed the established in-line separation system of MNP-HSCCC was efficient, recyclable and served to isolate potential flavonoids with similar polarities from natural complex mixtures. The in-line combination of magnetic nanoparticles with high-speed countercurrent chromatography eluting with the same solvent system during the whole separation process was established for the first time. Copyright © 2017 Elsevier B.V. All rights reserved.

Target-guided separation of Bougainvillea glabra betacyanins by direct coupling of preparative ion-pair high-speed countercurrent chromatography and electrospray ionization mass-spectrometry.

PubMed

Jerz, Gerold; Wybraniec, Sławomir; Gebers, Nadine; Winterhalter, Peter

2010-07-02

In this study, preparative ion-pair high-speed countercurrent chromatography was directly coupled to an electrospray ionization mass-spectrometry device (IP-HSCCC/ESI-MS-MS) for target-guided fractionation of high molecular weight acyl-oligosaccharide linked betacyanins from purple bracts of Bougainvillea glabra (Nyctaginaceae). The direct identification of six principal acyl-oligosaccharide linked betacyanins in the mass range between m/z 859 and m/z 1359 was achieved by positive ESI-MS ionization and gave access to the genuine pigment profile already during the proceeding of the preparative separation. Inclusively, all MS/MS-fragmentation data were provided during the chromatographic run for a complete analysis of substitution pattern. On-line purity evaluation of the recovered fractions is of high value in target-guided screening procedures and for immediate decisions about suitable fractions used for further structural analysis. The applied preparative hyphenation was shown to be a versatile screening method for on-line monitoring of countercurrent chromatographic separations of polar crude pigment extracts and also traced some minor concentrated compounds. For the separation of 760mg crude pigment extract the biphasic solvent system tert.-butylmethylether/n-butanol/acetonitrile/water 2:2:1:5 (v/v/v/v) was used with addition of ion-pair forming reagent trifluoroacetic acid. The preparative HSCCC-eluate had to be modified by post-column addition of a make-up solvent stream containing formic acid to reduce ion-suppression caused by trifluoroacetic acid and later significantly maximized response of ESI-MS/MS detection of target substances. A variable low-pressure split-unit guided a micro-eluate to the ESI-MS-interface for sensitive and direct on-line detection, and the major volume of the effluent stream was directed to the fraction collector for preparative sample recovery. The applied make-up solvent mixture significantly improved smoothness of the continuously measured IP-HSCCC-ESI-MS base peak ion trace in the experimental range of m/z 50-2200 by masking stationary phase bleeding and generating a stable single solvent phase for ESI-MS/MS detection. Immediate structural data were retrieved throughout the countercurrent chromatography run containing complete MS/MS-fragmentation pattern of the separated acyl-substituted betanidin oligoglycosides. Single ion monitoring indicated clearly the base-line separation of higher concentrated acylated betacyanin components. Copyright 2010 Elsevier B.V. All rights reserved.

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

Venkataraman, M.; Natarajan, R.; Raj, Baldev

The reprocessing of spent fuel from Fast Breeder Test Reactor (FBTR) has been successfully demonstrated in the pilot plant, CORAL (COmpact Reprocessing facility for Advanced fuels in Lead shielded cell). Since commissioning in 2003, spent mixed carbide fuel from FBTR of different burnups and varying cooling period, have been reprocessed in this facility. Reprocessing of the spent fuel with a maximum burnup of 100 GWd/t has been successfully carried out so far. The feed backs from these campaigns with progressively increasing specific activities, have been useful in establishing a viable process flowsheet for reprocessing the Prototype Fast Breeder Reactor (PFBR)more » spent fuel. Also, the design of various equipments and processes for the future plants, which are either under design for construction, namely, the Demonstration Fast Reactor Fuel Reprocessing Plant (DFRP) and the Fast reactor fuel Reprocessing Plant (FRP) could be finalized. (authors)« less

An Efficient Strategy Based on Liquid-Liquid Extraction with Three-Phase Solvent System and High Speed Counter-Current Chromatography for Rapid Enrichment and Separation of Epimers of Minor Bufadienolide from Toad Meat.

PubMed

Zou, Denglang; Zhu, Xuelin; Zhang, Fan; Du, Yurong; Ma, Jianbin; Jiang, Renwang

2018-01-31

This study presents an efficient strategy based on liquid-liquid extraction with three-phase solvent system and high speed counter-current chromatography for rapid enrichment and separation of epimers of minor bufadienolide from toad meat. The reflux extraction conditions were optimized by response surface methodology first, and a novel three-phase solvent system composed of n-hexane/methyl acetate/acetonitrile/water (3:6:5:5, v/v) was developed for liquid-liquid extraction of the crude extract. This integrative extraction process could enrich minor bufadienolide from complex matrix efficiently and minimize the loss of minor targets induced by repeated extraction with different kinds of organic solvents occurring in the classical liquid two-phase extraction. As a result, four epimers of minor bufadienolide were greatly enriched in the middle phase and total content of these epimers of minor bufadienolide was increased from 3.25% to 46.23%. Then, the enriched four epimers were separated by HSCCC with a two-phase solvent system composed of chloroform/methanol/water (4:2:2, v/v) successfully. Furthermore, we tested Na + ,K + -ATPase (NKA) inhibitory effect of the four epimers. 3β-Isomers of bufadienolide showed stronger (>8-fold) inhibitory activity than 3α-isomers. The characterization of minor bufadienolide in toad meat and their significant difference of inhibitory effect on NKA would promote the further quantitative analysis and safety evaluation of toad meat as a food source.

Separation of flavonoids from Millettia griffithii with high-performance counter-current chromatography guided by anti-inflammatory activity.

PubMed

Tang, Huan; Wu, Bo; Chen, Kai; Pei, Heying; Wu, Wenshuang; Ma, Liang; Peng, Aihua; Ye, Haoyu; Chen, Lijuan

2015-02-01

Millettia griffithii is a unique Chinese plant located in the southern part of Yunnan Province. Up to now, there is no report about its phytochemical or related bioactivity research. In our previous study, the n-hexane crude extract of Millettia griffithii revealed significant anti-inflammatory activity at 100 μg/mL, inspiring us to explore the anti-inflammatory constituents. Four fractions (I, II, III, and A) were fractionated from n-hexane crude extract by high-performance counter-current chromatography with solvent system composed of n-hexane/ethyl acetate/methanol/water (8:9:8:9, v/v) and then were investigated for the potent anti-inflammatory activity. Fraction A, with the most potent inhibitory activity was further separated to give another four fractions (IV, V, VI, and B) with solvent system composed of n-hexane/ethyl acetate/methanol/water (8:4:8:4, v/v). Compound V and fraction B exhibited remarkable anti-inflammatory activity with nitric oxide inhibitory rate of 80 and 65%, which was worth further fractionation. Then, three fractions (VII, VIII, and IX) were separated from fraction B with a solvent system composed of n-hexane/ethyl acetate/methanol/water (8:1:8:1, v/v), with compound VIII demonstrating the most potent inhibitory activity (80%). Finally, the IC50 values of compound V and VIII were tested as 38.2 and 14.9 μM. The structures were identified by electrospray ionization mass spectrometry and(1)H and (13)C NMR spectroscopy. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Using the liquid nature of the stationary phase in countercurrent chromatography. IV. The cocurrent CCC method.

PubMed

Berthod, Alain; Hassoun, Mahmoud

2006-05-26

The retention volumes of solutes in countercurrent chromatography (CCC) are directly proportional to their distribution coefficients, K(D) in the biphasic liquid system used as mobile and stationary phase in the CCC column. The cocurrent CCC method consists in putting the liquid "stationary" phase in slow motion in the same direction as the mobile phase. A mixture of five steroid compounds of widely differing polarities was used as a test mixture to evaluate the capabilities of the method with the biphasic liquid system made of water/methanol/ethyl acetate/heptane 6/5/6/5 (v/v) and a 53 mL CCC column of the coil planet centrifuge type. It is shown that the chromatographic resolution obtained in cocurrent CCC is very good because the solute band broadening is minimized as long as the solute is located inside the "stationary" phase. Pushing the method at its limits, it is demonstrated that the five steroids can still be (partly) separated when the flow rate of the two liquid phases is the same (2 mL/min). This is due to the higher volume of upper phase (72% of the column volume) contained inside the CCC column producing a lower linear speed compared to the aqueous lower phase linear speed. The capabilities of the cocurrent CCC method compare well with those of the gradient elution method in HPLC. Continuous detection is a problem due to the fact that two immiscible liquid phases elute from the column. It was partly solved using an evaporative light scattering detector.

Sludge Washing and Demonstration of the DWPF Nitric/Formic Flowsheet in the SRNL Shielded Cells for Sludge Batch 9 Qualification

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

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

Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) to qualify the next batch of sludge – Sludge Batch 9 (SB9). Current practice is to prepare sludge batches in Tank 51 by transferring sludge to Tank 51 from other tanks. The sludge is washed and transferred to Tank 40, the current Defense Waste Process Facility (DWPF) feed tank. Prior to sludge transfer from Tank 51 to Tank 40, the Tank 51 sludge must be qualified. SRNL qualifies the sludge in multiple steps. First, a Tank 51 sample is received, then characterized, washed, and again characterized. SRNL thenmore » demonstrates the DWPF Chemical Process Cell (CPC) flowsheet with the sludge. The final step of qualification involves chemical durability measurements of glass fabricated in the DWPF CPC demonstrations. In past sludge batches, SRNL had completed the DWPF demonstration with Tank 51 sludge. For SB9, SRNL has been requested to process a blend of Tank 51 and Tank 40 at a targeted ratio of 44% Tank 51 and 56% Tank 40 on an insoluble solids basis.« less

Validation of Kinetic-Turbulent-Neoclassical Theory for Edge Intrinsic Rotation in DIII-D Plasmas

NASA Astrophysics Data System (ADS)

Ashourvan, Arash

2017-10-01

Recent experiments on DIII-D with low-torque neutral beam injection (NBI) have provided a validation of a new model of momentum generation in a wide range of conditions spanning L- and H-mode with direct ion and electron heating. A challenge in predicting the bulk rotation profile for ITER has been to capture the physics of momentum transport near the separatrix and steep gradient region. A recent theory has presented a model for edge momentum transport which predicts the value and direction of the main-ion intrinsic velocity at the pedestal-top, generated by the passing orbits in the inhomogeneous turbulent field. In this study, this model-predicted velocity is tested on DIII-D for a database of 44 low-torque NBI discharges comprised of bothL- and H-mode plasmas. For moderate NBI powers (PNBI<4 MW), model prediction agrees well with the experiments for both L- and H-mode. At higher NBI power the experimental rotation is observed to saturate and even degrade compared to theory. TRANSP-NUBEAM simulations performed for the database show that for discharges with nominally balanced - but high powered - NBI, the net injected torque through the edge can exceed 1 N.m in the counter-current direction. The theory model has been extended to compute the rotation degradation from this counter-current NBI torque by solving a reduced momentum evolution equation for the edge and found the revised velocity prediction to be in agreement with experiment. Projecting to the ITER baseline scenario, this model predicts a value for the pedestal-top rotation (ρ 0.9) comparable to 4 kRad/s. Using the theory modeled - and now tested - velocity to predict the bulk plasma rotation opens up a path to more confidently projecting the confinement and stability in ITER. Supported by the US DOE under DE-AC02-09CH11466 and DE-FC02-04ER54698.

Continuous countercurrent membrane column for the separation of solute/solvent and solvent/solvent systems

DOEpatents

Nerad, Bruce A.; Krantz, William B.

1988-01-01

A reverse osmosis membrane process or hybrid membrane - complementary separator process for producing enriched product or waste streams from concentrated and dilute feed streams for both solvent/solvent and solute/solvent systems is described.

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

Newell, J; Miller, D; Stone, M

The Savannah River National Laboratory (SRNL) was tasked to provide an assessment of the downstream impacts to the Defense Waste Processing Facility (DWPF) of decisions regarding the implementation of Al-dissolution to support sludge mass reduction and processing. Based on future sludge batch compositional projections from the Liquid Waste Organization's (LWO) sludge batch plan, assessments have been made with respect to the ability to maintain comparable projected operating windows for sludges with and without Al-dissolution. As part of that previous assessment, candidate frits were identified to provide insight into melt rate for average sludge batches representing with and without Al-dissolution flowsheets.more » Initial melt rate studies using the melt rate furnace (MRF) were performed using five frits each for Cluster 2 and Cluster 4 compositions representing average without and with Al-dissolution. It was determined, however, that the REDOX endpoint (Fe{sup 2+}/{Sigma}Fe for the glass) for Clusters 2 and 4 resulted in an overly oxidized feed which negatively affected the initial melt rate tests. After the sludge was adjusted to a more reduced state, additional testing was performed with frits that contained both high and low concentrations of sodium and boron oxides. These frits were selected strictly based on the ability to ascertain compositional trends in melt rate and did not necessarily apply to any acceptability criteria for DWPF processing. The melt rate data are in general agreement with historical trends observed at SRNL and during processing of SB3 (Sludge Batch 3)and SB4 in DWPF. When MAR acceptability criteria were applied, Frit 510 was seen to have the highest melt rate at 0.67 in/hr for Cluster 2 (without Al-dissolution), which is compositionally similar to SB4. For Cluster 4 (with Al-dissolution), which is compositionally similar to SB3, Frit 418 had the highest melt rate at 0.63 in/hr. Based on this data, there appears to be a slight advantage of the Frit 510 based system without Al-dissolution relative to the Frit 418 based system with Al-dissolution. Though the without aluminum dissolution scenario suggests a slightly higher melt rate with frit 510, several points must be taken into consideration: (1) The MRF does not have the ability to assess liquid feeds and, thus, rheology impacts. Instead, the MRF is a 'static' test bed in which a mass of dried melter feed (SRAT product plus frit) is placed in an 'isothermal' furnace for a period of time to assess melt rate. These conditions, although historically effective in terms of identifying candidate frits for specific sludge batches and mapping out melt rate versus waste loading trends, do not allow for assessments of the potential impact of feed rheology on melt rate. That is, if the rheological properties of the slurried melter feed resulted in the mounding of the feed in the melter (i.e., the melter feed was thick and did not flow across the cold cap), melt rate and/or melter operations (i.e., surges) could be negatively impacted. This could affect one or both flowsheets. (2) Waste throughput factors were not determined for Frit 510 and Frit 418 over multiple waste loadings. In order to provide insight into the mission life versus canister count question, one needs to define the maximum waste throughput for both flowsheets. Due to funding limitations, the melt rate testing only evaluated melt rate at a fixed waste loading. (3) DWPF will be processing SB5 through their facility in mid-November 2008. Insight into the over arching questions of melt rate, waste throughput, and mission life can be obtained directly from the facility. It is recommended that processing of SB5 through the facility be monitored closely and that data be used as input into the decision making process on whether to implement Al-dissolution for future sludge batches.« less

Evaluate the role of organic acids in the protection of ligands from radiolytic degradation

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

Miller, Anneka; Mezyk, Stehpen; Peterman, Dean

In the Advanced TALSPEAK process, the bis(2-ethylhexyl)phosphoric acid (HDEHP) extractant used in the traditional TALSPEAK process is replaced by the extractant 2-ethylhexylphosphonic acid mono-2-ethylhexyl ester (HEH[EHP]). In addition, the aqueous phase complexant and buffer used in traditional TALSPEAK is replaced with the combination of N-(2-hydroxyethyl)ethylenediamine-N,N’,N’-triacetic acid (HEDTA) and citric acid. In order to evaluate the possible impacts of gamma radiolysis upon the efficacy of the Advanced TALSPEAK flowsheet, aqueous and organic phases corresponding to the extraction section of the proposed flowsheet were irradiated in the INL test loop under an ambient atmosphere. The results of these studies conducted at INL,more » led INL researchers to conclude that the scarcity of values of rate constants for the reaction of hydroxyl radical with the components of the Advanced TALSPEAK process chemistry was severely limiting the interpretation of the results of radiolysis studies performed at the INL. In this work, the rate of reaction of hydroxyl radical with citric acid at several pH values was measured using a competitive pulse radiolysis technique. This report describes those results and is written in completion of milestone M3FT-16IN030102028, the goal of which was to evaluate the role of organic acids in the protection of ligands from radiolytic degradation. The results reported here demonstrate the importance of obtaining hydroxyl radical reaction rate data for the conditions that closely resemble actual solution conditions expected to be used in an actual solvent extraction process. This report describes those results and is written in completion of milestone M3FT-16IN030102028, the goal of which was to evaluate the role of organic acids in the protection of ligands from radiolytic degradation.« less

Auto-thermal reforming using mixed ion-electronic conducting ceramic membranes for a small-scale H₂ production plant.

PubMed

Spallina, Vincenzo; Melchiori, Tommaso; Gallucci, Fausto; van Sint Annaland, Martin

2015-03-18

The integration of mixed ionic electronic conducting (MIEC) membranes for air separation in a small-to-medium scale unit for H2 production (in the range of 650-850 Nm3/h) via auto-thermal reforming of methane has been investigated in the present study. Membranes based on mixed ionic electronic conducting oxides such as Ba0.5Sr0.5Co0.8Fe0.2O3-δ (BSCF) give sufficiently high oxygen fluxes at temperatures above 800 °C with high purity (higher than 99%). Experimental results of membrane permeation tests are presented and used for the reactor design with a detailed reactor model. The assessment of the H2 plant has been carried out for different operating conditions and reactor geometry and an energy analysis has been carried out with the flowsheeting software Aspen Plus, including also the turbomachines required for a proper thermal integration. A micro-gas turbine is integrated in the system in order to supply part of the electricity required in the system. The analysis of the system shows that the reforming efficiency is in the range of 62%-70% in the case where the temperature at the auto-thermal reforming membrane reactor (ATR-MR) is equal to 900 °C. When the electric consumption and the thermal export are included the efficiency of the plant approaches 74%-78%. The design of the reactor has been carried out using a reactor model linked to the Aspen flowsheet and the results show that with a larger reactor volume the performance of the system can be improved, especially because of the reduced electric consumption. From this analysis it has been found that for a production of about 790 Nm3/h pure H2, a reactor with a diameter of 1 m and length of 1.8 m with about 1500 membranes of 2 cm diameter is required.

Advances on the Transfer of Lipids by Lipid Transfer Proteins.

PubMed

Wong, Louise H; Čopič, Alenka; Levine, Tim P

2017-07-01

Transfer of lipid across the cytoplasm is an essential process for intracellular lipid traffic. Lipid transfer proteins (LTPs) are defined by highly controlled in vitro experiments. The functional relevance of these is supported by evidence for the same reactions inside cells. Major advances in the LTP field have come from structural bioinformatics identifying new LTPs, and from the development of countercurrent models for LTPs. However, the ultimate aim is to unite in vitro and in vivo data, and this is where much progress remains to be made. Even where in vitro and in vivo experiments align, rates of transfer tend not to match. Here we set out some of the advances that might test how LTPs work. Copyright © 2017. Published by Elsevier Ltd.

Partition efficiencies of newly fabricated universal high-speed counter-current chromatograph for separation of two different types of sugar derivatives with organic-aqueous two-phase solvent systems.

PubMed

Shinomiya, Kazufusa; Sato, Kazuki; Yoshida, Kazunori; Tokura, Koji; Maruyama, Hiroshi; Yanagidaira, Kazuhiro; Ito, Yoichiro

2013-12-27

A new design of universal high-speed counter-current chromatograph (HSCCC) was fabricated in our laboratory. It holds a set of four column holders symmetrically around the rotary frame at a distance of 11.2cm from the central axis. By engaging the stationary gear on the central axis of the centrifuge to the planetary gears on the column holder shaft through a set of idle gears, two pairs of diagonally located column holders simultaneously rotate about their own axes in the opposite directions: one forward (type-J planetary motion) and the other backward (type-I planetary motion) each synchronously with the revolution. Using the eccentric coil assembly, partition efficiencies produced by these two planetary motions were compared on the separation of two different types of sugar derivatives (4-methylumbelliferyl and 5-bromo-4-chloro-3-indoxyl sugar derivatives) using organic-aqueous two-phase solvent systems composed of n-hexane/ethyl acetate/1-butanol/methanol/water and aqueous 0.1M sodium tetraborate, respectively. With lower phase mobile, better peak resolution was obtained by the type-J forward rotation for both samples probably due to higher retention of the stationary phase. With upper phase mobile, however, similar peak resolutions were obtained between these two planetary motions for both sugar derivatives. The overall results indicate that the present universal HSCCC is useful for counter-current chromatographic separation since each planetary motion has its specific applications: e.g., vortex CCC by the type-I planetary motion and HSCCC by the type-J planetary motion both for separation of various natural and synthetic products. Copyright © 2013 Elsevier B.V. All rights reserved.

Multiple dual mode counter-current chromatography with variable duration of alternating phase elution steps.

PubMed

Kostanyan, Artak E; Erastov, Andrey A; Shishilov, Oleg N

2014-06-20

The multiple dual mode (MDM) counter-current chromatography separation processes consist of a succession of two isocratic counter-current steps and are characterized by the shuttle (forward and back) transport of the sample in chromatographic columns. In this paper, the improved MDM method based on variable duration of alternating phase elution steps has been developed and validated. The MDM separation processes with variable duration of phase elution steps are analyzed. Basing on the cell model, analytical solutions are developed for impulse and non-impulse sample loading at the beginning of the column. Using the analytical solutions, a calculation program is presented to facilitate the simulation of MDM with variable duration of phase elution steps, which can be used to select optimal process conditions for the separation of a given feed mixture. Two options of the MDM separation are analyzed: 1 - with one-step solute elution: the separation is conducted so, that the sample is transferred forward and back with upper and lower phases inside the column until the desired separation of the components is reached, and then each individual component elutes entirely within one step; 2 - with multi-step solute elution, when the fractions of individual components are collected in over several steps. It is demonstrated that proper selection of the duration of individual cycles (phase flow times) can greatly increase the separation efficiency of CCC columns. Experiments were carried out using model mixtures of compounds from the GUESSmix with solvent systems hexane/ethyl acetate/methanol/water. The experimental results are compared to the predictions of the theory. A good agreement between theory and experiment has been demonstrated. Copyright © 2014 Elsevier B.V. All rights reserved.

The United States Army Medical Department Journal. October-December 2011

DTIC Science & Technology

2011-12-01

flowsheet with documentation of continuous fluid resuscitation decreased morbidity and mortality from burn wounds.6 Compartment syndrome ALARACT (all...Army action) memo mandated a high index of suspicion for compartment syndrome and a standardized approach to guide providers in the evaluation and...supervisors and staff concerning scheduling in order to foster a positive work environment, avoid burnout , increase morale, lower absenteeism, and

The measurement of U(VI) and Np(IV) mass transfer in a single stage centrifugal contactor

NASA Astrophysics Data System (ADS)

May, I.; Birkett, E. J.; Denniss, I. S.; Gaubert, E. T.; Jobson, M.

2000-07-01

BNFL currently operates two reprocessing plants for the conversion of spent nuclear fuel into uranium and plutonium products for fabrication into uranium oxide and mixed uranium and plutonium oxide (MOX) fuels. To safeguard the future commercial viability of this process, BNFL is developing novel single cycle flowsheets that can be operated in conjunction with intensified centrifugal contactors.

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

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

Reboul, S. H.

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

Method of extracting iodine from liquid mixtures of iodine, water and hydrogen iodide

DOEpatents

Mysels, Karol J.

1979-01-01

The components of a liquid mixture consisting essentially of HI, water and at least about 50 w/o iodine are separated in a countercurrent extraction zone by treating with phosphoric acid containing at least about 90 w/o H.sub.3 PO.sub.4. The bottom stream from the extraction zone is substantially completely molten iodine, and the overhead stream contains water, HI, H.sub.3 PO.sub.4 and a small fraction of the amount of original iodine. When the water and HI are present in near-azeotropic proportions, there is particular advantage in feeding the overhead stream to an extractive distillation zone wherein it is treated with additional concentrated phosphoric acid to create an anhydrous HI vapor stream and bottoms which contain at least about 85 w/o H.sub.3 PO.sub.4. Concentration of these bottoms provides phosphoric acid infeed for both the countercurrent extraction zone and for the extractive distillation zone.

Isolation and Purification of Three Ecdysteroids from the Stems of Diploclisia glaucescens by High-Speed Countercurrent Chromatography and Their Anti-Inflammatory Activities In Vitro.

PubMed

Fang, Lei; Li, Jialian; Zhou, Jie; Wang, Xiao; Guo, Lanping

2017-08-07

High-speed counter-current chromatography was used to separate and purify ecdysteroids for the first time from the stems of Diploclisia glaucescens using a two-phase solvent system composed of ethyl acetate- n -butanol-ethanol-water (3:0.2:0.8:3, v / v ). Three ecdysteroids were obtained from 260 mg of ethyl acetate extract of the residue obtained after evaporation of the crude ethanolicextractof D. glaucescens in one-step separation, which were identified as paristerone ( I , 30.5 mg), ecdysterone ( II , 7.2 mg), and capitasterone ( III , 8.1 mg) by electrospray ionization mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR). Their anti-inflammatory activities were evaluated by measuring the inhibitory ratios of β-glucuronidase release in rat polymorphonuclear leukocytes (PMNs) induced by platelet-activating factor. Compounds I - III showed significant anti-inflammatory activities with IC 50 -values ranging from 1.51 to 11.68 μM, respectively.

Preparative isolation and purification of macrolactin antibiotics from marine bacterium Bacillus amyloliquefaciens using high-speed counter-current chromatography in stepwise elution mode.

PubMed

He, Shan; Wang, Hongqiang; Yan, Xiaojun; Zhu, Peng; Chen, Juanjuan; Yang, Rui

2013-01-11

Preparative high-speed counter-current chromatography (HSCCC) was successfully applied to the isolation and purification of two macrolactin antibiotics from marine bacterium Bacillus amyloliquefaciens for the first time using stepwise elution with a pair of two-phase solvent systems composed of n-hexane-ethyl acetate-methanol-water at (1:4:1:4, v/v) and (3:4:3:4, v/v). The preparative HSCCC separation was performed on 300 mg of crude sample yielding macrolactin B (22.7 mg) and macrolactin A (40.4 mg) in a one-step separation, with purities over 95% as determined by HPLC. The structures of these compounds were identified by MS, (1)H NMR and (13)C NMR. Our results demonstrated that HSCCC was an efficient technique to separate marine antibiotics, which provide an approach to solve the problem of their sample availability for drug development. Copyright © 2012 Elsevier B.V. All rights reserved.

Characterization of pigments from different high speed countercurrent chromatography wine fractions.

PubMed

Salas, Erika; Dueñas, Montserrat; Schwarz, Michael; Winterhalter, Peter; Cheynier, Véronique; Fulcrand, Hélène

2005-06-01

A red wine, made from Cabernet Sauvignon (60%) and Tannat (40%) cultivars, was fractionated by high speed countercurrent chromatography (HSCCC). The biphasic solvent system consisting of tert-butyl methyl ether/n-butanol/acetonitrile/water (2/2/1/5, acidified with 0.1% trifluoroacetic acid) was chosen for its demonstrated efficiency in separating anthocyanins. The different native and derived anthocyanins were identified on the basis of their UV-visible spectra, their elution time on reversed-phase high-performance liquid chromatography (HPLC), and their mass spectra, before and after thiolysis. The HSCCC method allowed the separation of different families of anthocyanin-derived pigments that were eluted in different fractions according to their structures. The hydrosoluble fraction was almost devoid of native anthocyanins. Further characterization (glucose quantification, UV-visible absorbance measurements) indicated that it contained flavanol and anthocyanin copolymers in which parts of the anthocyanin units were in colorless forms. Pigments in the hydrosoluble fraction showed increased resistance to sulfite bleaching and to the nucleophilic attack of water.

Novel linear and step-gradient counter-current chromatography for bio-guided isolation and purification of cytotoxic podophyllotoxins from Dysosma versipellis (Hance).

PubMed

Yang, Zhi; Liu, Xiaoman; Wang, Kuiwu; Cao, Xiaoji; Wu, Shihua

2013-03-01

Dysosma versipellis (Hance) is a famous traditional Chinese medicine for the treatment of snakebite, weakness, condyloma accuminata, lymphadenopathy, and tumors for thousands of years. In this work, four podophyllotoxin-like lignans including 4'-demethylpodophyllotoxin (1), α-peltatin (2), podophyllotoxin (3), β-peltatin (4) as major cytotoxic principles of D. versipellis were successfully isolated and purified by several novel linear and step gradient counter-current chromatography methods using the systems of hexane/ethyl acetate/methanol/water (4:6:3:7 and 4:6:4:6, v/v/v/v). Compared with isocratic elution, linear and step-gradient elution can provide better resolution and save more time for the separation of photophyllotoxin and its congeners. Their cytotoxicities were further evaluated and their structures were validated by high-resolution electrospray TOF MS and nuclear magnetic resonance spectra. All components showed potent anticancer activity against human hepatoma cells HepG2. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultrahigh pressure extraction of lignan compounds from Dysosma versipellis and purification by high-speed counter-current chromatography.

PubMed

Zhu, Qing; Liu, Feng; Xu, Meixia; Lin, Xiaojing; Wang, Xiao

2012-09-15

Ultrahigh pressure extraction (UPE) was employed to extract podophyllotoxin and 4'-demethylpodophyllotoxin from Dysosma versipellis. The effects of extraction parameters including extraction solvents, pressure, time and solid/liquid ratio were investigated using a High Hydrostatic Pressure Processor. The optimal condition for UPE of the target compounds was 80% methanol, 200 MPa of pressure, 1 min of extraction time and 1:12 (g/mL) of solid/liquid ratio. Podophyllotoxin and 4'-demethylpodophyllotoxin in the crude extract were purified by high-speed counter-current chromatography (HSCCC) with a two-phase solvent system composed of petroleum ether-ethyl acetate-methanol-water (10:10:8:12, v/v), and the fractions were analyzed by HPLC, ESI-MS and (1)H NMR. As a result, 73.7 mg podophyllotoxin and 16.5mg 4'-demethylpodophyllotoxin with purities over 96% were obtained from 260 mg crude sample in one-step separation. Copyright © 2012 Elsevier B.V. All rights reserved.

Effect of Coriolis force on counter-current chromatographic separation by centrifugal partition chromatography.

PubMed

Ikehata, Jun-Ichi; Shinomiya, Kazufusa; Kobayashi, Koji; Ohshima, Hisashi; Kitanaka, Susumu; Ito, Yoichiro

2004-02-06

The effect of Coriolis force on the counter-current chromatographic separation was studied using centrifugal partition chromatography (CPC) with four different two-phase solvent systems including n-hexane-acetonitrile (ACN); tert-butyl methyl ether (MtBE)-aqueous 0.1% trifluoroacetic acid (TFA) (1:1); MtBE-ACN-aqueous 0.1% TFA (2:2:3); and 12.5% (w/w) polyethylene glycol (PEG) 1000-12.5% (w/w) dibasic potassium phosphate. Each separation was performed by eluting either the upper phase in the ascending mode or the lower phase in the descending mode, each in clockwise (CW) and counterclockwise column rotation. Better partition efficiencies were attained by the CW rotation in both mobile phases in all the two-phase solvent systems examined. The mathematical analysis also revealed the Coriolis force works favorably under the CW column rotation for both mobile phases. The overall results demonstrated that the Coriolis force produces substantial effects on CPC separation in both organic-aqueous and aqueous-aqueous two-phase systems.

Separation and purification of triterpene saponins from roots of Radix phytolaccae by high-speed countercurrent chromatography coupled with evaporative light scattering detection

PubMed Central

Ma, Jie; Chen, Qianliang; Lai, Daowan; Sun, Wenji; Zhang, Tianyou; Ito, Yoichiro

2009-01-01

Coupled with evaporative light scattering detection, high-speed countercurrent chromatography was successfully applied for the first time to separation and purification of four triterpene saponins including esculentoside A, B, C and D from roots of Radix Phytolaccae. The separation was performed with an optimized two-phase solvent system composed of chloroform-methanol-water (4:4:2, v/v) using the lower phase as the mobile phase at a flow rate of 1.5 ml/min,. From 150 mg of crude extract 46.3 mg of esculentoside A, 21.8 mg of esculentoside B, 7.3 mg of esculentoside C, and 13.6 mg of esculentoside D were obtained at purities of 96.7%, 99.2%, 96.5% and 97.8%, respectively, as determined by HPLC analysis. The structures of the four triterpene saponins were identified by ESI-MS,1H NMR and 13C NMR. PMID:20454595

Gas-liquid countercurrent integration process for continuous biodiesel production using a microporous solid base KF/CaO as catalyst.

PubMed

Hu, Shengyang; Wen, Libai; Wang, Yun; Zheng, Xinsheng; Han, Heyou

2012-11-01

A continuous-flow integration process was developed for biodiesel production using rapeseed oil as feedstock, based on the countercurrent contact reaction between gas and liquid, separation of glycerol on-line and cyclic utilization of methanol. Orthogonal experimental design and response surface methodology were adopted to optimize technological parameters. A second-order polynomial model for the biodiesel yield was established and validated experimentally. The high determination coefficient (R(2)=98.98%) and the low probability value (Pr<0.0001) proved that the model matched the experimental data, and had a high predictive ability. The optimal technological parameters were: 81.5°C reaction temperature, 51.7cm fill height of catalyst KF/CaO and 105.98kPa system pressure. Under these conditions, the average yield of triplicate experiments was 93.7%, indicating the continuous-flow process has good potential in the manufacture of biodiesel. Copyright © 2012 Elsevier Ltd. All rights reserved.

Colonization of the Hawaiian Archipelago via Johnston Atoll: a characterization of oceanographic transport corridors for pelagic larvae using computer simulation

NASA Astrophysics Data System (ADS)

Kobayashi, Donald R.

2006-08-01

Larval transport between Johnston Atoll and the Hawaiian Archipelago was examined using computer simulation and high-resolution ocean current data. The effects of pelagic larval duration and spawning seasonality on long-distance transport and local retention were examined using a Lagrangian, individual-based approach. Retention around Johnston Atoll appeared to be low, and there appeared to be seasonal effects on both retention and dispersal. Potential larval transport corridors between Johnston Atoll and the Hawaiian Archipelago were charted. One corridor connects Johnston Atoll with the middle portion of the Hawaiian Archipelago in the vicinity of French Frigate Shoals. Another corridor connects Johnston Atoll with the lower inhabited islands in the vicinity of Kauai. Transport appears to be related to the subtropical countercurrent and the Hawaiian Lee countercurrent, both located to the west of the archipelago and flowing to the east. A new analytical tool, termed CONREC-IRC is presented for the quantification of spatial patterns.

Preparative isolation and purification of theaflavins and catechins by high-speed countercurrent chromatography.

PubMed

Wang, Kunbo; Liu, Zhonghua; Huang, Jian-an; Dong, Xinrong; Song, Lubing; Pan, Yu; liu, Fang

2008-05-15

High-speed countercurrent chromatography (HSCCC) has been applied for the separation of theaflavins and catechins. The HSCCC run was carried out with a two-phase solvent system composed of hexane-ethyl acetate-methanol-water-acetic acid (1:5:1:5:0.25, v/v) by eluting the lower aqueous phase at 2 ml/min at 700 rpm. The results indicated that pure theaflavin, theaflavins-3-gallate, theaflavins-3'-gallate and theaflavin-3,3'-digallate could be obtained from crude theaflavins sample and black tea. The structures of the isolated compounds were positively confirmed by (1)H NMR and (13)C NMR, MS analysis, HPLC data and TLC data. Meanwhile, catechins including epigallocatechin gallate, gallocatechin gallate, epicatechin gallate and epigallocatechin were isolated from the aqueous extract of green tea by using the same solvent system. This study developed a modified method combined with enrichment theaflavins method by using HSCCC for separation of four individual theaflavins, especially for better separation of theaflavins monogallates.

Pulsed counter-current ultrasound-assisted extraction and characterization of polysaccharides from Boletus edulis.

PubMed

You, Qinghong; Yin, Xiulian; Ji, Chaowen

2014-01-30

Four methods for extracting polysaccharides from Boletus edulis, namely, hot-water extraction, ultrasonic clearer extraction, static probe ultrasonic extraction, and pulsed counter-current probe ultrasonic extraction (CCPUE), were studied. Results showed that CCPUE has the highest extraction efficiency among the methods studied. Under optimal CCPUE conditions, a B. edulis polysaccharide (BEP) yield of 8.21% was obtained. Three purified fractions, BEP-I, BEP-II, and BEP-III, were obtained through sequential purification by DEAE-52 and Sephadex G-75 chromatography. The average molecular weights of BEP-I, BEP-II, and BEP-III were 10,278, 23,761, and 42,736 Da, respectively. The polysaccharides were mainly composed of xylose, mannose, galactose, and glucose; of these, mannose contents were the highest. The antioxidant activities of the BEPs were further investigated by measurement of their ability to scavenge DPPH and hydroxyl radicals as well as their reducing power. The results indicated that the BEPs have good antioxidant activity. Copyright © 2013 Elsevier Ltd. All rights reserved.

High-throughput countercurrent microextraction in passive mode.

PubMed

Xie, Tingliang; Xu, Cong

2018-05-15

Although microextraction is much more efficient than conventional macroextraction, its practical application has been limited by low throughputs and difficulties in constructing robust countercurrent microextraction (CCME) systems. In this work, a robust CCME process was established based on a novel passive microextractor with four units without any moving parts. The passive microextractor has internal recirculation and can efficiently mix two immiscible liquids. The hydraulic characteristics as well as the extraction and back-extraction performance of the passive CCME were investigated experimentally. The recovery efficiencies of the passive CCME were 1.43-1.68 times larger than the best values achieved using cocurrent extraction. Furthermore, the total throughput of the passive CCME developed in this work was about one to three orders of magnitude higher than that of other passive CCME systems reported in the literature. Therefore, a robust CCME process with high throughputs has been successfully constructed, which may promote the application of passive CCME in a wide variety of fields.

Circulating moving bed system for CO.sub.2 separation, and method of same

DOEpatents

Elliott, Jeannine Elizabeth; Copeland, Robert James

2016-12-27

A circulating moving bed and process for separating a carbon dioxide from a gas stream is disclosed. The circulating moving bed can include an adsorption reactor and a desorption reactor, and a sorbent that moves through the two reactors. The sorbent can enter the adsorptive reactor and one end and move to an exit point distal to its entry point, while a CO.sub.2 feed stream can enter near the distal point and move countercurrently through the sorbent to exit at a position near the entry point of the sorbent. The sorbent can adsorb the CO.sub.2 by concentration swing adsorption and adsorptive displacement. The sorbent can then transfer to a regeneration reactor and can move countercurrently against a flow of steam through the regeneration reactor. The sorbent can be regenerated and the carbon dioxide recaptured by desorbing the carbon dioxide from the sorbent using concentration swing desorption and desorptive displacement with steam.

Chromium (Ⅵ) removal from aqueous solutions through powdered activated carbon countercurrent two-stage adsorption.

PubMed

Wang, Wenqiang

2018-01-01

To exploit the adsorption capacity of commercial powdered activated carbon (PAC) and to improve the efficiency of Cr(VI) removal from aqueous solutions, the adsorption of Cr(VI) by commercial PAC and the countercurrent two-stage adsorption (CTA) process was investigated. Different adsorption kinetics models and isotherms were compared, and the pseudo-second-order model and the Langmuir and Freundlich models fit the experimental data well. The Cr(VI) removal efficiency was >80% and was improved by 37% through the CTA process compared with the conventional single-stage adsorption process when the initial Cr(VI) concentration was 50 mg/L with a PAC dose of 1.250 g/L and a pH of 3. A calculation method for calculating the effluent Cr(VI) concentration and the PAC dose was developed for the CTA process, and the validity of the method was confirmed by a deviation of <5%. Copyright © 2017. Published by Elsevier Ltd.

One-step isolation of γ-oryzanol from rice bran oil by non-aqueous hydrostatic countercurrent chromatography.

PubMed

Angelis, Apostolis; Urbain, Aurélie; Halabalaki, Maria; Aligiannis, Nektarios; Skaltsounis, Alexios-Leandros

2011-09-01

The value-added γ-oryzanol was purified in one step from crude rice bran oil (RBO) using a preparative hydrostatic countercurrent chromatography (hydrostatic CCC) method, operating in the dual mode. The fractionation was performed using a non-aqueous biphasic solvent system consisting of heptane-acetonitrile-butanol (1.8:1.4:0.7, v/v/v), leading rapidly to the target compounds. Transfer of the analytical CCC method to large-scale isolation was also carried out yielding a high quantity-high purity fraction of γ-oryzanol. In addition, a fraction of hydroxylated triterpene alcohol ferulates (polar γ-oryzanol) was clearly separated and obtained. Furthermore, a fast HPLC-APCI(±)-HRMS method was developed and applied for the identification of γ-oryzanol as well as the polar γ-oryzanol in RBO and the resulting fractions. The purity of γ-oryzanol fraction was estimated as 97% based on HPLC-APCI-HRMS analysis. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

ORGANIC-HIGH IONIC STRENGTH AQUEOUS SOLVENT SYSTEMS FOR SPIRAL COUNTER-CURRENT CHROMATOGRAPHY: GRAPHIC OPTIMIZATION OF PARTITION COEFFICIENT

PubMed Central

Zeng, Yun; Liu, Gang; Ma, Ying; Chen, Xiaoyuan; Ito, Yoichiro

2012-01-01

A new series of organic-high ionic strength aqueous two-phase solvents systems was designed for separation of highly polar compounds by spiral high-speed counter-current chromatography. A total of 21 solvent systems composed of 1-butanol-ethanol-saturated ammonium sulfate-water at various volume ratios are arranged according to an increasing order of polarity. Selection of the two-phase solvent system for a single compound or a multiple sample mixture can be achieved by two steps of partition coefficient measurements using a graphic method. The capability of the method is demonstrated by optimization of partition coefficient for seven highly polar samples including tartrazine (K=0.77), tryptophan (K=1.00), methyl green (K= 0.93), tyrosine (0.81), metanephrine (K=0.89), tyramine (K=0.98), and normetanephrine (K=0.96). Three sulfonic acid components in D&C Green No. 8 were successfully separated by HSCCC using the graphic selection of the two-phase solvent system. PMID:23467197

SOLVENT EXTRACTION PROCESS FOR THE SEPARATION OF URANIUM AND THORIUM FROM PROTACTINIUM AND FISSION PRODUCTS

DOEpatents

Rainey, R.H.; Moore, J.G.

1962-08-14

A liquid-liquid extraction process was developed for recovering thorium and uranium values from a neutron irradiated thorium composition. They are separated from a solvent extraction system comprising a first end extraction stage for introducing an aqueous feed containing thorium and uranium into the system consisting of a plurality of intermediate extractiorr stages and a second end extractron stage for introducing an aqueous immiscible selective organic solvent for thorium and uranium in countercurrent contact therein with the aqueous feed. A nitrate iondeficient aqueous feed solution containing thorium and uranium was introduced into the first end extraction stage in countercurrent contact with the organic solvent entering the system from the second end extraction stage while intro ducing an aqueous solution of salting nitric acid into any one of the intermediate extraction stages of the system. The resultant thorium and uranium-laden organic solvent was removed at a point preceding the first end extraction stage of the system. (AEC)

Metal ion-improved complexation countercurrent chromatography for enantioseparation of dihydroflavone enantiomers.

PubMed

Han, Chao; Wang, Wenli; Xue, Guimin; Xu, Dingqiao; Zhu, Tianyu; Wang, Shanshan; Cai, Pei; Luo, Jianguang; Kong, Lingyi

2018-01-12

Cu(II) ion was selected as an additive to improve the enantioseparation efficiency of three dihydroflavone enantiomers in high-speed counter-current chromatography (HSCCC), using hydroxypropyl-β-cyclodextrin (HP-β-CyD) as the chiral selector. The influences of important parameters, including the metal ion, the concentrations of HP-β-CyD and the Cu(II) ion, and the sample size were investigated. Under optimal conditions, three dihydroflavone enantiomers, including (±)-hesperetin, (±)-naringenin, and (±)-farrerol, were successfully enantioseparated. The chiral recognition mechanism was investigated. The enantioseparation was attributed to the different thermodynamic stabilities of the binary complexes of HP-β-CyD and (±)-hesperetin, and Cu(II) ion could enhance this difference by forming ternary complexes with the binary complexes. This Cu(II) ion-improved complexation HSCCC system exhibited improved performance for chiral separation, and therefore it has great application potential in the preparative enantioseparation of other compounds with similar skeletons. Copyright © 2017 Elsevier B.V. All rights reserved.

Comprehensive separation of secondary metabolites in natural products by high-speed counter-current chromatography using a three-phase solvent system.

PubMed

Yanagida, Akio; Yamakawa, Yutaka; Noji, Ryoko; Oda, Ako; Shindo, Heisaburo; Ito, Yoichiro; Shibusawa, Yoichi

2007-06-01

High-speed counter-current chromatography (HSCCC) using the three-phase solvent system n-hexane-methyl acetate-acetonitrile-water at a volume ratio of 4:4:3:4 was applied to the comprehensive separation of secondary metabolites in several natural product extracts. A wide variety of secondary metabolites in each natural product was effectively extracted with the three-phase solvent system, and the filtered extract was directly submitted to the HSCCC separation using the same three-phase system. In the HSCCC profiles of crude natural drugs listed in the Japanese Pharmacopoeia, several physiologically active compounds were clearly separated from other components in the extracts. The HSCCC profiles of several tea products, each manufactured by a different process, clearly showed their compositional difference in main compounds such as catechins, caffeine, and pigments. These HSCCC profiles also provide useful information about hydrophobic diversity of whole components present in each natural product.

Separation of polyphenols and caffeine from the acetone extract of fermented tea leaves (Camellia sinensis) using high-performance countercurrent chromatography.

PubMed

Choi, Soo Jung; Hong, Yong Deog; Lee, Bumjin; Park, Jun Seong; Jeong, Hyun Woo; Kim, Wan Gi; Shin, Song Seok; Yoon, Kee Dong

2015-07-21

Leaves from Camellia sienensis are a popular natural source of various beverage worldwide, and contain caffeine and polyphenols derived from catechin analogues. In the current study, caffeine (CAF, 1) and three tea polyphenols including (-)-epigallocatechin 3-O-gallate (EGCg, 2), (-)-gallocatechin 3-O-gallate (GCg, 3), and (-)-epicatechin 3-O-gallate (ECg, 4) were isolated and purified by flow-rate gradient high-performance countercurrent chromatography (HPCCC) using a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (1:9:1:9, v/v). Two hundred milligrams of acetone-soluble extract from fermented C. sinensis leaves was separated by HPCCC to give 1 (25.4 mg), 2 (16.3 mg), 3 (11.1 mg) and 4 (4.4 mg) with purities over 98%. The structures of 1-4 were elucidated by QTOF-MS, as well as 1H- and 13C-NMR, and the obtained data were compared to the previously reported values.

Washing and caustic leaching of Hanford tank sludges: results of FY 1996 studies. Revision

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

Lumetta, G.J.; Rapko, B.M.; Wagner, M.J.

During the past few years, the primary mission at the US Department of Energy`s Hanford Site has changed from producing plutonium to restoring the environment. Large volumes of high-level radioactive wastes (HLW), generated during past Pu production and other operations, are stored in underground tanks on site. The current plan for remediating the Hanford tank farms consists of waste retrieval, pretreatment, treatment (immobilization), and disposal. The HLW will be immobilized in a borosilicate glass matrix and then disposed of in a geologic repository. Because of the expected high cost of HLW vitrification and geologic disposal, pretreatment processes will be implementedmore » to reduce the volume of borosilicate glass produced in disposing of the tank wastes. On this basis, a pretreatment plan is being developed. This report describes the sludge washing and caustic leaching test conducted to create a Hanford tank sludge pretreatment flowsheet.« less

ARC-2006-ACD06-0177-011

NASA Image and Video Library

2006-10-18

Ames Hypersonic Free Flight Aerodynamic Facility is used for research on gas dynamic problems of atmospheric entry. High relative speeds are achieved by launching models (in sabots if necessary) from high-speed guns into a countercurrent hypersonic air stream (14,000 ft/sec) driven by combustion-powered shock tube.

MICROBIAL COMETABOLISM OF RECALCITRANT CHEMICALS IN CONTAMINATED AIR STREAMS

EPA Science Inventory

Chlorinated Solvents: The treatment system consists of a laboratory-scale hollow fiber membrane (HFM) module containing a center baffle and a radial cross-flow pattern on the shell side of the fibers. The shell and lumen fluids are contacting in a counter-current f...

SPEEDUP{trademark} ion exchange column model

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

Hang, T.

2000-03-06

A transient model to describe the process of loading a solute onto the granular fixed bed in an ion exchange (IX) column has been developed using the SpeedUp{trademark} software package. SpeedUp offers the advantage of smooth integration into other existing SpeedUp flowsheet models. The mathematical algorithm of a porous particle diffusion model was adopted to account for convection, axial dispersion, film mass transfer, and pore diffusion. The method of orthogonal collocation on finite elements was employed to solve the governing transport equations. The model allows the use of a non-linear Langmuir isotherm based on an effective binary ionic exchange process.more » The SpeedUp column model was tested by comparing to the analytical solutions of three transport problems from the ion exchange literature. In addition, a sample calculation of a train of three crystalline silicotitanate (CST) IX columns in series was made using both the SpeedUp model and Purdue University's VERSE-LC code. All test cases showed excellent agreement between the SpeedUp model results and the test data. The model can be readily used for SuperLig{trademark} ion exchange resins, once the experimental data are complete.« less

Fuel Cycle Research & Development Technical Monthly-March 2012

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

Miller, Michael C.

2012-05-10

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

Evaluation of the Hydraulic Performance and Mass Transfer Efficiency of the CSSX Process with the Optimized Solvent in a Single Stage of 5.5-Cm Diameter Centrifugal Contactor

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

Law, J.D.; Tillotson, R.D.; Todd, T.A.

2002-09-19

The Caustic-Side Solvent Extraction (CSSX) process has been selected for the separation of cesium from Savannah River Site high-level waste. The solvent composition used in the CSSX process was recently optimized so that the solvent is no longer supersaturated with respect to the calixarene crown ether extractant. Hydraulic performance and mass transfer efficiency testing of a single stage of 5.5-cm ORNL-designed centrifugal contactor has been performed for the CSSX process with the optimized solvent. Maximum throughputs of the 5.5-cm centrifugal contactor, as a function of contactor rotor speed, have been measured for the extraction, scrub, strip, and wash sections ofmore » the CSSX flowsheet at the baseline organic/aqueous flow ratios (O/A) of the process, as well as at O/A's 20% higher and 20% lower than the baseline. Maximum throughputs are comparable to the design throughput of the contactor, as well as with throughputs obtained previously in a 5-cm centrifugal contactor with the non-optimized CSSX solvent formulation. The 20% variation in O/A had minimal effect on contactor throughput. Additionally, mass transfer efficiencies have been determined for the extraction and strip sections of the flowsheet. Efficiencies were lower than the process goal of greater than or equal to 80%, ranging from 72 to 75% for the extraction section and from 36 to 60% in the strip section. Increasing the mixing intensity and/or the solution level in the mixing zone of the centrifugal contactor (residence time) could potentially increase efficiencies. Several methods are available to accomplish this including (1) increasing the size of the opening in the bottom of the rotor, resulting in a contactor which is partially pumping instead of fully pumping, (2) decreasing the number of vanes in the contactor, (3) increasing the vane height, or (4) adding vanes on the rotor and baffles on the housing of the contactor. The low efficiency results obtained stress the importance of proper design of a centrifugal contactor for use in the CSSX process. A prototype of any centrifugal contactors designed for future pilot-scale or full-scale processing should be thoroughly tested prior to implementation.« less

Evaluation of the Hydraulic Capacity and Mass Transfer Efficiency of the CSSX Process with the Optimized Solvent in a Single Stage of 5.5-cm-Diameter Centrifugal Contactor

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

Law, Jack Douglas; Tillotson, Richard Dean; Todd, Terry Allen

2002-09-01

The Caustic-Side Solvent Extraction (CSSX) process has been selected for the separation of cesium from Savannah River Site high-level waste. The solvent composition used in the CSSX process was recently optimized so that the solvent is no longer supersaturated with respect to the calixarene crown ether extractant. Hydraulic performance and mass transfer efficiency testing of a single stage of 5.5-cm ORNL-designed centrifugal contactor has been performed for the CSSX process with the optimized solvent. Maximum throughputs of the 5.5-cm centrifugal contactor, as a function of contactor rotor speed, have been measured for the extraction, scrub, strip, and wash sections ofmore » the CSSX flowsheet at the baseline organic/aqueous flow ratios (O/A) of the process, as well as at O/A’s 20% higher and 20% lower than the baseline. Maximum throughputs are comparable to the design throughput of the contactor, as well as with throughputs obtained previously in a 5-cm centrifugal contactor with the non-optimized CSSX solvent formulation. The 20% variation in O/A had minimal effect on contactor throughput. Additionally, mass transfer efficiencies have been determined for the extraction and strip sections of the flowsheet. Efficiencies were lower than the process goal of greater than or equal to 80%, ranging from 72 to 75% for the extraction section and from 36 to 60% in the strip section. Increasing the mixing intensity and/or the solution level in the mixing zone of the centrifugal contactor (residence time) could potentially increase efficiencies. Several methods are available to accomplish this including (1) increasing the size of the opening in the bottom of the rotor, resulting in a contactor which is partially pumping instead of fully pumping, (2) decreasing the number of vanes in the contactor, (3) increasing the vane height, or (4) adding vanes on the rotor and baffles on the housing of the contactor. The low efficiency results obtained stress the importance of proper design of a centrifugal contactor for use in the CSSX process. A prototype of any centrifugal contactors designed for future pilot-scale or full-scale processing should be thoroughly tested prior to implementation.« less

Countercurrent extraction of soluble sugars from almond hulls and assessment of the bioenergy potential

USDA-ARS?s Scientific Manuscript database

Almond hulls contain considerable proportions (37 % by dry weight) of water soluble, fermentable sugars (sucrose, glucose, fructose) which can be extracted for industrial purposes. Optimization found that 20 % solids content was the maximum practical solids/liquor ratio for sugar extraction and tha...

How to Use Chromatography as a Science Teaching Aid.

ERIC Educational Resources Information Center

Ganis, Frank M.

Presented are five procedures which permit the effective teaching of chromatography with equipment which is readily available, economical, and simple in design. The first procedure involves a study of solute partition in two immiscible solvents and of countercurrent distribution. The second illustrates the use of unidimensional ascending paper…

Closed Fuel Cycle Waste Treatment Strategy

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

Vienna, J. D.; Collins, E. D.; Crum, J. V.

This study is aimed at evaluating the existing waste management approaches for nuclear fuel cycle facilities in comparison to the objectives of implementing an advanced fuel cycle in the U.S. under current legal, regulatory, and logistical constructs. The study begins with the Global Nuclear Energy Partnership (GNEP) Integrated Waste Management Strategy (IWMS) (Gombert et al. 2008) as a general strategy and associated Waste Treatment Baseline Study (WTBS) (Gombert et al. 2007). The tenets of the IWMS are equally valid to the current waste management study. However, the flowsheet details have changed significantly from those considered under GNEP. In addition, significantmore » additional waste management technology development has occurred since the GNEP waste management studies were performed. This study updates the information found in the WTBS, summarizes the results of more recent technology development efforts, and describes waste management approaches as they apply to a representative full recycle reprocessing flowsheet. Many of the waste management technologies discussed also apply to other potential flowsheets that involve reprocessing. These applications are occasionally discussed where the data are more readily available. The report summarizes the waste arising from aqueous reprocessing of a typical light-water reactor (LWR) fuel to separate actinides for use in fabricating metal sodium fast reactor (SFR) fuel and from electrochemical reprocessing of the metal SFR fuel to separate actinides for recycle back into the SFR in the form of metal fuel. The primary streams considered and the recommended waste forms include; Tritium in low-water cement in high integrity containers (HICs); Iodine-129: As a reference case, a glass composite material (GCM) formed by the encapsulation of the silver Mordenite (AgZ) getter material in a low-temperature glass is assumed. A number of alternatives with distinct advantages are also considered including a fused silica waste form with encapsulated nano-sized AgI crystals; Carbon-14 immobilized as a CaCO3 in a cement waste form; Krypton-85 stored as a compressed gas; An aqueous reprocessing high-level waste (HLW) raffinate waste immobilized by the vitrification process; An undissolved solids (UDS) fraction from aqueous reprocessing of LWR fuel either included in the borosilicate HLW glass or immobilized in the form of a metal alloy or titanate ceramics; Zirconium-based LWR fuel cladding hulls and stainless steel (SS) fuel assembly hardware super-compacted for disposal or purified for reuse (or disposal as low-level waste, LLW) of Zr by reactive gas separations; Electrochemical process salt HLW incorporated into a glass bonded Sodalite waste form; and Electrochemical process UDS and SS cladding hulls melted into an iron based alloy waste form. Mass and volume estimates for each of the recommended waste forms based on the source terms from a representative flowsheet are reported. In addition to the above listed primary waste streams, a range of secondary process wastes are generated by aqueous reprocessing of LWR fuel, metal SFR fuel fabrication, and electrochemical reprocessing of SFR fuel. These secondary wastes have been summarized and volumes estimated by type and classification. The important waste management data gaps and research needs have been summarized for each primary waste stream and selected waste process.« less

DWPF simulant CPC studies for SB8

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

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

2013-06-25

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

EXPERIMENTAL MOLTEN-SALT-FUELED 30-Mw POWER REACTOR

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

Alexander, L.G.; Kinyon, B.W.; Lackey, M.E.

1960-03-24

A preliminary design study was made of an experimental molten-salt- fueled power reactor. The reactor considered is a single-region homogeneous burner coupled with a Loeffler steam-generating cycle. Conceptual plant layouts, basic information on the major fuel circuit components, a process flowsheet, and the nuclear characteristics of the core are presented. The design plant electrical output is 10 Mw, and the total construction cost is estimated to be approximately ,000,000. (auth)

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

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

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

METHOD OF CENTRIFUGE OPERATION

DOEpatents

Cohen, K.

1960-05-10

A method of isotope separation is described in which two streams are flowed axially of, and countercurrently through, a cylindrical centrifuge bowl. Under the influence of a centrifugal field, the light fraction is concentrated in a stream flowing through the central portion of the bowl, whereas the heavy fraction is concentrated in a stream at the periphery thereof.

User's guide to the SEPHIS computer code for calculating the Thorex solvent extraction system

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

Watson, S.B.; Rainey, R.H.

1979-05-01

The SEPHIS computer program was developed to simulate the countercurrent solvent extraction process. The code has now been adapted to model the Acid Thorex flow sheet. This report represents a practical user's guide to SEPHIS - Thorex containing a program description, user information, program listing, and sample input and output.

A "Greenhouse Gas" Experiment for the Undergraduate Laboratory

ERIC Educational Resources Information Center

Gomez, Elaine; Paul, Melissa; Como, Charles; Barat, Robert

2014-01-01

This experiment and analysis offer an effective experience in greenhouse gas reduction. Ammoniated water is flowed counter-current to a simulated flue gas of air and CO2 in a packed column. The gaseous CO2 concentrations are measured with an on-line, non- dispersive, infrared analyzer. Column operating parameters include total gas flux, dissolved…

Countercurrent fixed-bed gasification of biomass at laboratory scale

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

Di Blasi, C.; Signorelli, G.; Portoricco, G.

1999-07-01

A laboratory-scale countercurrent fixed-bed gasification plant has been designed and constructed to produce data for process modeling and to compare the gasification characteristics of several biomasses (beechwood, nutshells, olive husks, and grape residues). The composition of producer gas and spatial temperature profiles have been measured for biomass gasification at different air flow rates. The gas-heating value always attains a maximum as a function of this operating variable, associated with a decrease of the air-to-fuel ratio. Optical gasification conditions of wood and agricultural residues give rise to comparable gas-heating values, comprised in the range 5--5.5 MJ/Nm{sup 3} with 28--30% CO, 5--7%more » CO{sub 2}, 6--8% H{sub 2}, 1--2% CH{sub 4}, and small amounts of C{sub 2}- hydrocarbons (apart from nitrogen). However, gasification of agricultural residues is more difficult because of bed transport, partial ash sintering, nonuniform flow distribution, and the presence of a muddy phase in the effluents, so that proper pretreatments are needed for largescale applications.« less

Isolation of two new prenylated flavonoids from Sinopodophyllum emodi fruit by silica gel column and high-speed counter-current chromatography.

PubMed

Sun, Yanjun; Sun, Yinshi; Chen, Hui; Hao, Zhiyou; Wang, Junmin; Guan, Yanbin; Zhang, Yanli; Feng, Weisheng; Zheng, Xiaoke

2014-10-15

Two new prenylated flavonoids, sinoflavonoids A-B, were isolated from the dried fruits of Sinopodophyllum emodi by silica gel column chromatography (SGCC) and high-speed counter-current chromatography (HSCCC). The 95% ethanol extract was partitioned with petroleum ether, dichloromethane, ethyl acetate, and n-butanol in water, respectively. The ethyl acetate fraction was pre-separated by SGCC with a petroleum ether-acetone gradient. The eluates containing target compounds were further separated by HSCCC with n-hexane-ethyl acetate-methanol-water (4:6:4:4, v/v). Finally, 17.3mg of sinoflavonoid A and 25.9mg of sinoflavonoid B were obtained from 100mg of the pretreated concentrate. The purities of sinoflavonoid A and sinoflavonoid B were 98.47% and 99.38%, respectively, as determined by HPLC. Their structures were elucidated on the basis of spectroscopic evidences (HR-ESI-MS, (1)H-NMR, (13)C-NMR, HSQC, HMBC). The separation procedures proved to be efficient, especially for trace prenylated flavonoids. Copyright © 2014 Elsevier B.V. All rights reserved.

Isolation and purification of prenylated phenolics from Amorpha fruticosa by high-speed counter-current chromatography.

PubMed

Chen, Chu; Wu, Yan; Chen, Yang; Du, Leilei

2015-08-01

Prenylated phenolics such as amorfrutins are recently identified potent anti-inflammatory and antidiabetic natural products. In this work, high-speed counter-current chromatography was investigated for the isolation and purification of prenylated phenolics from the fruits of Amorpha fruticosa by using a two-phase solvent system composed of n-hexane/ethanol/water (5:4:1, v/v). As a result, 14.2 mg of 5,7-dihydroxy-8-geranylflavanone, 10.7 mg of amorfrutin A and 17.4 mg of amorfrutin B were obtained from 200 mg of n-hexane-soluble crude extract in one step within 250 min. The purities of 5,7-dihydroxy-8-geranylflavanone, amorfrutins A and B were 95.2, 96.7 and 97.1%, respectively, as determined by ultra high performance liquid chromatography. The structural identification was performed by mass spectrometry and (1) H and (13) C NMR spectroscopy. The results indicated that the established method is an efficient and convenient way to purified prenylated phenolics from A. fruticosa extract. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Simultaneous isolation and purification of gallic acid and brevifolincarboxylic acid from Polygonum capitatum by high-speed counter-current chromatography].

PubMed

Chen, Xinxia; Zhang, Liyan; Wan, Jinzhi; Liang, Bin; Xie, Yu

2010-08-01

To isolate and purify gallic acid and brevifolincarboxylic acid simultaneously by high-speed counter-current chromatography (HSCCC) from a crude extract of Polygonum capitatum. The biphasic solvent system composed of ethyl acetate-n-butanol-0.44% acetic acid (3:1:5) was used at a flow rate of 2.0 mL x min(-1), while the aqueous phase was selected as the mobile phase and the apparatus was rotated at 860 r x min(-1). The effluent was detected at 272 nm. 51.5 mg of gallic acid and 5.9 mg of brevifolincarboxylic acid were separated from 1.07 g of the crude extract with the purities of 99.7% and 97.5%, respectively, while brevifolincarboxylic acid was obtained firstly from the genus Polygonum. The structures of the compounds were identified by ultraviolet spectrometry (UV), infra-red spectrometry (IR), liquid chromatography/mass spectrometry (LC/MS), time-of-flight mass spectrometry( TOF-MS), 1H-nuclear magnetic resonance (NMR) and 13C-NMR. This method is feasible and rapid for isolation and purification of gallice acid and brevifolincarboxylil acid.

Preparative isolation and purification of senkyunolide-I, senkyunolide-H and ferulic acid from Rhizoma Chuanxiong using counter-current chromatography.

PubMed

Wei, Yun; Hu, Jia; Li, Hao; Liu, Jiangang

2011-12-01

Three active compounds, senkyunolide-I, senkyunolide-H and ferulic acid (FA), were successfully isolated and purified from the extracts of Rhizoma Chuanxiong by counter-current chromatography (CCC). Based on the principle of the partition coefficient values (k) for target compounds and the separation factor (α) between target compounds, the two-phase solvent system that contains n-hexane-ethyl acetate-methanol-water at an optimized volume ratio of 3:7:4:6 v/v was selected for the CCC separation, and the lower phase was employed as the mobile phase in the head-to-tail elution mode. In a single run, 400 mg of the crude extract yielded pure senkyunolide-I (6.4 mg), senkyunolide-H (1.7 mg) and FA (4.4 mg) with the purities of 98, 93 and 99%, respectively. The CCC fractions were analyzed by high-performance liquid chromatography, and the structures of the three active compounds were identified by MS and (1)H NMR. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation of amaranthine-type betacyanins by ion-pair high-speed countercurrent chromatography.

PubMed

Jerz, Gerold; Gebers, Nadine; Szot, Dominika; Szaleniec, Maciej; Winterhalter, Peter; Wybraniec, Slawomir

2014-05-30

Betacyanins, red-violet plant pigments, were fractionated by ion-pair high-speed countercurrent chromatography (IP-HSCCC) from leaves extract of Iresine lindenii Van Houtte, an ornamental plant of the family Amaranthaceae. An HSCCC solvent system consisting of TBME-1-BuOH-ACN-H2O (1:3:1:5, v/v/v/v) was applied using ion-pair forming heptafluorobutyric acid (HFBA). Significantly different elution profiles of betacyanin diastereomeric pairs (derivatives based on betanidin and isobetanidin) observed in the HSCCC in comparison to HPLC systems indicate a complementarity of both techniques' fractionation capabilities. The numerous diastereomeric pairs can be selectively separated from each other using the HSCCC system simplifying the pigment purification process. Apart from the three well known highly abundant pigments (amaranthine, betanin and iresinin I) together with their isoforms, three new acylated (feruloylated and sinapoylated) betacyanins as well as known pigment hylocerenin (previously isolated from cacti fruits) were characterized in the plant for the first time and they are new for the whole Amaranthaceae family. Copyright © 2014 Elsevier B.V. All rights reserved.

Topsy-turvy: Turning the counter-current heat exchange of leatherback turtles upside down

USGS Publications Warehouse

Davenport, John; Jones, T. Todd; Work, Thierry M.; Balazs, George H.

2015-01-01

Counter-current heat exchangers associated with appendages of endotherms feature bundles of closely applied arteriovenous vessels. The accepted paradigm is that heat from warm arterial blood travelling into the appendage crosses into cool venous blood returning to the body. High core temperature is maintained, but the appendage functions at low temperature. Leatherback turtles have elevated core temperatures in cold seawater and arteriovenous plexuses at the roots of all four limbs. We demonstrate that plexuses of the hindlimbs are situated wholly within the hip musculature, and that, at the distal ends of the plexuses, most blood vessels supply or drain the hip muscles, with little distal vascular supply to, or drainage from the limb blades. Venous blood entering a plexus will therefore be drained from active locomotory muscles that are overlaid by thick blubber when the adults are foraging in cold temperate waters. Plexuses maintain high limb muscle temperature and avoid excessive loss of heat to the core, the reverse of the accepted paradigm. Plexuses protect the core from overheating generated by muscular thermogenesis during nesting.

Energy-efficient membrane separations in the sweetener industry. Final report for Phase I

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

Babcock, W.C.

1984-02-14

The objective of the program is to investigate the use of membrane processes as energy-efficient alternatives to conventional separation processes in current use in the corn sweetener industry. Two applications of membranes were studied during the program: (1) the concentration of corn steep water by reverse osmosis; and (2) the concentration of dilute wastes called sweetwater with a combination of reverse osmosis and a process known as countercurrent reverse osmosis. Laboratory experiments were conducted for both applications, and the results were used to conduct technical and economic analyses of the process. It was determined that the concentration of steep watermore » by reverse osmosis plus triple-effect evaporation offers savings of a factor of 2.5 in capital costs and a factor of 4.5 in operating costs over currently used triple-effect evaporation. In the concentration of sweetwater by reverse osmosis and countercurrent reverse osmosis, capital costs would be about the same as those for triple-effect evaporation, but operating costs would be only about one-half those of triple-effect evaporation.« less

Topsy-turvy: turning the counter-current heat exchange of leatherback turtles upside down.

PubMed

Davenport, John; Jones, T Todd; Work, Thierry M; Balazs, George H

2015-10-01

Counter-current heat exchangers associated with appendages of endotherms feature bundles of closely applied arteriovenous vessels. The accepted paradigm is that heat from warm arterial blood travelling into the appendage crosses into cool venous blood returning to the body. High core temperature is maintained, but the appendage functions at low temperature. Leatherback turtles have elevated core temperatures in cold seawater and arteriovenous plexuses at the roots of all four limbs. We demonstrate that plexuses of the hindlimbs are situated wholly within the hip musculature, and that, at the distal ends of the plexuses, most blood vessels supply or drain the hip muscles, with little distal vascular supply to, or drainage from the limb blades. Venous blood entering a plexus will therefore be drained from active locomotory muscles that are overlaid by thick blubber when the adults are foraging in cold temperate waters. Plexuses maintain high limb muscle temperature and avoid excessive loss of heat to the core, the reverse of the accepted paradigm. Plexuses protect the core from overheating generated by muscular thermogenesis during nesting. © 2015 The Author(s).

The impact of capillary backpressure on spontaneous counter-current imbibition in porous media

NASA Astrophysics Data System (ADS)

Foley, Amir Y.; Nooruddin, Hasan A.; Blunt, Martin J.

2017-09-01

We investigate the impact of capillary backpressure on spontaneous counter-current imbibition. For such displacements in strongly water-wet systems, the non-wetting phase is forced out through the inlet boundary as the wetting phase imbibes into the rock, creating a finite capillary backpressure. Under the assumption that capillary backpressure depends on the water saturation applied at the inlet boundary of the porous medium, its impact is determined using the continuum modelling approach by varying the imposed inlet saturation in the analytical solution. We present analytical solutions for the one-dimensional incompressible horizontal displacement of a non-wetting phase by a wetting phase in a porous medium. There exists an inlet saturation value above which any change in capillary backpressure has a negligible impact on the solutions. Above this threshold value, imbibition rates and front positions are largely invariant. A method for identifying this inlet saturation is proposed using an analytical procedure and we explore how varying multiphase flow properties affects the analytical solutions and this threshold saturation. We show the value of this analytical approach through the analysis of previously published experimental data.

Steady state preparative multiple dual mode counter-current chromatography: Productivity and selectivity. Theory and experimental verification.

PubMed

Kostanyan, Artak E; Erastov, Andrey A

2015-08-07

In the steady state (SS) multiple dual mode (MDM) counter-current chromatography (CCC), at the beginning of the first step of every cycle the sample dissolved in one of the phases is continuously fed into a CCC device over a constant time, not exceeding the run time of the first step. After a certain number of cycles, the steady state regime is achieved, where concentrations vary over time during each cycle, however, the concentration profiles of solutes eluted with both phases remain constant in all subsequent cycles. The objective of this work was to develop analytical expressions to describe the SS MDM CCC separation processes, which can be helpful to simulate and design these processes and select a suitable compromise between the productivity and the selectivity in the preparative and production CCC separations. Experiments carried out using model mixtures of compounds from the GUESSmix with solvent system hexane/ethyl acetate/methanol/water demonstrated a reasonable agreement between the predictions of the theory and the experimental results. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparative separation of cacao bean procyanidins by high-speed counter-current chromatography.

PubMed

Li, Lingxi; Zhang, Shuting; Cui, Yan; Li, Yuanyuan; Luo, Lanxin; Zhou, Peiyu; Sun, Baoshan

2016-11-15

In this work, an efficient method for preparative separation of procyanidins from raw cacao bean extract by high-speed counter-current chromatography (HSCCC) was developed. Under the optimized solvent system of n-hexane-ethyl acetate-water (1:50:50, v/v/v) with a combination of head-tail and tail-head elution modes, various procyanidins fractions with different polymerization degrees were successfully separated. UPLC, QTOF-MS and 1 H NMR analysis verified that these fractions contained monomer up to pentamer respectively. Dimeric procyanidin B2 (purity>86%) could be isolated by HSCCC in a single run. Other individual procyanidins in these fractions could be further isolated and purified by preparative HPLC. The developed HSCCC together with preparative HPLC techniques appeared to be a useful tool for large preparation of different procyanidins from cacao beans. Furthermore, by antioxidant activity assays, it was proved that both fractions and individual procyanidins possessed greater antioxidant activities compared to standard trolox. The antioxidant activities of procyanidins increase as the increase of their polymerization degree. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparative Isolation and Purification of Flavone C-Glycosides from the Leaves of Ficus microcarpa L. f by Medium-Pressure Liquid Chromatography, High-Speed Countercurrent Chromatography, and Preparative Liquid Chromatography

PubMed Central

Wang, Xiaohong; Liang, Yong; Zhu, Licai; Xie, Huichun; Li, Hang; He, Junting; Pan, Man; Zhang, Tianyou; Ito, Yoichiro

2009-01-01

Combined with medium-pressure liquid chromatography (MPLC) and preparative high-performance liquid chromatography (perp-HPLC), high-speed countercurrent chromatography (HSCCC) was applied for separation and purification of flavone C-glycosides from the crude extract of leaves of Ficus microcarpae L. f. HSCCC separation was performed on a two-phase solvent system composed of methyl tert- butyl ether - ethyl acetate – 1-butanol – acetonitrile – 0.1% aqueous trifluoroacetic acid at a volume ratio of 1:3:1:1:5. Partially resolved peak fractions from HSCCC separation were further purified by preparative HPLC. Four well-separated compounds were obtained and their purities were determined by HPLC. The purities of these peaks were 97.28%, 97.20%, 92.23%, and 98.40%.. These peaks were characterized by ESI-MSn. According to the reference, they were identified as orientin (peak I), isovitexin-3″-O-glucopyranoside (peak II), isovitexin (peak III), and vitexin (peak IV), yielded 1.2 mg, 4.5 mg, 3.3 mg, and 1.8 mg, respectively. PMID:20190866

A laplace transform-based technique for solving multiscale and multidomain problems: Application to a countercurrent hemodialyzer model.

PubMed

Simon, Laurent

2017-08-01

An integral-based method was employed to evaluate the behavior of a countercurrent hemodialyzer model. Solute transfer from the blood into the dialysate was described by writing mass balance equations over a section of the device. The approach provided Laplace transform concentration profiles on both sides of the membrane. Applications of the final value theorem led to the development of the effective time constants and steady-state concentrations in the exit streams. Transient responses were derived by a numerical inversion algorithm. Simulations show that the period elapsed, before reaching equilibrium in the effluents, decreased when the blood flow rate increased from 0.25 to 0.30 ml/s. The performance index decreased from 0.80 to 0.71 when the blood-to-dialysate flow ratio increased by 20% and increased from 0.80 to 0.85 when this fraction was reduced by 17%. The analytical solution predicted methadone removal in patients undergoing dialysis. Clinicians can use these findings to predict the time required to achieve a target extraction ratio. Copyright © 2017 Elsevier Ltd. All rights reserved.

Countercurrent extraction of soluble sugars from almond hulls and assessment of the bioenergy potential.

PubMed

Holtman, Kevin M; Offeman, Richard D; Franqui-Villanueva, Diana; Bayati, Andre K; Orts, William J

2015-03-11

Almond hulls contain considerable proportions (37% by dry weight) of water-soluble, fermentable sugars (sucrose, glucose, and fructose), which can be extracted for industrial purposes. The maximum optimal solids loading was determined to be 20% for sugar extraction, and the addition of 0.5% (w/v) pectinase aided in maintaining a sufficient free water volume for sugar recovery. A laboratory countercurrent extraction experiment utilizing a 1 h steep followed by three extraction (wash) stages produced a high-concentration (131 g/L fermentable sugar) syrup. Overall, sugar recovery efficiency was 88%. The inner stage washing efficiencies were compatible with solution equilibrium calculations, indicating that efficiency was high. The concentrated sugar syrup was fermented to ethanol at high efficiency (86% conversion), and ethanol concentrations in the broth were 7.4% (v/v). Thin stillage contained 233 g SCOD/L, which was converted to biomethane at an efficiency of 90% with a biomethane potential of 297 mL/g SCODdestroyed. Overall, results suggested that a minima of 49 gal (185 L) ethanol and 75 m(3) methane/t hulls (dry whole hull basis) are achievable.

Preparative separation of grape skin polyphenols by high-speed counter-current chromatography.

PubMed

Luo, Lanxin; Cui, Yan; Zhang, Shuting; Li, Lingxi; Li, Yuanyuan; Zhou, Peiyu; Sun, Baoshan

2016-12-01

To develop an efficient method for large preparation of various individual polyphenols from white grape skins (Fernão Pires; Vitis vinifera) by preparative high-speed counter-current chromatography (HSCCC) and preparative-HPLC, an optimized preparative HSCCC condition with two-phase solvent system composed of Hex-EtOAc-H2O (1:50:50, v/v) was used to separate grape skin polyphenols into various fractions. Both the tail-head and head-tail elution modes were used with a flow rate of 3.0ml/min and a rotary speed of 950rpm. Afterwards, a preparative-HPLC separation was applied to isolate individual polyphenols in each of the fractions from HSCCC. Total of 7 fractions (Fraction A to G) were obtained from grape skin extract by HSCCC. After preparative-HPLC isolation, fifteen individual compounds were obtained, most of which presented high yields and purity (all over 90%). The HSCCC method followed with preparative-HPLC appeared to be convenient and economical, constituting an efficient strategy for the isolation of grape skin polyphenols. Copyright © 2016 Elsevier Ltd. All rights reserved.

Preparative enantioseparation of propafenone by counter-current chromatography using di-n-butyl L-tartrate combined with boric acid as the chiral selector.

PubMed

Tong, Shengqiang; Shen, Mangmang; Zheng, Ye; Chu, Chu; Li, Xing-Nuo; Yan, Jizhong

2013-09-01

This paper extends the research of the utilization of borate coordination complexes in chiral separation by counter-current chromatography (CCC). Racemic propafenone was successfully enantioseparated by CCC with di-n-butyl l-tartrate combined with boric acid as the chiral selector. The two-phase solvent system was composed of chloroform/ 0.05 mol/L acetate buffer pH 3.4 containing 0.10 mol/L boric acid (1:1, v/v), in which 0.10 mol/L di-n-butyl l-tartrate was added in the organic phase. The influence of factors in the enantioseparation of propafenone were investigated and optimized. A total of 92 mg of racemic propafenone was completely enantioseparated using high-speed CCC in a single run, yielding 40-42 mg of (R)- and (S)-propafenone enantiomers with an HPLC purity over 90-95%. The recovery for propafenone enantiomers from fractions of CCC was in the range of 85-90%. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Countercurrent flow limited (CCFL) heat flux in the high flux isotope reactor (HFIR) fuel element

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

Ruggles, A.E.

1990-10-12

The countercurrent flow (CCF) performance in the fuel element region of the HFIR is examined experimentally and theoretically. The fuel element consists of two concentric annuli filled with aluminum clad fuel plates of 1.27 mm thickness separated by 1.27 mm flow channels. The plates are curved as they go radially outward to accomplish constant flow channel width and constant metal-to-coolant ratio. A full-scale HFIR fuel element mock-up is studied in an adiabatic air-water CCF experiment. A review of CCF models for narrow channels is presented along with the treatment of CCFs in system of parallel channels. The experimental results aremore » related to the existing models and a mechanistic model for the annular'' CCF in a narrow channel is developed that captures the data trends well. The results of the experiment are used to calculate the CCFL heat flux of the HFIR fuel assembly. It was determined that the HFIR fuel assembly can reject 0.62 Mw of thermal power in the CCFL situation. 31 refs., 17 figs.« less

Preparation of Sesquiterpenoids from Tussilago farfara L. by High-speed Counter-current Chromatography

PubMed Central

Cao, Kun; Xu, Yi; Zhao, Tian-Ming; Zhang, Qing

2016-01-01

Background: Sesquiterpenoids, such as tussilagone, has effects of raising blood pressure, antiplatelet aggregation, and anti-inflammation activities, which is regarded as index compound for quality control of Tussilago farfara L. Objective: This study was aimed to obtain an effective method for fast isolation of sesquiterpenoids from T. farfara L. by high-speed counter-current chromatography (HSCCC). Materials and Methods: A solvent optimization method for HSCCC was presented, i.e., the separation factors of compounds after the K values of solvent system should be investigated. Results: A ternary solvent system of n-hexane:methanol:water (5:8:2, v/v/v) was selected and applied for the HSCCC, and 56 mg of tussilagone (2) was isolated from T. farfara L., along with two other sesquiterpenoids 5.6 mg of 2,2-dimethyl-6-acetylchromanone (1) and 22 mg of 14-acetoxy-7 β-(3’-ethyl cis-crotonoyloxy)-lα-(2’-methylbutyryloxy)-notonipetranone (3) by HSCCC with high purities. Their chemical structures were elucidated by liquid chromatography-mass spectrometry and nuclear magnetic resonance experiments. Conclusion: These results offered an efficient strategy for preparation of potentially health-relevant phytochemicals from T. farfara L., which might be used for further chemical research and pharmacological studies by preparative HSCCC. SUMMARY The real separation efficiency has been verified by analytical HSCCC.A solvent optimization method for HSCCC was presented and applied to separate and prepare active compounds.A method for rapid and effective separation of target compound Tussilagone with high yield and purity from the flower buds of Tussilago farfara.Two other compounds 2,2-Dimethyl-6-acetylchromanone and 14-acetoxy-7β-(3’-ethyl cis-crotonoyloxy) -lα- (2’-methylbutyryloxy). notonipetranone hasbeen obtained with high purities from flower buds of Tussilago farfara. Abbreviations used: HSCCC: High-Speed Counter-Current Chromatography; LC-MS: Liquid Chromatograph-Mass Spectrometer; NMR: Nuclear Magnetic Resonance; TCM: Traditional Chinese Medicine; HPLC: High Performance Liquid Chromatography; ESI-MS: Electrospray Ionization Mass Spectrometry; PE: petroleum ether PMID:27867270

Heat and Momentum Transfer Studies in High Reynolds Number Wavy Films at Normal and Reduced Gravity Conditions

NASA Technical Reports Server (NTRS)

Balakotaiah, V.

1996-01-01

We examined the effect of the gas flow on the liquid film when the gas flows in the countercurrent direction in a vertical pipe at normal gravity conditions. The most dramatic effect of the simultaneous flow of gas and liquid in pipes is the greatly increased transport rates of heat, mass, and momentum. In practical situations this enhancement can be a benefit or it can result in serious operational problems. For example, gas-liquid flow always results in substantially higher pressure drop and this is usually undesirable. However, much higher heat transfer coefficients can be expected and this can obviously be of benefit for purposes of design. Unfortunately, designers know so little of the behavior of such two phase systems and as a result these advantages are not utilized. Due to the complexity of the second order boundary model as well as the fact that the pressure variation across the film is small compared to the imposed gas phase pressure, the countercurrent gas flow affect was studied for the standard boundary layer model. A different stream function that can compensate the shear stress affect was developed and this stream function also can predict periodic solutions. The discretized model equations were transformed to a traveling wave coordinate system. A stability analysis of these sets of equations showed the presence of a Hopf bifurcation for certain values of the traveling wave velocity and the shear stress. The Hopf celerity was increased due to the countercurrent shear. For low flow rate the increases of celerity are more than for the high flow rate, which was also observed in experiments. Numerical integration of a traveling wave simplification of the model also predicts the existence of chaotic large amplitude, nonperiodic waves as observed in the experiments. The film thickness was increased by the shear.

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

Zhang, Z.; Pike, R.W.; Hertwig, T.A.

An effective approach for source reduction in chemical plants has been demonstrated using on-line optimization with flowsheeting (ASPEN PLUS) for process optimization and parameter estimation and the Tjao-Biegler algorithm implemented in a mathematical programming language (GAMS/MINOS) for data reconciliation and gross error detection. Results for a Monsanto sulfuric acid plant with a Bailey distributed control system showed a 25% reduction in the sulfur dioxide emissions and a 17% improvement in the profit over the current operating conditions. Details of the methods used are described.

Preliminary technical data summary No. 3 for the Defense Waste Processing Facility

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

Landon, L.F.

1980-05-01

This document presents an update on the best information presently available for the purpose of establishing the basis for the design of a Defense Waste Processing Facility. Objective of this project is to provide a facility to fix the radionuclides present in Savannah River Plant (SRP) high-level liquid waste in a high-integrity form (glass). Flowsheets and material balances reflect the alternate CAB case including the incorporation of low-level supernate in concrete. (DLC)

A flowsheet concept for an Am/Ln separation based on Am{sup VI} solvent extraction

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

Mincher, B.J.; Law, J.D.

2013-07-01

The separation of Am from the lanthanides and curium is a key step in proposed advanced fuel cycle scenarios. The partitioning and transmutation of Am is desirable to minimize the long-term radiotoxicity of material interred in a future high-level waste repository. However, a separation amenable to process scale-up remains elusive. Higher oxidation states of americium have recently been used to demonstrate solvent extraction-based separations using conventional fuel cycle ligands. Here, the successful partitioning of Am{sup VI} from the bulk of lanthanides and curium using diamyl-amyl-phosphonate (DAAP) extraction is reported. Due to the instability of Am{sup VI} in the organic phasemore » it was readily selectively stripped to a new acidic aqueous phase to provide separation from co-extracted Ce{sup IV}. The use of NaBiO{sub 3} as an oxidant to separate Am from the lanthanides and Cm by solvent extraction has been successfully demonstrated on the bench scale. Based on these results, flowsheet concepts can be designed that result in 96 % Am recovery in the presence of a few percent of the remaining Cm and the lanthanides in two extraction contacts. Preliminary results also indicate that the DAAP extractant is robust toward γ- irradiation under realistic conditions of acidity and dissolved oxygen concentration.« less

Liquid cooled counter flow turbine bucket

DOEpatents

Dakin, James T.

1982-09-21

Means and a method are provided whereby liquid coolant flows radially outward through coolant passages in a liquid cooled turbine bucket under the influence of centrifugal force while in contact with countercurrently flowing coolant vapor such that liquid is entrained in the flow of vapor resulting in an increase in the wetted cooling area of the individual passages.

10 CFR Appendix E to Part 110 - Illustrative List of Chemical Exchange or Ion Exchange Enrichment Plant Equipment and Components...

Code of Federal Regulations, 2011 CFR

2011-01-01

... contactors employed in the separation cascade can be liquid-liquid exchange columns (such as pulsed columns.... Plastic, plastic-lined (including use of fluorocarbon polymers) and/or glass-lined columns and piping are therefore used. (1) Liquid-liquid exchange columns. Countercurrent liquid-liquid exchange columns having...

10 CFR Appendix E to Part 110 - Illustrative List of Chemical Exchange or Ion Exchange Enrichment Plant Equipment and Components...

Code of Federal Regulations, 2013 CFR

2013-01-01

... contactors employed in the separation cascade can be liquid-liquid exchange columns (such as pulsed columns.... Plastic, plastic-lined (including use of fluorocarbon polymers) and/or glass-lined columns and piping are therefore used. (1) Liquid-liquid exchange columns. Countercurrent liquid-liquid exchange columns having...

10 CFR Appendix E to Part 110 - Illustrative List of Chemical Exchange or Ion Exchange Enrichment Plant Equipment and Components...

Code of Federal Regulations, 2014 CFR

2014-01-01

... contactors employed in the separation cascade can be liquid-liquid exchange columns (such as pulsed columns.... Plastic, plastic-lined (including use of fluorocarbon polymers) and/or glass-lined columns and piping are therefore used. (1) Liquid-liquid exchange columns. Countercurrent liquid-liquid exchange columns having...

Hydrodynamics of a Multistage Wet Scrubber Incineration Conditions

ERIC Educational Resources Information Center

Said, M. M.; Manyele, S. V.; Raphael, M. L.

2012-01-01

The objective of the study was to determine the hydrodynamics of the two stage counter-current cascade wet scrubbers used during incineration of medical waste. The dependence of the hydrodynamics on two main variables was studied: Inlet air flow rate and inlet liquid flow rate. This study introduces a new wet scrubber operating features, which are…

Silicon production process evaluations

NASA Technical Reports Server (NTRS)

1982-01-01

Chemical engineering analyses involving the preliminary process design of a plant (1,000 metric tons/year capacity) to produce silicon via the technology under consideration were accomplished. Major activities in the chemical engineering analyses included base case conditions, reaction chemistry, process flowsheet, material balance, energy balance, property data, equipment design, major equipment list, production labor and forward for economic analysis. The process design package provided detailed data for raw materials, utilities, major process equipment and production labor requirements necessary for polysilicon production in each process.

DESIGN CRITERIA FOR FUEL DISSOLUTION SYSTEMS AND ASSOCIATED SERVICE FACILITIES. PLANT MODIFICATIONS FOR REPROCESSING NON-PRODUCTION REACTOR FUELS. PROJECT CGC-830

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

Bierman, S.R.; Graf, W.A.; Kass, M.

1960-07-29

Design panameters are presented for phases of the facility to reprocess low-enrichment fuels from nonproduction reactors. Included are plant flowsheets and equipment layouts for fuel element dissolution, centrifugation, solution adjustment, and waste handling. Also included are the basic design criteria for the supporting facilities which service these phases and all other facilites located in the vicinity of the selected building (Bldg. 221-U). (J.R.D.)

Mercury Phase II Study - Mercury Behavior across the High-Level Waste Evaporator System

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

Bannochie, C. J.; Crawford, C. L.; Jackson, D. G.

2016-06-17

The Mercury Program team’s effort continues to develop more fundamental information concerning mercury behavior across the liquid waste facilities and unit operations. Previously, the team examined the mercury chemistry across salt processing, including the Actinide Removal Process/Modular Caustic Side Solvent Extraction Unit (ARP/MCU), and the Defense Waste Processing Facility (DWPF) flowsheets. This report documents the data and understanding of mercury across the high level waste 2H and 3H evaporator systems.

DISPOSAL OF LIQUID WASTE IN THE DURANGO-TYPE URANIUM MILLING FLOWSHEET

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

Tame, K.E.; Valdez, E.G.; Rosenbaum, J.B.

1961-01-01

Possible modifications were studied in conventional uraniuum ore- processing steps to confine and permit controlled disposal of radioactive wastes. Surveys of Ra/sup 226/ contamination of liquid wastes from uranium mills indicated that the Vanadium Corporation of America plant at Durango, Colo., had one of the more urgent problems. A possible procedure for minimizing the waste disposal problem was to reuse the waste solution in the mill-in effect, erasing the need for disposal of liquid waste. In examining this possibility, interlocked bench-scale leaching and solvent extraction tests simulating the Durango fiowsheet were made. The simulated reuse of barren raffinate for leachingmore » and washing was carried through three separate campaigns of 9, 12, and 35 cycles each. An attempt to expedite the test work by using agitation leaching during the first campaign resulted in pregnant solutions of varying turbidity, giving a discordant pattern of radioactivity analyses. Percolation leaching and washing patterned more nearly after the Durango flowsheet was used in the second and third campaigns and consistently gave solutions of satisfactory clarity. The radioactivity was somewhat variable but did not build up with prolonged recycling of the raffinate. The buildup of other impurities in the pregnant solution had little noticeabIe effect on the operation of the percolation leach column. Operational difficulties from slow phase disengagement and entrainment in the solvent extraction stripping and scrubbing units occurred during the first two campaigns. In the third campaign slow phase disengagement and aqueous entrainment in the strippers were practically eliminated by heating the last stage to about 40 deg C and operating with the aqueous phase continuous. Increased mixing time in the scrubbing section was successful in reducing entrainment of aqueous in the organic from the settlers. Also, the concentrations of active reagents in the solvent extraction system were increased during the third campaign to correspond to an increase made at the Durango plant. The recovery of uranium and vanadium from the acid leach solution was excellent, averaging 99.7 and 95.6%, respectively. During the test work the Durango plant made several changes in tailing disposal procedures to minimize the waste problem. The most important comprised impounding all barren raffinate in two large lagoons. This was a successful temporary solution to the problem. However, as evaporation is relied upon to eliminate the water, it is estimated that 40 acres of area will be needed. The use of barren raffinate for washing in the Durango process would greatly diminish the quantity of solution to be disposed of by solar evaporation and the conjunctive need for a large disposal area. (auth)« less

Pilot-Scale Test of Counter-Current Ion Exchange (CCIX) Using UOP IONSIV IE-911

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

Wester, Dennis W; Leugemors, Robert K; Taylor, Paul W

2001-09-24

A pilot-scale test of a moving-bed configuration of a UOP IONSIV? IE-911 ion-exchange column was performed over 17 days at Severn Trent Services facilities. The objectives of the test, in order of priority, were to determine if aluminosilicate precipitation caused clumping of IE-911 particles in the column, to observe the effect on aluminum-hydroxide precipitation of water added to a simulant-filled column, to evaluate the extent of particle attrition, and to measure the expansion of the mass-transfer zone under the influence of column pulsing. The IE-911 moved through the column with no apparent clumping during the test, although analytical results indicatemore » that little if any aluminosilicate precipitated onto the particles. A precipitate of aluminum hydroxide was not produced when water was added to the simulant-filled column, indicating that this upset scenario is probably of little concern. Particle-size distributions remained relatively constant with time and position in the column, indicating that particle attrition was not significant. The expansion of the mass-transfer zone could not be accurately measured because of the slow loading kinetics of the IE-911 and the short duration of the test; however, the information obtained indicates that back-mixing of sorbent is not extensive.« less

Summer Study Program in Geophysical Fluid Dynamics, The Woods Hole Oceanographic Institution. Baroclinic Instability and Ocean Fronts.

DTIC Science & Technology

1983-11-01

spectrum of the linear stability theory has multiple roots with zero real parts. Then the general forms of the amplitude equations may be found for given...76 Dynamical Generation of Eastern Boundary Currents George eronis. .......................... 77 ..Amplitude Equations Edward...Associated Countercurrent. Benoit Cushman-Roisin ....... .................... ... 103 Turbulently Generated Eastern Boundary Currents Roger L. Hughes

Supercritical Fluid Fractionation of JP-8

DTIC Science & Technology

1991-12-26

applications, such as coffee decaffeination , spice extraction, and lipids purification. The processing principles have also long been well known and ipracticed...PRINCIPLES OF SUPERCRITICAL FLUID EXTRACTION 8 A. Background on Supercritical Fluid Solubility 8 B. Supercritical Fluid Extraction Process ...Operation I0 1. Batch Extraction of Solid Materials 10 2. Counter-Current Continuous SCF Processing of Liquid 15 Products 3. Supercritical Fluid Extraction vs

Recovery of Butanol by Counter-Current Carbon Dioxide Fractionation with its Potential Application to Butanol Fermentation

PubMed Central

Solana, Miriam; Qureshi, Nasib; Bertucco, Alberto; Eller, Fred

2016-01-01

A counter-current CO2 fractionation method was applied as a mean to recover n-butanol and other compounds that are typically obtained from biobutanol fermentation broth from aqueous solutions. The influence of operating variables, such as solvent-to-feed ratio, temperature, pressure and feed solution composition was experimentally studied in terms of separation efficiency, butanol removal rate, total removal and butanol concentration in the extract at the end of the continuous cycle. With respect to the temperature and pressure conditions investigated, results show that the highest separation efficiency was obtained at 35 °C and 10.34 MPa. At these operating conditions, 92.3% of the butanol present in the feed solution was extracted, and a concentration of 787.5 g·L−1 of butanol in the extract was obtained, starting from a feed solution of 20 g·L−1. Selectivity was calculated from experimental data, concluding that our column performs much better than a single equilibrium stage. When adding ethanol and acetone to the feed solution, ethanol was detected in the water-rich fraction (raffinate), whereas the highest concentration of acetone was found in the butanol rich fraction (extract). PMID:28773654

Separation of polyphenols from leaves of Malus hupehensis (Pamp.) Rehder by off-line two-dimensional High Speed Counter-Current Chromatography combined with recycling elution mode.

PubMed

Liu, Qi; Zeng, Hualiang; Jiang, Shujing; Zhang, Li; Yang, Fuzhu; Chen, Xiaoqing; Yang, Hua

2015-11-01

In this study, off-line two-dimensional High Speed Counter-Current Chromatography (2D HSCCC) strategy combined with recycling elution mode was developed to isolate compounds from the ethyl acetate extract of a common green tea--leaves of Malus hupehensis (Pamp.) Rehder. In the orthogonal separation system, a conventional HSCCC was employed for the first dimension and two recycling HSCCCs were used for the second in parallel. Using a solvent system consisting of n-hexane-ethyl acetate-methanol-water (1:4:0.6:4.4, v/v) in the first and second dimension, four compounds including 3-hydroxy-phlorizin (1), phloretin (2), avicularin (3) and kaempferol 3-O-β-D-glucoside (4) were obtained. The purities of these four compounds were all over 95.0% as determined by HPLC. And their structures were all identified through UV, MS and (1)H NMR. It has been demonstrated that the combination of off-line 2D HSCCC with recycling elution mode is an efficient technique to isolate compounds with similar polarities in natural products. Copyright © 2014 Elsevier Ltd. All rights reserved.

Continuous counter-current chromatography for capture and polishing steps in biopharmaceutical production.

PubMed

Steinebach, Fabian; Müller-Späth, Thomas; Morbidelli, Massimo

2016-09-01

The economic advantages of continuous processing of biopharmaceuticals, which include smaller equipment and faster, efficient processes, have increased interest in this technology over the past decade. Continuous processes can also improve quality assurance and enable greater controllability, consistent with the quality initiatives of the FDA. Here, we discuss different continuous multi-column chromatography processes. Differences in the capture and polishing steps result in two different types of continuous processes that employ counter-current column movement. Continuous-capture processes are associated with increased productivity per cycle and decreased buffer consumption, whereas the typical purity-yield trade-off of classical batch chromatography can be surmounted by continuous processes for polishing applications. In the context of continuous manufacturing, different but complementary chromatographic columns or devices are typically combined to improve overall process performance and avoid unnecessary product storage. In the following, these various processes, their performances compared with batch processing and resulting product quality are discussed based on a review of the literature. Based on various examples of applications, primarily monoclonal antibody production processes, conclusions are drawn about the future of these continuous-manufacturing technologies. Copyright © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Preparative isolation and purification of lignans from Justicia procumbens using high-speed counter-current chromatography in stepwise elution mode.

PubMed

Zhou, Peijuan; Luo, Qijun; Ding, Lijian; Fang, Fang; Yuan, Ye; Chen, Juanjuan; Zhang, Jinrong; Jin, Haixiao; He, Shan

2015-04-20

Lignans, which are recognized as main constituents in Justicia procumbens, have attracted considerable attention due to their pharmacological activities, including antitumor, anti-hepatitic, cytotoxic, anti-microbial, and anti-virus properties. Preparative high-speed counter-current chromatography (HSCCC) was successfully applied to the isolation and purification of four lignans (justicidin B (1), justicidin A (2), 6'-hydroxyjusticidin C (3) and lignan J1 (4)) from J. procumbens using stepwise elution with a pair of two-phase solvent systems composed of n-hexane-ethyl acetate-methanol-water at (1.3:1:1.3:1, v/v) and (2.5:1:2.5:1, v/v). The preparative HSCCC separation was performed on 300 mg of crude sample yielding compounds 1 (19.7 mg), 2 (9.86 mg), 3 (11.26 mg), and 4 (2.54 mg) in a one-step separation, with purities over 95% as determined by HPLC. The structures of these compounds were identified by MS, 1H-NMR and 13C-NMR. This is the first report on the application of HSCCC to the efficient separation of lignans from J. procumbens.

Isolation and purification of macrocyclic components from Penicillium fermentation broth by high-speed counter-current chromatography.

PubMed

Gao, Xiang; Zhuang, Rongqiang; Guo, Jiannan; Bao, Jian; Fang, Meijuan; Liu, Yan; Xu, Pengxiang; Zhao, Yufen

2010-02-01

In this paper, high-speed counter-current chromatography (HSCCC), assisted with ESI-MS, was first successfully applied to the preparative separation of three macrolide antibiotics, brefeldin A (12.6 mg, 99.0%), 7'-O-formylbrefeldin A (6.5 mg, 95.0%) and 7'-O-acetylbrefeldin A (5.0 mg, 92.3%) from the crude extract of the microbe Penicillium SHZK-15. Considering the chemical nature and partition coefficient (K) values of the three target compounds, a two-step HSCCC isolation protocol was developed in order to obtain products with high purity. In the two-step method, the crude ethyl acetate extract was first fractionated and resulted in two peak fractions by HSCCC using solvent system n-hexane/ethyl acetate/methanol/water (HEMWat) (3:7:5:5 v/v/v/v), then purified using solvent systems HEMWat (3:5:3:5 v/v/v/v) and HEMWat (7:3:5:5 v/v/v/v) for each fraction. The purities and structures of the isolated compounds were determined by HPLC, X-ray crystallography, ESI-MS and NMR. The results demonstrated that HSCCC is a fast and efficient technique for systematic isolation of bioactive compounds from the microbes.

Enhancement of Condensation Heat Transfer by Counter-Corrent Wavy Flow in a Vertical Tube

NASA Astrophysics Data System (ADS)

Teranishi, Tsunenobu; Ozawa, Takanori; Takimoto, Akira

As a basic research for the development of a high-performance and environment-friendly thermal energy recovery system, detailed experiments have been conducted to investigate the mechanism of the enhancement of condensation heat transfer by the counter-current moist air flow in a vertical tube. From the results of visual observation of the phenomena by using a high-speed video recorder and the measurement of condensate rate respectively from an upper and a bottom end of a cooled tube, in which various humidity vapor of air and water flowed upward or downward, the dynamic behavior of liquid film condensed on cooled surface and moist air flow was classified into four distinctive patterns in quality and quantity. Further, the effect of the scale and the operating condition such as the diameter and the length of tube, the vapor concentration and the moist air temperature, on the condensation rate of counter-current wavy flow was clarified in relation to the pattern and condition of occurrence of the wavy flow of liquid film and flooding due to the shear forces between the interface of liquid and moist air flow.

Separation and preparation of xanthochymol and guttiferone E by high performance liquid chromatography and high speed counter-current chromatography combined with silver nitrate coordination reaction.

PubMed

Li, Jun; Gao, Ruixi; Zhao, Dan; Huang, Xianju; Chen, Yu; Gan, Fei; Liu, Hui; Yang, Guangzhong

2017-08-18

Xanthochymol (XCM) and guttiferone E (GFE), a pair of π bond benzophenone isomers from Garcinia xanthochymus, were once reported to be difficult or impossible to separate. The present study reports the successful separation of these two isomers through high performance liquid chromatography (HPLC), as well as their effective isolation using high speed counter-current chromatography (HSCCC) based on the silver nitrate (AgNO 3 ) coordination reaction. First, an effective HPLC separation system was developed, achieving a successful baseline separation with resolution of 2.0. Based on the partition coefficient (K) resolved by HPLC, the two-phase solvent system was determined as n-hexane, methanol and water with the uncommon volume ratio of 4:6:1. A crude extract of Garcinia xanthochymus (0.2g) was purified by normal HSCCC and refined with AgNO 3 -HSCCC. Monomers of XCM and GFE were identified by HPLC, mass spectrometry (MS) and nuclear magnetic resonance (NMR). The results demonstrate the separation and isolation of π bond benzophenone isomers using ordinary octadecyl silane (C 18 ) columns and HSCCC. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparative separation of sulfur-containing diketopiperazines from marine fungus Cladosporium sp. using high-speed counter-current chromatography in stepwise elution mode.

PubMed

Gu, Binbin; Zhang, Yanying; Ding, Lijian; He, Shan; Wu, Bin; Dong, Junde; Zhu, Peng; Chen, Juanjuan; Zhang, Jinrong; Yan, Xiaojun

2015-01-09

High-speed counter-current chromatography (HSCCC) was successively applied to the separation of three sulfur-containing diketopiperazines (DKPs) (including two new compounds cladosporin A (1) and cladosporin B (3), and a known compound haematocin (2)) from a marine fungus Cladosporium sp. The two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water at (1:1:1:1, v/v) and (2:1:2:1, v/v), in stepwise elution mode, was used for HSCCC. The preparative HSCCC separation was performed on 300 mg of crude sample yielding 26.7 mg of compound 3 at a purity of over 95%, 53.6 mg of a mixture of compounds 1 and 2, which was further separated by preparative-HPLC yielding 14.3 mg of compound 1 and 25.4 mg of compound 2 each at a purity of over 95%. Their structures were established by spectroscopic methods. The sulfur-containing DKPs suppressed the proliferation of hepatocellular carcinoma cell line HepG2. The present work represents the first application of HSCCC in the efficient preparation of marine fungal natural products.

Preparative Separation of Sulfur-Containing Diketopiperazines from Marine Fungus Cladosporium sp. Using High-Speed Counter-Current Chromatography in Stepwise Elution Mode

PubMed Central

Gu, Binbin; Zhang, Yanying; Ding, Lijian; He, Shan; Wu, Bin; Dong, Junde; Zhu, Peng; Chen, Juanjuan; Zhang, Jinrong; Yan, Xiaojun

2015-01-01

High-speed counter-current chromatography (HSCCC) was successively applied to the separation of three sulfur-containing diketopiperazines (DKPs) (including two new compounds cladosporin A (1) and cladosporin B (3), and a known compound haematocin (2)) from a marine fungus Cladosporium sp. The two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water at (1:1:1:1, v/v) and (2:1:2:1, v/v), in stepwise elution mode, was used for HSCCC. The preparative HSCCC separation was performed on 300 mg of crude sample yielding 26.7 mg of compound 3 at a purity of over 95%, 53.6 mg of a mixture of compounds 1 and 2, which was further separated by preparative-HPLC yielding 14.3 mg of compound 1 and 25.4 mg of compound 2 each at a purity of over 95%. Their structures were established by spectroscopic methods. The sulfur-containing DKPs suppressed the proliferation of hepatocellular carcinoma cell line HepG2. The present work represents the first application of HSCCC in the efficient preparation of marine fungal natural products. PMID:25584683

Separation and Purification of Ombuoside from Gynostemma Pentaphyllum by Microwave-Assisted Extraction Coupled with High-Speed Counter-current Chromatography.

PubMed

Jiang, Wenhui; Shan, Hu; Song, Jiying; Lü, Haitao

2017-01-01

A rapid and efficient method for the separation and purification of ombuoside from Gynostemma pentaphyllum by microwave-assisted extraction coupled with high-speed counter-current chromatography (HSCCC) was successfully developed. Using an orthogonal array design L 9 (3 4 ), the extraction conditions, including microwave power, irradiation time, solid-to-liquid ratio and extraction times, were optimized. Ombuoside was isolated and purified from the crude extraction by HSCCC with two-phase solvent system composed of n-hexane:ethyl acetate:ethanol:water (5:6:5:5, v/v) in a single run. A 210 mg quantity of the crude extract containing 2.16% ombuoside was loaded, yielding 3.9 mg of ombuoside at 96.7% purity. The chemical structure of ombuoside was determined by comparison with the high-performance liquid chromatography retention time of standard substance as well as UV, FT-IR, ESI-MS, 1 H NMR and 13 C NMR spectra. The purified ombuoside had strong 1,1-diphenyl-2-picrylhydrazyl and hydroxyl free radical scavenging activities. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

PREPARATIVE ISOLATION AND PURIFICATION OF THREE GLYCINE-CONJUGATED CHOLIC ACIDS FROM PULVIS FELLIS SUIS BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY COUPLED WITH ELSD DETECTION.

PubMed

He, Jiao; Li, Jing; Sun, Wenji; Zhang, Tianyou; Ito, Yoichiro

2012-01-01

Coupled with evaporative light scattering detection, a high-speed counter-current chromatography (HSCCC) method was developed for preparative isolation and purification of three glycine-conjugated cholic acids, glycochenodeoxycholic acid (GCDCA), glycohyodeoxycholic acid (GHDCA) and glycohyocholic acid (GHCA) from Pulvis Fellis Suis (Pig gallbladder bile) for the first time. The separation was performed with a two-phase solvent system consisted of chloroform-methanol-water-acetic acid (65:30:10:1.5, v/v/v/v) by eluting the lower phase in the head-to-tail elution mode. The revolution speed of the separation column, flow rate of the mobile phase and separation temperature were 800 rpm, 2 ml/min and 25 °C, respectively. In a single operation, 33 mg of GCDCA, 38 mg of GHDCA and 23 mg of GHCA were obtained from 200 mg of crude extract with the purity of 95.65%, 96.72% and 96.63%, respectively, in one step separation. The HSCCC fractions were analyzed by high-performance liquid chromatography (HPLC) and the structures of the three glycine-conjugated cholic acids were identified by ESI-MS, (1)H NMR and (13)C NMR.

Preparative separation of capsaicin and dihydrocapsaicin from Capsicum frutescens by high-speed counter-current chromatography.

PubMed

Peng, Aihua; Ye, Haoyu; Li, Xia; Chen, Lijuan

2009-09-01

Capsaicin and dihydrocapsaicin are two main bioactive components of Capsicum frutescens and are widely used as food additives and drugs in China and India. Due to their similarity in structures, isolation of capsaicin and dihydrocapsaicin with traditional methods such as silica gel column chromatography, normal-phase thin-layer chromatography (TLC) becomes difficult. This study involves separating capsaicin and dihydrocapsaicin with sufficient purity and recovery using high-speed counter-current chromatography (HSCCC) with a solvent system composed of n-hexane-ethyl acetate-methanol-water-acetic acid (20:20:20:20:2, v/v/v/v/v). Separation parameters such as sample volume, and sample concentration were first optimized on analytical HSCCC, and then scaled up to preparative HSCCC. 0.65 g capsaicin and 0.28 g dihydrocapsaicin were obtained from 1.2 g crude extract and their purities were 98.5 and 97.8%, respectively. The recoveries of the two compounds were 86.3 and 85.4%, respectively. The purity of the isolated compounds was analyzed by high-performance liquid chromatography (HPLC) and their structures were identified by (1)H nuclear magnetic resonance (NMR) and (13)C NMR analysis.

Interstitial hyperthermia treatment of countercurrent vascular tissue: a comparison of Pennes, WJ and porous media bioheat models.

PubMed

Hassanpour, Saied; Saboonchi, Ahmad

2014-12-01

Development of appropriate heat transfer models to investigate the thermal behavior of living tissues has become increasingly important in simulations of cancer hyperthermia. In this paper, a review is initially presented of the more important general models developed for heat transfer description of perfused tissues. Comparisons are then made between Pennes' simplified Weinbaum and Jiji "WJ" and the more recent porous media "PM" bioheat models. For this purpose, a mathematical model is developed for the heat transfer in a cylindrical medium containing parallel counter-current pairs of small vessels with characteristics as much as possible similar to those of living tissues. The validity of the models is examined and confirmed using the Pennes in vivo experiments and one-dimensional analytical solutions. For consideration of interstitial hyperthermia treatment the smaller cylindrical zone with typical heat generation, is assumed in the center of the main cylinder. The numerical simulation results revealed that, despite difference in temperature distributions calculated by these three models at normal condition, the heat affected zone at hyperthermic condition predicted by all three models are similar. Copyright © 2014 Elsevier Ltd. All rights reserved.

Preparative isolation of alkaloids from Corydalis bungeana Turcz. by high-speed counter-current chromatography using stepwise elution

PubMed Central

Niu, Lili; Xie, Zhensheng; Cai, Tanxi; Wu, Peng; Xue, Peng; Chen, Xiulan; Wu, Zhiyong; Ito, Yoichiro; Li, Famei; Yang, Fuquan

2011-01-01

High-speed counter-current chromatography (HSCCC) was successfully applied for the preparative separation and purification of alkaloids from Corydalis bungeana Turcz. (Kudiding in Chinese) for the first time. After the measurement of partition coefficient of seven target alkaloids in the nine two-phase solvent systems composed of CHCl3–MeOH–(0.1 M; 0.2 M; 0.3 M) HCl (4:1.5:2; 4:2:2; 4:3:2, v/v), CHCl3–MeOH–0.2 M HCl (4:2:2, v/v) and CHCl3–MeOH–0.3 M HCl (4:3:2, v/v) were finally selected for the HSCCC separation using the first upper phase as the stationary phase and the stepwise elution of the two lower mobile phases. Consequently, sanguinarine (10 mg), corynoline (25 mg), protopine (20 mg), corynoloxine (18 mg), and 12-hydroxycorynoline (8 mg) were obtained from 200 mg of crude alkaloid extracts with purities of 94–99% as determined by HPLC. Their chemical structures were characterized on the basis of 1H-NMR, 13C-NMR, and LC-ESI-Q-TOF-MS/MS analyses. PMID:21387560

Preparative isolation of alkaloids from Dactylicapnos scandens using pH-zone-refining counter-current chromatography by changing the length of the separation column.

PubMed

Wang, Xiao; Dong, Hongjing; Yang, Bin; Liu, Dahui; Duan, Wenjuan; Huang, Luqi

2011-12-01

pH-Zone-refining counter-current chromatography was successfully applied for the preparative separation of alkaloids from Dactylicapnos scandens. The two-phase solvent system was composed of petroleum ether-ethyl acetate-methanol-water (3:7:1:9, v/v), where 20 mM of triethylamine (TEA) was added to the upper phase as a retainer and 5 mM of hydrochloric acid (HCl) to the aqueous phase as an eluter. In this experiment, the apparatus with an adjustable length of the separation column was used for the separation of alkaloids from D. scandens and the resolution of the compounds can be remarkably improved by increasing the length of the separation column. As a result, 70 mg protopin, 30 mg (+) corydine, 120 mg (+) isocorydine and 40 mg (+) glaucine were obtained from 1.0 g of the crude extracts and each with 99.2%, 96.5%, 99.3%, 99.5% purity as determined by HPLC. The chemical structures of these compounds were confirmed by positive ESI-MS and (1)H NMR. Copyright © 2011 Elsevier B.V. All rights reserved.

Creating Economic Incentives for Waste Disposal in Developing Countries Using the MixAlco Process.

PubMed

Lonkar, Sagar; Fu, Zhihong; Wales, Melinda; Holtzapple, Mark

2017-01-01

In rapidly growing developing countries, waste disposal is a major challenge. Current waste disposal methods (e.g., landfills and sewage treatment) incur costs and often are not employed; thus, wastes accumulate in the environment. To address this challenge, it is advantageous to create economic incentives to collect and process wastes. One approach is the MixAlco process, which uses methane-inhibited anaerobic fermentation to convert waste biomass into carboxylate salts, which are chemically converted to industrial chemicals and fuels. In this paper, humanure (raw human feces and urine) is explored as a possible nutrient source for fermentation. This work focuses on fermenting municipal solid waste (energy source) and humanure (nutrient source) in batch fermentations. Using the Continuum Particle Distribution Model (CPDM), the performance of continuous countercurrent fermentation was predicted at different volatile solid loading rates (VSLR) and liquid residence times (LRT). For a four-stage countercurrent fermentation system at VSLR = 4 g/(L∙day), LRT = 30 days, and solids concentration = 100 g/L liquid, the model predicts carboxylic acid concentration of 68 g/L and conversion of 78.5 %.

Mass transfer in thin films under counter-current gas: experiments and numerical study

NASA Astrophysics Data System (ADS)

Lucquiaud, Mathieu; Lavalle, Gianluca; Schmidt, Patrick; Ausner, Ilja; Wehrli, Marc; O Naraigh, Lennon; Valluri, Prashant

2016-11-01

Mass transfer in liquid-gas stratified flows is strongly affected by the waviness of the interface. For reactive flows, the chemical reactions occurring at the liquid-gas interface also influence the mass transfer rate. This is encountered in several technological applications, such as absorption units for carbon capture. We investigate the absorption rate of carbon dioxide in a liquid solution. The experimental set-up consists of a vertical channel where a falling film is sheared by a counter-current gas flow. We measure the absorption occurring at different flow conditions, by changing the liquid solution, the liquid flow rate and the gas composition. With the aim to support the experimental results with numerical simulations, we implement in our level-set flow solver a novel module for mass transfer taking into account a variant of the ghost-fluid formalism. We firstly validate the pure mass transfer case with and without hydrodynamics by comparing the species concentration in the bulk flow to the analytical solution. In a final stage, we analyse the absorption rate in reactive flows, and try to reproduce the experimental results by means of numerical simulations to explore the active role of the waves at the interface.

Investigation of nutrient feeding strategies in a countercurrent mixed-acid multi-staged fermentation: development of segregated-nitrogen model.

PubMed

Smith, Aaron D; Holtzapple, Mark T

2010-12-01

The MixAlco process is a biorefinery based on the production of carboxylic acids via mixed-culture fermentation. Nitrogen is essential for microbial growth and metabolism, and may exist in soluble (e.g., ammonia) or insoluble forms (e.g., cells). Understanding the dynamics of nitrogen flow in a countercurrent fermentation is necessary to develop control strategies to maximize performance. To estimate nitrogen concentration profiles in a four-stage fermentation train, a mass balance-based segregated-nitrogen model was developed, which uses separate balances for solid- and liquid-phase nitrogen with nitrogen reaction flux between phases assumed to be zero. Comparison of predictions with measured nitrogen profiles from five trains, each with a different nutrient contacting pattern, shows the segregated-nitrogen model captures basic behavior and is a reasonable tool for estimating nitrogen profiles. The segregated-nitrogen model may be used to (1) estimate optimal nitrogen loading patterns, (2) develop a reaction-based model, (3) understand influence of model inputs (e.g., operating parameters, feedstock properties, nutrient loading pattern) on the steady-state nitrogen profile, and (4) determine the direction of the nitrogen reaction flux between liquid and solid phases. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

PREPARATIVE ISOLATION AND PURIFICATION OF THREE GLYCINE-CONJUGATED CHOLIC ACIDS FROM PULVIS FELLIS SUIS BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY COUPLED WITH ELSD DETECTION

PubMed Central

He, Jiao; Li, Jing; Sun, Wenji; Zhang, Tianyou; Ito, Yoichiro

2011-01-01

Coupled with evaporative light scattering detection, a high-speed counter-current chromatography (HSCCC) method was developed for preparative isolation and purification of three glycine-conjugated cholic acids, glycochenodeoxycholic acid (GCDCA), glycohyodeoxycholic acid (GHDCA) and glycohyocholic acid (GHCA) from Pulvis Fellis Suis (Pig gallbladder bile) for the first time. The separation was performed with a two-phase solvent system consisted of chloroform-methanol-water-acetic acid (65:30:10:1.5, v/v/v/v) by eluting the lower phase in the head-to-tail elution mode. The revolution speed of the separation column, flow rate of the mobile phase and separation temperature were 800 rpm, 2 ml/min and 25 °C, respectively. In a single operation, 33 mg of GCDCA, 38 mg of GHDCA and 23 mg of GHCA were obtained from 200 mg of crude extract with the purity of 95.65%, 96.72% and 96.63%, respectively, in one step separation. The HSCCC fractions were analyzed by high-performance liquid chromatography (HPLC) and the structures of the three glycine-conjugated cholic acids were identified by ESI-MS, 1H NMR and 13C NMR. PMID:23008527

Vascular adaptations for heat conservation in the tail of Florida manatees (Trichechus manatus latirostris)

PubMed Central

Rommel, Sentiel A; Caplan, Heather

2003-01-01

Although Florida manatees (Trichechus manatus latirostris) have relatively low basal metabolic rates for aquatic mammals of their size, they maintain normal mammalian core temperatures. We describe vascular structures in the manatee tail that permit countercurrent heat exchange (CCHE) to conserve thermal energy. Approximately 1000 arteries juxtaposed to 2000 veins are found at the cranial end of the caudal vascular bundle (CVB); these numbers decrease caudally, but the 1 : 2 ratio of arteries to veins persists. Arterial walls are relatively thin when compared to those previously described in vascular countercurrent heat exchangers in cetaceans. It is assumed that CCHE in the CVB helps manatees to maintain core temperatures. Activity in warm water, however, mandates a mechanism that prevents elevated core temperatures. The tail could transfer heat to the environment if arterial blood delivered to the skin were warmer than the surrounding water; unfortunately, CCHE prevents this heat transfer. We describe deep caudal veins that provide a collateral venous return from the tail. This return, which is physically outside the CVB, reduces the venous volume within the bundle and allows arterial expansion and increased arterial supply to the skin, and thus helps prevent elevated core temperatures. PMID:12739612

Vascular adaptations for heat conservation in the tail of Florida manatees (Trichechus manatus latirostris).

PubMed

Rommel, Sentiel A; Caplan, Heather

2003-04-01

Although Florida manatees (Trichechus manatus latirostris) have relatively low basal metabolic rates for aquatic mammals of their size, they maintain normal mammalian core temperatures. We describe vascular structures in the manatee tail that permit countercurrent heat exchange (CCHE) to conserve thermal energy. Approximately 1000 arteries juxtaposed to 2000 veins are found at the cranial end of the caudal vascular bundle (CVB); these numbers decrease caudally, but the 1:2 ratio of arteries to veins persists. Arterial walls are relatively thin when compared to those previously described in vascular countercurrent heat exchangers in cetaceans. It is assumed that CCHE in the CVB helps manatees to maintain core temperatures. Activity in warm water, however, mandates a mechanism that prevents elevated core temperatures. The tail could transfer heat to the environment if arterial blood delivered to the skin were warmer than the surrounding water; unfortunately, CCHE prevents this heat transfer. We describe deep caudal veins that provide a collateral venous return from the tail. This return, which is physically outside the CVB, reduces the venous volume within the bundle and allows arterial expansion and increased arterial supply to the skin, and thus helps prevent elevated core temperatures.

Analytical separation of tea catechins and food-related polyphenols by high-speed counter-current chromatography.

PubMed

Yanagida, Akio; Shoji, Atsushi; Shibusawa, Yoichi; Shindo, Heisaburo; Tagashira, Motoyuki; Ikeda, Mitsuo; Ito, Yoichiro

2006-04-21

High-speed counter-current chromatography (HSCCC) using the type-J coil planet centrifuge was applied to compositional analysis of tea catechins and separation of other food-related polyphenols. The HSCCC separation of nine different standard compounds and those from extracts of commercial tea leaves was performed with a two-phase solvent system composed of tert-butyl methyl ether-acetonitrile-0.1% aqueous trifluoroacetic acid (TFA) (2:2:3, v/v/v) by eluting the upper organic phase at a flow rate of 2 ml/min. The main compounds in the extract of non-fermented green tea were found to be monomeric catechins, their galloylated esters and caffeine. In addition to these compounds, oxidized pigments, such as hydrophobic theaflavins (TFs) and polar thearubigins (TRs) were also separated and detected from the extracts of semi-fermented oolong tea and fermented black tea. Furthermore, several food-related polyphenols, such as condensed catechin oligomers (procyanidins), phenolic acids and flavonol glycosides were clearly separated under the same HSCCC condition. These separation profiles of HSCCC provide useful information about the hydrophobic diversity of these bioactive polyphenols present in various types of teas and food products.

High-speed countercurrent chromatographic recovery and off-line electrospray ionization mass spectrometry profiling of bisdesmodic saponins from Saponaria officinalis possessing synergistic toxicity enhancing properties on targeted antitumor toxins.

PubMed

Thakur, Mayank; Jerz, Gerold; Tuwalska, Dorota; Gilabert-Oriol, Roger; Wybraniec, Sławomir; Winterhalter, Peter; Fuchs, Hendrik; Weng, Alexander

2014-04-01

Saponaria officinalis L. (Caryophyllaceae), also known as fuller's herb or soapwort is a medicinal plant, which grows from Europe to Central Asia. Medicinal properties attributed to this plant include its antitussive and galactogogue properties. Recently, bisdesmodic saponins with very specific structural features from S. officinalis have been shown to strongly enhance the efficacy of specific targeted toxins (anti-tumor antibodies connected to protein toxins) in-vitro and in-vivo in a synergistic manner. In the presently reported novel approach we used preparative all-liquid high-speed countercurrent chromatography (HSCCC) to recover a total of 22 fractions using biphasic solvent system tert-butylmethylether/n-butanol/acetonitrile/water 1:3:1:5 (v/v/v/v) from a complex precipitated crude saponin mixture. Out of these 22 fractions, 3 fractions had the enhancer effect on anti-tumor toxins out of which one fraction (F7) was further tested elaborately in different cell lines. The molecular weight distribution and compound profiles of separated saponins were monitored by off-line injections of the sequentially collected fractions to an electrospray ion-trap mass-spectrometry system (ESI-IT-MS). The functional saponin fractions were mainly bisdesmosidc and contained saponin m/z 1861 amongst other. Using the bio-assay guided monitoring, the highly active fractions containing 2 to 3 bisdesmodic saponins (5μg/mL) were screened for their effectiveness in enhancing the anti-tumor activity of targeted toxin Sap3-EGF, which was determined using the impedance based real-time cell cytotoxicity evaluation. This novel combination of HSCCC fractionation, MS-target-guided profiling procedure and bio-assay guided fractionation yielded 100mg of functional saponins from a 60g crude drug powder in a rapid and convenient manner. Copyright © 2014 Elsevier B.V. All rights reserved.

Separation of polar betalain pigments from cacti fruits of Hylocereus polyrhizus by ion-pair high-speed countercurrent chromatography.

PubMed

Wybraniec, Sławomir; Stalica, Paweł; Jerz, Gerold; Klose, Bettina; Gebers, Nadine; Winterhalter, Peter; Spórna, Aneta; Szaleniec, Maciej; Mizrahi, Yosef

2009-10-09

Polar betacyanin pigments together with betaxanthins from ripe cactus fruits of Hylocereus polyrhizus (Cactaceae) were fractionated by means of preparative ion-pair high-speed countercurrent chromatography (IP-HSCCC) also using the elution-extrusion (EE) approach for a complete pigment recovery. HSCCC separations were operated in the classical 'head-to-tail' mode with an aqueous mobile phase. Different CCC solvent systems were evaluated in respect of influence and effectiveness of fractionation capabilities to separate the occurring pigment profile of H. polyrhizus. For that reason, the additions of two different volatile ion-pair forming perfluorinated carboxylic acids (PFCA) were investigated. For a direct comparison, five samples of Hylocereus pigment extract were run on preparative scale (900 mg) in 1-butanol-acetonitrile-aqueous TFA 0.7% (5:1:6, v/v/v) and the modified systems tert.-butyl methyl ether-1-butanol-acetonitrile-aqueous PFCA (2:2:1:5, v/v/v/v) using 0.7% and 1.0% trifluoroacetic acid (TFA) or heptafluorobutyric acid (HFBA) in the aqueous phase, respectively. The chemical affinity to the organic stationary CCC solvent phases and in consequence the retention of these highly polar betalain pigments was significantly increased by the use of the more lipophilic fluorinated ion-pair reagent HFBA instead of TFA. The HFBA additions separated more effectively the typical cacti pigments phyllocactin and hylocerenin from betanin as well as their iso-forms. Unfortunately, similar K(D) ratios and selectivity factors alpha around 1.0-1.1 in all tested solvent systems proved that the corresponding diastereomers, 15S-type pigments cannot be resolved from the 15R-epimers (iso-forms). Surprisingly, additions of the stronger ion-pair reagent (HFBA) resulted in a partial separation of hylocerenin from phyllocactin which were not resolved in the other solvent systems. The pigments were detected by means of HPLC-DAD and HPLC-electrospray ionization-MS using also authentic reference materials.

Validation of the kinetic-turbulent-neoclassical theory for edge intrinsic rotation in DIII-D

NASA Astrophysics Data System (ADS)

Ashourvan, Arash; Grierson, B. A.; Battaglia, D. J.; Haskey, S. R.; Stoltzfus-Dueck, T.

2018-05-01

In a recent kinetic model of edge main-ion (deuterium) toroidal velocity, intrinsic rotation results from neoclassical orbits in an inhomogeneous turbulent field [T. Stoltzfus-Dueck, Phys. Rev. Lett. 108, 065002 (2012)]. This model predicts a value for the toroidal velocity that is co-current for a typical inboard X-point plasma at the core-edge boundary (ρ ˜ 0.9). Using this model, the velocity prediction is tested on the DIII-D tokamak for a database of L-mode and H-mode plasmas with nominally low neutral beam torque, including both signs of plasma current. Values for the flux-surface-averaged main-ion rotation velocity in the database are obtained from the impurity carbon rotation by analytically calculating the main-ion—impurity neoclassical offset. The deuterium rotation obtained in this manner has been validated by direct main-ion measurements for a limited number of cases. Key theoretical parameters of ion temperature and turbulent scale length are varied across a wide range in an experimental database of discharges. Using a characteristic electron temperature scale length as a proxy for a turbulent scale length, the predicted main-ion rotation velocity has a general agreement with the experimental measurements for neutral beam injection (NBI) powers in the range PNBI < 4 MW. At higher NBI power, the experimental rotation is observed to saturate and even degrade compared to theory. TRANSP-NUBEAM simulations performed for the database show that for discharges with nominally balanced—but high powered—NBI, the net injected torque through the edge can exceed 1 Nm in the counter-current direction. The theory model has been extended to compute the rotation degradation from this counter-current NBI torque by solving a reduced momentum evolution equation for the edge and found the revised velocity prediction to be in agreement with experiment. Using the theory modeled—and now tested—velocity to predict the bulk plasma rotation opens up a path to more confidently projecting the confinement and stability in ITER.

Effect of extended and daily short-term starvation/shut-down events on the performance of a biofilter treating toluene vapors.

PubMed

Jiménez, Lucero; Arriaga, Sonia; Muñoz, Raúl; Aizpuru, Aitor

2017-12-01

Industrial emissions of Volatile Organic Compounds are usually discontinuous. To assess the impact of interruptions in pollutant supply on the performance of biological treatment systems, two identical biofilters previously operated under continuous toluene loadings were subjected for 110 days to extended (12, 24, 36, 48, 60, 72, 84 and 96 h) and for a week to daily (8 h on, 16 h off) toluene starvation/shutdown events. One biofilter was operated under complete shutdowns (both air and toluene supply were interrupted), while the other maintained the air supply under toluene starvation. The biofilter operated under complete shutdowns was able to withstand both the extended and daily pollutant interruptions, while starvation periods >24 h severely impacted the performance of the other biofilter, with a removal efficiency decrease from 97.7 ± 0.1% to 45.4 ± 6.7% at the end of the extended starvation periods. This deterioration was likely due to a reduction in liquid lixiviation (from a total volume of 2380 mL to 1800 mL) mediated by the countercurrent airflow during the starvation periods. The presence of air under toluene starvation also favored the accumulation of inactive biomass, thus increasing the pressure drop from 337 to 700 mm H 2 O.m -1 , while decreasing the wash out of acidic by-products with a significantly higher pH of leachates (Student paired t-test <0.05). This study confirmed the need to prevent the accumulation of inhibitory compounds produced during process perturbation in order to increase biofiltration robustness. Process operation with sufficient drainage in the packing material and the absence of countercurrent airflow are highly recommended during toluene deprivation periods. Copyright © 2017. Published by Elsevier Ltd.

An efficient and target-oriented sample enrichment method for preparative separation of minor alkaloids by pH-zone-refining counter-current chromatography.

PubMed

Feng, Rui-Hong; Hou, Jin-Jun; Zhang, Yi-Bei; Pan, Hui-Qin; Yang, Wenzhi; Qi, Peng; Yao, Shuai; Cai, Lu-Ying; Yang, Min; Jiang, Bao-Hong; Liu, Xuan; Wu, Wan-Ying; Guo, De-An

2015-08-28

An efficient and target-oriented sample enrichment method was established to increase the content of the minor alkaloids in crude extract by using the corresponding two-phase solvent system applied in pH-zone-refining counter-current chromatography. The enrichment and separation of seven minor indole alkaloids from Uncaria rhynchophylla (Miq.) Miq. ex Havil(UR) were selected as an example to show the advantage of this method. An optimized two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (3:7:1:9, v/v) was used in this study, where triethylamine (TEA) as the retainer and hydrochloric acid (HCl) as the eluter were added at the equimolar of 10mM. Crude alkaloids of UR dissolved in the corresponding upper phase (containing 10mM TEA) were extracted twice with lower phase (containing 10mM TEA) and lower phase (containing 10mM HCl), respectively, the second lower phase extract was subjected to pH-zone-refining CCC separation after alkalization and desalination. Finally, from 10g of crude alkaloids, 4g of refined alkaloids was obtained and the total content of seven target indole alkaloids was increased from 4.64% to 15.78%. Seven indole alkaloids, including 54mg isocorynoxeine, 21mg corynoxeine, 46mg isorhynchophylline, 35mg rhynchophylline, 65mg hirsutine, 51mg hirsuteine and 27mg geissoschizine methylether were all simultaneously separated from 2.5g of refined alkaloids, with the purity of 86.4%, 97.5%, 90.3%, 92.1%, 98.5%, 92.3%, and 92.8%, respectively. The total content and purities of the seven minor indole alkaloids were tested by HPLC and their chemical structures were elucidated by ESI-HRMS and (1)H NMR. Copyright © 2015 Elsevier B.V. All rights reserved.

Computational Investigation of Fluidic Counterflow Thrust Vectoring

NASA Technical Reports Server (NTRS)

Hunter, Craig A.; Deere, Karen A.

1999-01-01

A computational study of fluidic counterflow thrust vectoring has been conducted. Two-dimensional numerical simulations were run using the computational fluid dynamics code PAB3D with two-equation turbulence closure and linear Reynolds stress modeling. For validation, computational results were compared to experimental data obtained at the NASA Langley Jet Exit Test Facility. In general, computational results were in good agreement with experimental performance data, indicating that efficient thrust vectoring can be obtained with low secondary flow requirements (less than 1% of the primary flow). An examination of the computational flowfield has revealed new details about the generation of a countercurrent shear layer, its relation to secondary suction, and its role in thrust vectoring. In addition to providing new information about the physics of counterflow thrust vectoring, this work appears to be the first documented attempt to simulate the counterflow thrust vectoring problem using computational fluid dynamics.

Scaling of counter-current imbibition recovery curves using artificial neural networks

NASA Astrophysics Data System (ADS)

Jafari, Iman; Masihi, Mohsen; Nasiri Zarandi, Masoud

2018-06-01

Scaling imbibition curves are of great importance in the characterization and simulation of oil production from naturally fractured reservoirs. Different parameters such as matrix porosity and permeability, oil and water viscosities, matrix dimensions, and oil/water interfacial tensions have an effective on the imbibition process. Studies on the scaling imbibition curves along with the consideration of different assumptions have resulted in various scaling equations. In this work, using an artificial neural network (ANN) method, a novel technique is presented for scaling imbibition recovery curves, which can be used for scaling the experimental and field-scale imbibition cases. The imbibition recovery curves for training and testing the neural network were gathered through the simulation of different scenarios using a commercial reservoir simulator. In this ANN-based method, six parameters were assumed to have an effect on the imbibition process and were considered as the inputs for training the network. Using the ‘Bayesian regularization’ training algorithm, the network was trained and tested. Training and testing phases showed superior results in comparison with the other scaling methods. It is concluded that using the new technique is useful for scaling imbibition recovery curves, especially for complex cases, for which the common scaling methods are not designed.

Office of River Protection Advanced Low-Activity Waste Glass Research and Development Plan

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

Peeler, David K.; Kim, Dong-Sang; Vienna, John D.

2015-11-01

The U.S. Department of Energy Office of River Protection (ORP) has initiated and leads an integrated Advanced Waste Glass (AWG) program to increase the loading of Hanford tank wastes in glass while meeting melter lifetime expectancies and process, regulatory, and product performance requirements. The integrated ORP program is focused on providing a technical, science-based foundation for making key decisions regarding the successful operation of the Hanford Tank Waste Treatment and Immobilization Plant (WTP) facilities in the context of an optimized River Protection Project (RPP) flowsheet. The fundamental data stemming from this program will support development of advanced glass formulations, keymore » product performance and process control models, and tactical processing strategies to ensure safe and successful operations for both the low-activity waste (LAW) and high-level waste vitrification facilities. These activities will be conducted with the objective of improving the overall RPP mission by enhancing flexibility and reducing cost and schedule. The purpose of this advanced LAW glass research and development plan is to identify the near-term, mid-term, and longer-term research and development activities required to develop and validate advanced LAW glasses, property-composition models and their uncertainties, and an advanced glass algorithm to support WTP facility operations, including both Direct Feed LAW and full pretreatment flowsheets. Data are needed to develop, validate, and implement 1) new glass property-composition models and 2) a new glass formulation algorithm. Hence, this plan integrates specific studies associated with increasing the Na2O and SO3/halide concentrations in glass, because these components will ultimately dictate waste loadings for LAW vitrification. Of equal importance is the development of an efficient and economic strategy for 99Tc management. Specific and detailed studies are being implemented to understand the fate of Tc throughout the WTP flowsheet and the underlying mechanisms that dictate its partitioning between streams within the LAW vitrification facility. These studies are aimed at increasing the single-pass Tc retention in glass and the potential use of high-temperature mineral phases to capture Tc. The Tc-bearing mineral phases would be thermally stable and resistant to Tc release during feed melting reactions or they could serve as alternative waste forms. The LAW glass research and development is focused on reducing the total volume of LAW glass produced and minimizing the impact of (or potentially eliminating) the need for recycle.« less

Velocity and void distribution in a counter-current two-phase flow

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

Gabriel, S.; Schulenberg, T.; Laurien, E.

2012-07-01

Different flow regimes were investigated in a horizontal channel. Simulating a hot leg injection in case of a loss of coolant accident or flow conditions in reflux condenser mode, the hydraulic jump and partially reversed flow were identified as major constraints for a high amount of entrained water. Trying to simulate the reflux condenser mode, the test section now includes an inclined section connected to a horizontal channel. The channel is 90 mm high and 110 mm wide. Tests were carried out for water and air at ambient pressure and temperature. High speed video-metry was applied to obtain velocities frommore » flow pattern maps of the rising and falling fluid. In the horizontal part of the channel with partially reversed flow the fluid velocities were measured by planar particle image velocimetry. To obtain reliable results for the gaseous phase, this analysis was extended by endoscope measurements. Additionally, a new method based on the optical refraction at the interface between air and water in a back-light was used to obtain time-averaged void fraction. (authors)« less

Validation of theoretical models of intrinsic torque in DIII-D

NASA Astrophysics Data System (ADS)

Grierson, B. A.; Wang, W. X.; Battaglia, D. J.; Chrystal, C.; Solomon, W. M.; Degrassie, J. S.; Staebler, G. M.; Boedo, J. A.

2016-10-01

Plasma rotation experiments in DIII-D are validating models of main-ion intrinsic rotation by testing Reynolds stress induced toroidal flow in the plasma core and intrinsic rotation induced by ion orbit losses in the plasma edge. In the core of dominantly electron heated plasmas with Te=Ti, the main-ion intrinsic toroidal rotation undergoes a reversal that correlates with the critical gradient for ITG turbulence. Residual stress arising from zonal-flow ExB shear and turbulence intensity gradient produce residual stress and counter-current intrinsic torque, which is balanced by momentum diffusion, creating the hollow profile. Quantitative agreement is obtained for the first time between the measured main-ion toroidal rotation and the rotation profile predicted by nonlinear GTS gyrokinetic simulations. At the plasma boundary, new main-ion CER measurements show a co-current rotation layer and this is tested against ion orbit loss models as the source of bulk plasma rotation. Work supported by the US Department of Energy under DE-AC02-09CH11466 and DE-FC02-04ER54698.

The Impact Of The MCU Life Extension Solvent On Sludge Batch 8 Projected Operating Windows

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

Peeler, D. K.; Edwards, T. B.; Stone, M. E.

2013-08-14

As a part of the Actinide Removal Process (ARP)/Modular Caustic Side Solvent Extraction Unit (MCU) Life Extension Project, a next generation solvent (NGS) and a new strip acid will be deployed. The strip acid will be changed from dilute nitric acid to dilute boric acid (0.01 M). Because of these changes, experimental testing or evaluations with the next generation solvent are required to determine the impact of these changes (if any) to Chemical Process Cell (CPC) activities, glass formulation strategies, and melter operations at the Defense Waste Processing Facility (DWPF). The introduction of the dilute (0.01M) boric acid stream intomore » the DWPF flowsheet has a potential impact on glass formulation and frit development efforts since B2O3 is a major oxide in frits developed for DWPF. Prior knowledge of this stream can be accounted for during frit development efforts but that was not the case for Sludge Batch 8 (SB8). Frit 803 has already been recommended and procured for SB8 processing; altering the frit to account for the incoming boron from the strip effluent (SE) is not an option for SB8. Therefore, the operational robustness of Frit 803 to the introduction of SE including its compositional tolerances (i.e., up to 0.0125M boric acid) is of interest and was the focus of this study. The primary question to be addressed in the current study was: What is the impact (if any) on the projected operating windows for the Frit 803 – SB8 flowsheet to additions of B2O3 from the SE in the Sludge Receipt and Adjustment Tank (SRAT)? More specifically, will Frit 803 be robust to the potential compositional changes occurring in the SRAT due to sludge variation, varying additions of ARP and/or the introduction of SE by providing access to waste loadings (WLs) of interest to DWPF? The Measurement Acceptability Region (MAR) results indicate there is very little, if any, impact on the projected operating windows for the Frit 803 – SB8 system regardless of the presence or absence of ARP and SE (up to 2 wt% B2O3 contained in the SRAT and up to 2000 gallons of ARP). It should be noted that 0.95 wt% B2O3 is the nominal projected concentration in the SRAT based on a 0.0125M boric acid flowsheet with 70,000 liters of SE being added to the SRAT. The impact on CPC processing of a 0.01M boric acid solution for elution of cesium during Modular Caustic Side Solvent Extraction Unit (MCU) processing has previously been evaluated by the Savannah River National Laboratory (SRNL). Increasing the acid strength to 0.0125M boric acid to account for variations in the boric acid strength has been reviewed versus the previous evaluation. The amount of acid from the boric acid represented approximately 5% of the total acid during the previous evaluation. An increase from 0.01 to 0.0125M boric acid represents a change of approximately 1.3% which is well within the error of the acid calculation. Therefore, no significant changes to CPC processing (hydrogen generation, metal solubilities, rheological properties, REDOX control, etc.) are expected from an increase in allowable boric acid concentration from 0.01M to 0.0125M.« less

Chemotaxis-defective mutants of the nematode Caenorhabditis elegans.

PubMed

Dusenbery, D B; Sheridan, R E; Russell, R L

1975-06-01

The technique of countercurrent separation has been used to isolate 17 independent chemotaxis-defective mutants of the nematode Caenorhabditis elegans. The mutants, selected to be relatively insensitive to the normally attractive salt NaCl, show varying degrees of residual sensitivity; some are actually weakly repelled by NaCl. The mutants are due to single gene defects, are autosomal and recessive, and identify at least five complementation groups.

Application Potential of Energy Systems at Navy Sites. Volume I. Methodology and Results.

DTIC Science & Technology

1980-01-01

see Table 5-4). Flue gas desulfurization (FGD), electrostatic precipitators (ESP), and staged combustion (SC) were selected to control SOX...energy sources are required to meet proposed Federal Stationary Source Standards. Flue gas desulfurization (FGD), electrostatic precipitators (ESP...pollution control equipment follows: * FGD -- Flue gas from the furnace is passed counter-currently through a limestone (CaCO3) slurry which reacts with

A general ionic liquid pH-zone-refining countercurrent chromatography method for separation of alkaloids from Nelumbo nucifera Gaertn.

PubMed

Fang, Yingtong; Li, Quan; Shao, Qian; Wang, Binghai; Wei, Yun

2017-07-21

The alkaloids from lotus (Nelumbo nucifera Gaertn) are effective in lowering hyperlipemia and level of cholesterol. However, there is not a general method for their separation. In this work, a general ionic liquid pH-zone-refining countercurrent chromatography method for isolation and purification of six alkaloids from the whole lotus plant was successfully established by using ionic liquids as the modifier of the two-phase solvent system. The conditions of ionic liquid pH-zone-refining countercurrent chromatography, involving solvent systems, concentration of retainer and eluter, types of ionic liquids, the content of ionic liquids as well as ionic liquids posttreatment, were optimized to improve extraction efficiency. Finally, the separation of these six alkaloids was performed with a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water-[C 4 mim][PF 6 ] at a volume ratio of 5:2:2:8:0.1, where 10mM TEA was added to the organic stationary phase as a retainer and 3mM HCl was added to the aqueous mobile phase as an eluter. As a result, six alkaloids including N-nornuciferine, liensinine, nuciferine, isoliensinine, roemerine and neferine were successfully separated with the purities of 97.0%, 90.2%, 94.7%, 92.8%, 90.4% and 95.9%, respectively. The established general method has been respectively applied to the crude samples of lotus leaves and lotus plumules. A total of 37.3mg of liensinine, 57.7mg of isoliensinine and 179.9mg of neferine were successfully purified in one run from 1.00g crude extract of lotus plumule with the purities of 93.2%, 96.5% and 98.8%, respectively. Amount of 45.6mg N-nornuciferine, 21.6mg nuciferine and 11.7mg roemerine was obtained in one step separation from 1.05g crude extract of lotus leaves with the purity of 96.9%, 95.6% and 91.33%, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

A combination strategy for extraction and isolation of multi-component natural products by systematic two-phase solvent extraction-(13)C nuclear magnetic resonance pattern recognition and following conical counter-current chromatography separation: Podophyllotoxins and flavonoids from Dysosma versipellis (Hance) as examples.

PubMed

Yang, Zhi; Wu, Youqian; Wu, Shihua

2016-01-29

Despite of substantial developments of extraction and separation techniques, isolation of natural products from natural resources is still a challenging task. In this work, an efficient strategy for extraction and isolation of multi-component natural products has been successfully developed by combination of systematic two-phase liquid-liquid extraction-(13)C NMR pattern recognition and following conical counter-current chromatography separation. A small-scale crude sample was first distributed into 9 systematic hexane-ethyl acetate-methanol-water (HEMWat) two-phase solvent systems for determination of the optimum extraction solvents and partition coefficients of the prominent components. Then, the optimized solvent systems were used in succession to enrich the hydrophilic and lipophilic components from the large-scale crude sample. At last, the enriched components samples were further purified by a new conical counter-current chromatography (CCC). Due to the use of (13)C NMR pattern recognition, the kinds and structures of major components in the solvent extracts could be predicted. Therefore, the method could collect simultaneously the partition coefficients and the structural information of components in the selected two-phase solvents. As an example, a cytotoxic extract of podophyllotoxins and flavonoids from Dysosma versipellis (Hance) was selected. After the systematic HEMWat system solvent extraction and (13)C NMR pattern recognition analyses, the crude extract of D. versipellis was first degreased by the upper phase of HEMWat system (9:1:9:1, v/v), and then distributed in the two phases of the system of HEMWat (2:8:2:8, v/v) to obtain the hydrophilic lower phase extract and lipophilic upper phase extract, respectively. These extracts were further separated by conical CCC with the HEMWat systems (1:9:1:9 and 4:6:4:6, v/v). As results, total 17 cytotoxic compounds were isolated and identified. In general, whole results suggested that the strategy was very efficient for the systematic extraction and isolation of biological active components from the complex biomaterials. Copyright © 2016 Elsevier B.V. All rights reserved.

Trip report. Eurochemic company assistance: Hanford Atomic Products Operation spent fuel processing technology

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

Shank, E.M.

1959-06-23

Information obtained from HAPO during visit by M.K. Twichell, UCNC, and E.M. Shank, ORNL, is given. Included are the tentative procedures for obtaining and transmitting information to the Eurochemic company. Discussions are given on pulsed columns, corrosion, puse generators, centrifuges, valves, in-line instrumentation, evaporators, resin column design, off-gas processing, solvent recovery, liquid-waste handling, process control, equipment decontamination, criticality, radiation protection, diluent, and solvent stability, backmixing in a pulsed column, and use of 40% TBP in the purex flowsheet.

Dissolution of used nuclear fuel using recycled nitric acid

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

Almond, Philip M.; Daniel, Jr., William E.; Rudisill, Tracy S.

An evaluation was performed on the feasibility of using HB-Line anion exchange column waste streams from Alternate Feedstock 2 (AFS-2) processing for the dissolver solution for used nuclear fuel (UNF) processing. The targeted UNF for dissolution using recycled solution are fuels similar to the University of Missouri Research Reactor (MURR) fuel. Furthermore, the objectives of this experimental program were to validate the feasibility of using impure dissolver solutions with the MURR dissolution flowsheet to verify they would not significantly affect dissolution of the UNF in a detrimental manner.

Nitrogen Trifluoride-Based Fluoride- Volatility Separations Process: Initial Studies

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

McNamara, Bruce K.; Scheele, Randall D.; Casella, Andrew M.

2011-09-28

This document describes the results of our investigations on the potential use of nitrogen trifluoride as the fluorinating and oxidizing agent in fluoride volatility-based used nuclear fuel reprocessing. The conceptual process uses differences in reaction temperatures between nitrogen trifluoride and fuel constituents that produce volatile fluorides to achieve separations and recover valuable constituents. We provide results from our thermodynamic evaluations, thermo-analytical experiments, kinetic models, and provide a preliminary process flowsheet. The evaluations found that nitrogen trifluoride can effectively produce volatile fluorides at different temperatures dependent on the fuel constituent.

Randolph Plant passes 60-million-ton milestone

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

Sprouls, M.W.; Adam, B.O.

1983-09-01

Peabody Coal Co.'s Randolph coal preparation plant has processed 60 million tons of coal during 10 years of operation. The plant, which is in Illinois, receives coal from 3 mines and 2 more will eventually send their output for cleaning. Coal from one mine travels 2 miles overland to a 30,000 ton conical bunker constructed of Reinforced Earth. Clean coal is supplied for electricity generation. The plant uses water-only processes, with a jig and three stages of hydrocyclones. A flowsheet of the scalper circuit is given.

The Design of Pressure Safety Systems in the Alumina Industry

NASA Astrophysics Data System (ADS)

Haneman, Brady

The alumina refinery presents the designer with multiple challenges. For a given process flowsheet, the mechanical equipment installed must be routinely inspected and maintained. Piping systems must also be inspected routinely for signs of erosion and/or corrosion. Rapid deposits of chemical species such as lime, silica, and alumina on equipment and piping need special consideration in the mechanical design of the facilities, such that fluid flows are not unduly interrupted. Above and beyond all else, the process plant must be a safe place of work for refinery personnel.

Dissolution of used nuclear fuel using recycled nitric acid

DOE PAGES

Almond, Philip M.; Daniel, Jr., William E.; Rudisill, Tracy S.

2017-03-20

An evaluation was performed on the feasibility of using HB-Line anion exchange column waste streams from Alternate Feedstock 2 (AFS-2) processing for the dissolver solution for used nuclear fuel (UNF) processing. The targeted UNF for dissolution using recycled solution are fuels similar to the University of Missouri Research Reactor (MURR) fuel. Furthermore, the objectives of this experimental program were to validate the feasibility of using impure dissolver solutions with the MURR dissolution flowsheet to verify they would not significantly affect dissolution of the UNF in a detrimental manner.

Hydrometallurgical recovery of germanium from coal gasification fly ash: pilot plant scale evaluation

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

Arroyo, F.; Fernandez-Pereira, C.; Olivares, J.

2009-04-15

In this article, a hydrometallurgical method for the selective recovery of germanium from fly ash (FA) has been tested at pilot plant scale. The pilot plant flowsheet comprised a first stage of water leaching of FA, and a subsequent selective recovery of the germanium from the leachate by solvent extraction method. The solvent extraction method was based on Ge complexation with catechol in an aqueous solution followed by the extraction of the Ge-catechol complex (Ge(C{sub 6}H{sub 4}O{sub 2}){sub 3}{sup 2-}) with an extracting organic reagent (trioctylamine) diluted in an organic solvent (kerosene), followed by the subsequent stripping of the organicmore » extract. The process has been tested on a FA generated in an integrated gasification with combined cycle (IGCC) process. The paper describes the designed 5 kg/h pilot plant and the tests performed on it. Under the operational conditions tested, approximately 50% of germanium could be recovered from FA after a water extraction at room temperature. Regarding the solvent extraction method, the best operational conditions for obtaining a concentrated germanium-bearing solution practically free of impurities were as follows: extraction time equal to 20 min; aqueous phase/organic phase volumetric ratio equal to 5; stripping with 1 M NaOH, stripping time equal to 30 min, and stripping phase/organic phase volumetric ratio equal to 5. 95% of germanium were recovered from water leachates using those conditions.« less

GASEOUS DISPOSAL PROCESS

DOEpatents

Ryan, R.F.; Thomasson, F.R.; Hicks, J.H.

1963-01-22

A method is described of removing gaseous radioactive Xe and Kr from water containing O. The method consists in stripping the gases from the water stream by means of H flowing countercurrently to the stream. The gases are then heated in a deoxo bed to remove O. The carrier gas is next cooled and passed over a charcoal adsorbent bed maintained at a temperature of about --280 deg F to remove the Xe and Kr. (AEC)

Compact type-I coil planet centrifuge for counter-current chromatography

PubMed Central

Yang, Yi; Gu, Dongyu; Liu, Yongqiang; Aisa, Haji Akber; Ito, Yoichiro

2009-01-01

A compact type-I coil planet centrifuge has been developed for performing counter-current chromatography. It has a revolution radius of 10 cm and a column holder height of 5 cm compared with 37 cm and 50 cm in the original prototype, respectively. The reduction in the revolution radius and column length permits application of higher revolution speed and more stable balancing of the rotor which leads us to learn more about its performance and the future potential of type-I coil planet centrifuge. The chromatographic performance of this apparatus was evaluated in terms of retention of the stationary phase (Sf), peak resolution (Rs), theoretical plate (N) and peak retention time (tR). The results of the experiment indicated that increasing the revolution speed slightly improved both the retention of the stationary phase and the peak resolution while the separation time is remarkably shortened to yield an excellent peak resolution at a revolution speed of 800 rpm. With a 12 ml capacity coiled column, DNP-glu, DNP-β-ala and DNP-ala were resolved at Rs of 2.75 and 2.16 within 90 min at a flow rate of 0.4 ml/min. We believe that the compact type-I coil planet centrifuge has a high analytical potential. PMID:20060979

Compact type-I coil planet centrifuge for counter-current chromatography.

PubMed

Yang, Yi; Gu, Dongyu; Liu, Yongqiang; Aisa, Haji Akber; Ito, Yoichiro

2010-02-19

A compact type-I coil planet centrifuge has been developed for performing counter-current chromatography. It has a revolution radius of 10 cm and a column holder height of 5 cm compared with 37 and 50 cm in the original prototype, respectively. The reduction in the revolution radius and column length permits application of higher revolution speed and more stable balancing of the rotor which leads us to learn more about its performance and the future potential of type-I coil planet centrifuge. The chromatographic performance of this apparatus was evaluated in terms of retention of the stationary phase (S(f)), peak resolution (R(s)), theoretical plate (N) and peak retention time (t(R)). The results of the experiment indicated that increasing the revolution speed slightly improved both the retention of the stationary phase and the peak resolution while the separation time is remarkably shortened to yield an excellent peak resolution at a revolution speed of 800 rpm. With a 12 ml capacity coiled column, DNP-DL-glu, DNP-beta-ala and DNP-l-ala were resolved at R(s) of 2.75 and 2.16 within 90 min at a flow rate of 0.4 ml/min. We believe that the compact type-I coil planet centrifuge has a high analytical potential. Published by Elsevier B.V.

Rational approach to solvent system selection for liquid-liquid extraction-assisted sample pretreatment in counter-current chromatography.

PubMed

Wang, Jiajia; Gu, Dongyu; Wang, Miao; Guo, Xinfeng; Li, Haoquan; Dong, Yue; Guo, Hong; Wang, Yi; Fan, Mengqi; Yang, Yi

2017-05-15

A rational liquid-liquid extraction approach was established to pre-treat samples for high-speed counter-current chromatography (HSCCC). n-Hexane-ethyl acetate-methanol-water (4:5:4:5, v/v) and (1:5:1:5, v/v) were selected as solvent systems for liquid-liquid extraction by systematically screening K of target compounds to remove low- and high-polarity impurities in the sample, respectively. After liquid-liquid extraction was performed, 1.4g of crude sample II was obtained from 18.5g of crude sample I which was extracted from the flowers of Robinia pseudoacacia L., and then separated with HSCCC by using a solvent system composed of n-hexane-ethyl acetate-methanol-water (1:2:1:2, v/v). As a result, 31mg of robinin and 37mg of kaempferol 7-O-α-l-rhamnopyranoside were isolated from 200mg of crude sample II in a single run of HSCCC. A scale-up separation was also performed, and 160mg of robinin with 95% purity and 188mg of kaempferol 7-O-α-l-rhamnopyranoside with 97% purity were produced from 1.2g of crude sample II. Copyright © 2017 Elsevier B.V. All rights reserved.

Hydrophilic organic/salt-containing aqueous two-phase solvent system for counter-current chromatography: a novel technique for separation of polar compounds.

PubMed

Liu, Dan; Zou, Xiaowei; Gao, Mingzhe; Gu, Ming; Xiao, Hongbin

2014-08-22

Hydrophilic organic/salt-containing aqueous two-phase system composing of ethanol, water and ammonium sulfate for separation polar compounds was investigated on multilayer coil associated with J-type HSCCC devices. Compared to the classical polar solvent system based on 1-butanol-water or PEG1000-ammonium sulfate-water, the water content of upper phase in ethanol-ammonium sulfate-water systems was from 53.7% to 32.8% (wt%), closed to PEG1000-ammonium sulfate-water aqueous two-phase systems and higher than 1-butanol-water (22.0%, wt%). Therefore, the polarity of ethanol-ammonium sulfate-water is in the middle of 1-butanol-water and PEG-ammonium sulfate-water system, which is quite good for separating polar compounds like phenols, nucleosides and amino acids with low partition coefficient in 1-octanol-water system. The retention of stationary phase in four elution mode on type-J counter-current chromatography devices with multilayer coil column changed from 26% to 71%. Hydrodynamic trend possess both intermediate and hydrophilic solvent system property, which closely related to the composition of solvent system. The applicability of this system was demonstrated by successful separation of adenosine, uridine guanosine and cytidine. Copyright © 2014 Elsevier B.V. All rights reserved.

Simulations of toroidal Alfvén eigenmode excited by fast ions on the Experimental Advanced Superconducting Tokamak

NASA Astrophysics Data System (ADS)

Pei, Youbin; Xiang, Nong; Shen, Wei; Hu, Youjun; Todo, Y.; Zhou, Deng; Huang, Juan

2018-05-01

Kinetic-MagnetoHydroDynamic (MHD) hybrid simulations are carried out to study fast ion driven toroidal Alfvén eigenmodes (TAEs) on the Experimental Advanced Superconducting Tokamak (EAST). The first part of this article presents the linear benchmark between two kinetic-MHD codes, namely MEGA and M3D-K, based on a realistic EAST equilibrium. Parameter scans show that the frequency and the growth rate of the TAE given by the two codes agree with each other. The second part of this article discusses the resonance interaction between the TAE and fast ions simulated by the MEGA code. The results show that the TAE exchanges energy with the co-current passing particles with the parallel velocity |v∥ | ≈VA 0/3 or |v∥ | ≈VA 0/5 , where VA 0 is the Alfvén speed on the magnetic axis. The TAE destabilized by the counter-current passing ions is also analyzed and found to have a much smaller growth rate than the co-current ions driven TAE. One of the reasons for this is found to be that the overlapping region of the TAE spatial location and the counter-current ion orbits is narrow, and thus the wave-particle energy exchange is not efficient.

Semi-industrial isolation of salicin and amygdalin from plant extracts using slow rotary counter-current chromatography.

PubMed

Du, Qizhen; Jerz, Gerold; Ha, Yangchun; Li, Lei; Xu, Yuanjin; Zhang, Qi; Zheng, Qunxiong; Winterhalter, Peterb; Ito, Yoichiro

2005-05-13

Salicin in the bark extract of Salix alba and amygdalin in the fruit extract of Semen armeniacae were each separated by slow rotary counter-current chromatography (SRCCC). The apparatus was equipped with a 40-L column made of 17 mm i.d. convoluted Teflon tubing. A 500g amount of crude extract containing salicin at 13.5% was separated yielding 63.5 g of salicin at 95.3% purity in 20h using methyl tert-butyl ether-l-butanol (1:3) saturated by methanol-water (1:5) as a stationary phase and methanol-water (1:5) saturated by methyl tert-butyl ether-1-butanol (1:3) as a mobile phase. A 400g amount of crude extract containing amygdalin at 55.3% was isolated to yield 221.2g of amygdalin at 94.1% purity in 19h using ethyl acetate-1-butanol (1:2) saturated by water as a stationary phase and water saturated by ethyl acetate-1-butanol (1:2) as a mobile phase. The flow rate of the mobile phase was 50 ml/min. The results show that industrial SRCCC separation of salicin and amygdalin is feasible using a larger column at a higher flow rate of the mobile phase.

Rapid isolation and purification of phorbol esters from Jatropha curcas by high-speed countercurrent chromatography.

PubMed

Hua, Wan; Hu, Huiling; Chen, Fang; Tang, Lin; Peng, Tong; Wang, Zhanguo

2015-03-18

In this work, a high-speed countercurrent chromatography (HSCCC) method was established for the preparation of phorbol esters (PEs) from Jatropha curcas. n-Hexane-ethyl acetate-methanol-water (1.5:1.5:1.2:0.5, v/v) was selected as the optimum two-phase solvent system to separate and purify jatropha factor C1 (JC1) with a purity of 85.2%, as determined by HPLC, and to obtain a mixture containing four or five PEs. Subsequently, continuous semipreparative HPLC was applied to further purify JC1 (99.8% as determined by HPLC). In addition, UPLC-PDA and UPLC-MS were established and successfully used to evaluate the isolated JC1 and PE-rich crude extract. The purity of JC1 was only 87.8% by UPLC-UV. A peak (a compound highly similar to JC1) was indentified as the isomer of JC1 by comparing the characteristic UV absorption and MS spectra. Meanwhile, this strategy was also applied to analyze the PE-rich crude extract from J. curcas. It is interesting that there may be more than 15 PEs according to the same quasi-molecular ion peaks, highly similar sequence-specific fragment ions, and similar UV absorption spectrum.

SEPARATION OF THE MINOR FLAVONOLS FROM FLOS GOSSYPII BY HIGH-SPEED COUNTERCURRENT CHROMATOGRAPHY

PubMed Central

Yang, Yi; Zhao, Yongxin; Gu, Dongyu; Ayupbek, Amatjan; Huang, Yun; Dou, Jun; Ito, Yoichiro; Zhang, Tianyou; Aisa, Haji Akber

2010-01-01

An effective high-speed countercurrent chromatography (HSCCC) method was established for further separation and purification of four minor flavonols in addition to five major flavonols which were reported by our previous study from extracts of Flos Gossypii. HSCCC was performed with three two-phase solvent systems composed of n-hexane-ethyl acetate-methanol-water (7.5:15:6:7, v/v), (2.5:15:2:7, v/v) and (0:1:0:1, v/v). The separation was repeated 3 times, and 3.8 mg of 8-methoxyl-kaempferol-7-O-β-D-rhamnoside (HPLC purity 98.27%), 6.7 mg of astragalin (HPLC purity 94.18%), 3.3 mg of 4′-methoxyl-quercetin-7-O-β-D-glucoside (HPLC purity 94.30%) and 8.2 mg of hyperoside (HPLC purity 93.48%) were separated from 150 mg of the crude sample. The chemical structures of the flavonols were confirmed by MS, 1H NMR and 13C NMR. Meanwhile, the results indicated that the target compound with smaller K value (<0.5) can be separated by increasing column length of HSCCC. And four separation rules of flavonols according to the present study and references were summarized, which can be used as a useful guide for separation of flavonols by HSCCC. PMID:21494318

Purification of optical imaging ligand-Cybesin by high-speed counter-current chromatography

PubMed Central

Ma, Zhiyong; Ma, Ying; Sun, Xilin; Ye, Yunpeng; Shen, Baozhong; Chen, Xiaoyuan; Ito, Yoichiro

2010-01-01

Fluorescent Cybesin (Cypate-Bombesin Peptide Analogue Conjugate) was synthesized from Indocyanine Green (ICG) and the bombesin receptor ligand as a contrast agent for detecting pancreas tumors. However, the LC–MS analysis indicated that the target compound was only a minor component in the reaction mixture. Since preparative HPLC can hardly separate such a small amount of the target compound directly from the original crude reaction mixture without a considerable adsorptive loss onto the solid support, high-speed counter-current chromatography (HSCCC) was used for purification since the method uses no solid support and promises high sample recovery. A suitable two-phase solvent system composed of hexane/ethyl acetate/methanol/methyl t.-butyl ether/acetonitrile/water) at a volume ratio of 1:1:1:4:4:7 was selected based on the partition coefficient of Cybesin (K ≈ 0.9) determined by LC–MS. The separation was performed in two steps using the same solvent system with lower aqueous mobile phase. From 400 mg of the crude reaction mixture the first separation yielded 7.7 mg of fractions containing the target compound at 12.8% purity, and in the second run 1 mg of Cybesin was obtained at purity of 94.0% with a sample recovery rate of over 95% based on the LC–MS Analysis. PMID:20933483

Hepatoprotective Flavonoids in Opuntia ficus-indica Fruits by Reducing Oxidative Stress in Primary Rat Hepatocytes.

PubMed

Kim, Jung Wha; Kim, Tae Bum; Kim, Hyun Woo; Park, Sang Wook; Kim, Hong Pyo; Sung, Sang Hyun

2017-01-01

Liver disorder was associated with alcohol consumption caused by hepatic cellular damages. Opuntia ficus-indica fruit extracts (OFIEs), which contain betalain pigments and polyphenols including flavonoids, have been introduced as reducing hangover symptoms and liver protective activity. To evaluate hepatoprotective activity of OFIEs and isolated compounds by high-speed countercurrent chromatography (HSCCC). The extract of O. ficus-indica fruits was fractionated into methylene chloride and n -butanol. The n -butanol fraction was isolated by HSCCC separation (methylene chloride-methanol- n -butanol-water, 5:4:3:5, v/v/v/v). The hepatoprotective activity of OFIEs and isolated compounds was evaluated on rat primary hepatocytes against ethanol-induced toxicity. Antioxidative parameters such as glutathione reductase and glutathione peroxidase (GSH-P x ) enzymes and the GSH content were measured. Two flavonoids, quercetin 3- O -methyl ester (1) and (+)-taxifolin, and two flavonoid glycosides, isorhamnetin 3- O -β- d -glucoside (3) and narcissin (4), were isolated from the n -butanol fraction by HSCCC separation. Among them, compound 2 significantly protected rat primary hepatocytes against ethanol exposure by preserving antioxidative properties of GR and GSH-P x . OFIEs and (+)-taxifolin were suggested to reduce hepatic damage by alcoholic oxidative stress. Hepatoprotective Flavonoids were isolated from Opuntia ficus-indica by high -speed countercurrent chromatography (HSCCC).

Purification of Active Myrosinase from Plants by Aqueous Two-Phase Counter-Current Chromatography

PubMed Central

Wade, Kristina L.; Ito, Yoichiro; Ramarathnam, Aarthi; Holtzclaw, W. David; Fahey, Jed W.

2014-01-01

Introduction Myrosinase (thioglucoside glucohydrolase; E.C. 3.2.1.147), is a plant enzyme of increasing interest and importance to the biomedical community. Myrosinase catalyses the formation of isothiocyanates such as sulforaphane (frombroccoli) and 4-(α-l-rhamnopyranosyloxy)benzyl isothiocyanate (from moringa), which are potent inducers of the cytoprotective phase-2 response in humans, by hydrolysis of their abundant glucosinolate (β-thioglucoside N-hydroxysulphate) precursors. Objective To develop an aqueous two-phase counter-current chromatography (CCC) system for the rapid, three-step purification of catalytically active myrosinase. Methods A high-concentration potassium phosphate and polyethylene glycol biphasic aqueous two-phase system (ATPS) is used with a newly developed CCC configuration that utilises spiral-wound, flat-twisted tubing (with an ovoid cross-section). Results Making the initial crude plant extract directly in the ATPS and injecting only the lower phase permitted highly selective partitioning of the myrosinase complex before a short chromatography on a spiral disk CCC. Optimum phase retention and separation of myrosinase from other plant proteins afforded a 60-fold purification. Conclusion Catalytically active myrosinase is purified from 3-day broccoli sprouts, 7-day daikon sprouts, mustard seeds and the leaves of field-grown moringa trees, in a CCC system that is predictably scalable. PMID:25130502

Comparison in partition efficiency of protein separation between four different tubing modifications in spiral high-speed countercurrent chromatography

PubMed Central

Ito, Yoichiro; Clary, Robert

2016-01-01

High-speed countercurrent chromatography with a spiral tube assembly can retain a satisfactory amount of stationary phase of polymer phase systems used for protein separation. In order to improve the partition efficiency a simple tool to modify the tubing shapes was fabricated, and the following four different tubing modifications were made: intermittently pressed at 10 mm width, flat, flat-wave, and flat-twist. Partition efficiencies of the separation column made from these modified tubing were examined in protein separation with an aqueous-aqueous polymer phase system at flow rates of 1–2 ml/min under 800 rpm. The results indicated that the column with all modified tubing improved the partition efficiency at a flow rate of 1 ml/min, but at a higher flow rate of 2 ml/min the columns made of flattened tubing showed lowered partition efficiency apparently due to the loss of the retained stationary phase. Among all the modified columns, the column with intermittently pressed tubing gave the best peak resolution. It may be concluded that the intermittently pressed and flat-twist improve the partition efficiency in a semi-preparative separation while other modified tubing of flat and flat-wave configurations may be used for analytical separations with a low flow rate. PMID:27790621

Comparison in partition efficiency of protein separation between four different tubing modifications in spiral high-speed countercurrent chromatography.

PubMed

Ito, Yoichiro; Clary, Robert

2016-12-01

High-speed countercurrent chromatography with a spiral tube assembly can retain a satisfactory amount of stationary phase of polymer phase systems used for protein separation. In order to improve the partition efficiency a simple tool to modify the tubing shapes was fabricated, and the following four different tubing modifications were made: intermittently pressed at 10 mm width, flat, flat-wave, and flat-twist. Partition efficiencies of the separation column made from these modified tubing were examined in protein separation with an aqueous-aqueous polymer phase system at flow rates of 1-2 ml/min under 800 rpm. The results indicated that the column with all modified tubing improved the partition efficiency at a flow rate of 1 ml/min, but at a higher flow rate of 2 ml/min the columns made of flattened tubing showed lowered partition efficiency apparently due to the loss of the retained stationary phase. Among all the modified columns, the column with intermittently pressed tubing gave the best peak resolution. It may be concluded that the intermittently pressed and flat-twist improve the partition efficiency in a semi-preparative separation while other modified tubing of flat and flat-wave configurations may be used for analytical separations with a low flow rate.

Purification of active myrosinase from plants by aqueous two-phase counter-current chromatography.

PubMed

Wade, Kristina L; Ito, Yoichiro; Ramarathnam, Aarthi; Holtzclaw, W David; Fahey, Jed W

2015-01-01

Myrosinase (thioglucoside glucohydrolase; E.C. 3.2.1.147), is a plant enzyme of increasing interest and importance to the biomedical community. Myrosinase catalyses the formation of isothiocyanates such as sulforaphane (from broccoli) and 4-(α-l-rhamnopyranosyloxy)benzyl isothiocyanate (from moringa), which are potent inducers of the cytoprotective phase-2 response in humans, by hydrolysis of their abundant glucosinolate (β-thioglucoside N-hydroxysulphate) precursors. To develop an aqueous two-phase counter-current chromatography (CCC) system for the rapid, three-step purification of catalytically active myrosinase. A high-concentration potassium phosphate and polyethylene glycol biphasic aqueous two-phase system (ATPS) is used with a newly developed CCC configuration that utilises spiral-wound, flat-twisted tubing (with an ovoid cross-section). Making the initial crude plant extract directly in the ATPS and injecting only the lower phase permitted highly selective partitioning of the myrosinase complex before a short chromatography on a spiral disk CCC. Optimum phase retention and separation of myrosinase from other plant proteins afforded a 60-fold purification. Catalytically active myrosinase is purified from 3-day broccoli sprouts, 7-day daikon sprouts, mustard seeds and the leaves of field-grown moringa trees, in a CCC system that is predictably scalable. Copyright © 2014 John Wiley & Sons, Ltd.

Separation and preparation of 6-gingerol from molecular distillation residue of Yunnan ginger rhizomes by high-speed counter-current chromatography and the antioxidant activity of ginger oils in vitro.

PubMed

Gan, Zhilin; Liang, Zheng; Chen, Xiaosong; Wen, Xin; Wang, Yuxiao; Li, Mo; Ni, Yuanying

2016-02-01

Molecular distillation residue (MD-R) from ginger had the most total phenol content of 247.6mg gallic acid equivalents per gram (GAE/g) among the ginger oils. High-speed counter-current chromatography (HSCCC) technique in semi-preparative scale was successfully performed in separation and purification of 6-gingerol from MD-R by using a two-phase solvent system composed of n-hexane-ethyl acetate-methanol-water (10:2:5:7, v/v/v/v). The target compound was isolated, collected, purified by HSCCC in the head-tail mode, and then analyzed by HPLC. A total of 90.38±0.53mg 6-gingerol was obtained from 600mg MD-R, with purity of 99.6%. In addition, the structural identification of 6-gingerol was performed by EI/MS, (1)H NMR and (13)C NMR. Moreover, the orders of antioxidant activity were vitamin E (VE)>supercritical fluid extraction oleoresin (SFE-O)=MD-R=6-gingerol>molecular distillation essential oil (MD-EO) and butylated hydroxytoluene (BHT)=VE>6-gingerol>MD-R=SFE-O>MD-EO, respectively in 2,2-diphenyl-1-picrylhydrazyl radical (DPPH) scavenging and β-Carotene bleaching. Copyright © 2016 Elsevier B.V. All rights reserved.

Gas holdup and flow regime transition in spider-sparger bubble column: effect of liquid phase properties

NASA Astrophysics Data System (ADS)

Besagni, G.; Inzoli, F.; De Guido, G.; Pellegrini, L. A.

2017-01-01

This paper discusses the effects of the liquid velocity and the liquid phase properties on the gas holdup and the flow regime transition in a large-diameter and large-scale counter-current two-phase bubble column. In particular, we compared and analysed the experimental data obtained in our previous experimental studies. The bubble column is 5.3 m in height, has an inner diameter of 0.24 m, it was operated with gas superficial velocities in the range of 0.004-0.20 m/s and, in the counter-current mode, the liquid was recirculated up to a superficial velocity of -0.09 m/s. Air was used as the dispersed phase and various fluids (tap water, aqueous solutions of sodium chloride, ethanol and monoethylene glycol) were employed as liquid phases. The experimental dataset consist in gas holdup measurements and was used to investigate the global fluid dynamics and the flow regime transition between the homogeneous flow regime and the transition flow regime. We found that the liquid velocity and the liquid phase properties significantly affect the gas holdup and the flow regime transition. In this respect, a possible relationship (based on the lift force) between the flow regime transition and the gas holdup was proposed.

Characterizing the interaction between enantiomers of eight psychoactive drugs and highly sulfated-β-cyclodextrin by counter-current capillary electrophoresis.

PubMed

Asensi-Bernardi, Lucía; Escuder-Gilabert, Laura; Martín-Biosca, Yolanda; Sagrado, Salvador; Medina-Hernández, María José

2014-01-01

The estimation of apparent binding constants and limit mobilities of the complexes of the enantiomers that characterize the interaction of enantiomers with chiral selectors, in this case highly sulfated β-cyclodextrin, was approached using a simple and economic electrophoretic modality, the complete filling technique (CFT) in counter-current mode. The enantiomers of eight psychoactive drugs, four antihistamines (dimethindene, promethazine, orphenadrine and terfenadine) and four antidepressants (bupropion, fluoxetine, nomifensine and viloxazine) were separated for the first time for this cyclodextrin (CD). Estimations of thermodynamic and electrophoretic enantioselectivies were also performed. Results indicate that, in general, thermodynamic enantioselectivity is the main component explaining the high resolution found, but also one case suggests that electrophoretic enantioselectivity itself is enough to obtain a satisfactory resolution. CFT results advantageous compared with conventional capillary electrophoresis (CE) and partial filling technique (PFT) for the study of the interaction between drugs and chiral selectors. It combines the use of a simple fitting model (as in CE), when the enantiomers do not exit the chiral selector plug during the separation (i.e. mobility of electroosmotic flow larger than mobility of CD), and drastic reduction of the consumption (and cost; ~99.7%) of the CD reagent (as in PFT) compared with the conventional CE. Copyright © 2013 John Wiley & Sons, Ltd.

Experimental design of a twin-column countercurrent gradient purification process.

PubMed

Steinebach, Fabian; Ulmer, Nicole; Decker, Lara; Aumann, Lars; Morbidelli, Massimo

2017-04-07

As typical for separation processes, single unit batch chromatography exhibits a trade-off between purity and yield. The twin-column MCSGP (multi-column countercurrent solvent gradient purification) process allows alleviating such trade-offs, particularly in the case of difficult separations. In this work an efficient and reliable procedure for the design of the twin-column MCSGP process is developed. This is based on a single batch chromatogram, which is selected as the design chromatogram. The derived MCSGP operation is not intended to provide optimal performance, but it provides the target product in the selected fraction of the batch chromatogram, but with higher yield. The design procedure is illustrated for the isolation of the main charge isoform of a monoclonal antibody from Protein A eluate with ion-exchange chromatography. The main charge isoform was obtained at a purity and yield larger than 90%. At the same time process related impurities such as HCP and leached Protein A as well as aggregates were at least equally well removed. Additionally, the impact of several design parameters on the process performance in terms of purity, yield, productivity and buffer consumption is discussed. The obtained results can be used for further fine-tuning of the process parameters so as to improve its performance. Copyright © 2017 Elsevier B.V. All rights reserved.

Solvent systems with n-hexane and/or cyclohexane in countercurrent chromatography--Physico-chemical parameters and their impact on the separation of alkyl hydroxybenzoates.

PubMed

Englert, Michael; Vetter, Walter

2014-05-16

Countercurrent chromatography (CCC) is an efficient preparative separation technique based on the liquid-liquid distribution of compounds between two phases of a biphasic liquid system. The crucial parameter for the successful application is the selection of the solvent system. Especially for nonpolar analytes the selection options are limited. On the search for a suitable solvent system for the separation of an alkyl hydroxybenzoate homologous series, we noted that the substitution of cyclohexane with n-hexane was accompanied with unexpected differences in partitioning coefficients of the individual analytes. In this study, we investigated the influence of the subsequent substitution of n-hexane with cyclohexane in the n-hexane/cyclohexane/tert-butylmethylether/methanol/water solvent system family. Exact phase compositions and polarity, viscosity and density differences were determined to characterize the different mixtures containing n-hexane and/or cyclohexane. Findings were confirmed by performing CCC separations with different mixtures, which led to baseline resolution for positional isomers when increasing the amount of cyclohexane while the resolution between two pairs of structural isomers decreased. With the new methodology described, structurally similar compounds could be resolved by choosing a certain ratio of n-hexane to cyclohexane. Copyright © 2014 Elsevier B.V. All rights reserved.

Passive restriction of blood flow and counter-current heat exchange via lingual retia in the tongue of a neonatal gray whale Eschrichtius robustus (Cetacea, Mysticeti).

PubMed

Ekdale, Eric G; Kienle, Sarah S

2015-04-01

Retia mirabilia play broad roles in cetacean physiology, including thermoregulation during feeding and pressure regulations during diving. Vascular bundles of lingual retia are described within the base of the tongue of a neonatal female gray whale (Eschrichtius robustus). Each rete consists of a central artery surrounded by four to six smaller veins. The retia and constituent vessels decrease in diameter as they extend anteriorly within the hyoglossus muscle from a position anterior to the basihyal cartilage toward the apex of the tongue. The position of the retia embedded in the hyoglossus and the anterior constriction of the vessels differs from reports of similar vascular bundles that were previously identified in gray whales. The retia likely serve as a counter-current heat exchange system to control body temperature during feeding. Cold blood flowing toward the body center within the periarterial veins would accept heat from warm blood in the central artery flowing toward the anterior end of the tongue. Although thermoregulatory systems have been identified within the mouths of a few mysticete species, the distribution of such vascular structures likely is more widespread among baleen whales than has previously been described. © 2015 Wiley Periodicals, Inc.

Separation and purification of four phenolic compounds from persimmon by high-speed counter-current chromatography.

PubMed

Peng, Jinming; Li, Kaikai; Zhu, Wei; Deng, Xiangyi; Li, Chunmei

2018-01-01

An efficient method was established by high-speed counter-current chromatography (HSCCC) for preparation of four phenolic compounds from the depolymerization products of persimmon tannin. Using the two solvent systems of n-hexane/ethyl acetate/water (3:17:20, v/v/v) and ethyl acetate/methanol/water (50:1:50, v/v/v), the preparative isolation was successfully performed by a two-step separation. The yields of one run (150mg crude sample) for gallic acid, methyl gallate, and epigallocatechin-3-gallate-(4β→8, 2β→O→7)-epigallocatechin-3-gallate dimer (A-type EGCG dimer) were 4.7, 44.2 and 5.9mg, respectively. In addition, 4.6mg epicatechin-3-gallate-(4β→8, 2β→O→7)-epicatechin-3-gallate dimer (A-type ECG dimer) was obtained by further preparative high-performance liquid chromatography (prep-HPLC). The purities of these compounds were all above 95.0% and their structures were identified by HPLC/ESI-MS. We found that HSCCC had definite advantages for the preparation of dimeric procyanidins compared with previous methods. Furthermore, it was shown that the four phenolic compounds possessed greater antioxidant activities than Trolox. Copyright © 2017. Published by Elsevier B.V.

Fuel injection staged sectoral combustor for burning low-BTU fuel gas

DOEpatents

Vogt, Robert L.

1981-01-01

A high-temperature combustor for burning low-BTU coal gas in a gas turbine is described. The combustor comprises a plurality of individual combustor chambers. Each combustor chamber has a main burning zone and a pilot burning zone. A pipe for the low-BTU coal gas is connected to the upstream end of the pilot burning zone; this pipe surrounds a liquid fuel source and is in turn surrounded by an air supply pipe; swirling means are provided between the liquid fuel source and the coal gas pipe and between the gas pipe and the air pipe. Additional preheated air is provided by counter-current coolant air in passages formed by a double wall arrangement of the walls of the main burning zone communicating with passages of a double wall arrangement of the pilot burning zone; this preheated air is turned at the upstream end of the pilot burning zone through swirlers to mix with the original gas and air input (and the liquid fuel input when used) to provide more efficient combustion. One or more fuel injection stages (second stages) are provided for direct input of coal gas into the main burning zone. The countercurrent air coolant passages are connected to swirlers surrounding the input from each second stage to provide additional oxidant.

Fuel injection staged sectoral combustor for burning low-BTU fuel gas

DOEpatents

Vogt, Robert L.

1985-02-12

A high-temperature combustor for burning low-BTU coal gas in a gas turbine is described. The combustor comprises a plurality of individual combustor chambers. Each combustor chamber has a main burning zone and a pilot burning zone. A pipe for the low-BTU coal gas is connected to the upstream end of the pilot burning zone: this pipe surrounds a liquid fuel source and is in turn surrounded by an air supply pipe: swirling means are provided between the liquid fuel source and the coal gas pipe and between the gas pipe and the air pipe. Additional preheated air is provided by counter-current coolant air in passages formed by a double wall arrangement of the walls of the main burning zone communicating with passages of a double wall arrangement of the pilot burning zone: this preheated air is turned at the upstream end of the pilot burning zone through swirlers to mix with the original gas and air input (and the liquid fuel input when used) to provide more efficient combustion. One or more fuel injection stages (second stages) are provided for direct input of coal gas into the main burning zone. The countercurrent air coolant passages are connected to swirlers surrounding the input from each second stage to provide additional oxidant.

Microwave-Assisted Extraction and Purification of Arctiin and Arctigenin from Fructus Arctii by High-Speed Countercurrent Chromatography.

PubMed

Lü, Haitao; Sun, Zhaoyun; Shan, Hu; Song, Jiying

2016-03-01

An efficient method for the rapid extraction, separation and purification of bioactive lignans, arctiin and arctigenin, from Fructus arctii by microwave-assisted extraction coupled with high-speed countercurrent chromatography was developed. The optimal extraction conditions of arctiin and arctigenin were evaluated by orthogonal array. Arctigenin could be converted from arctiin by hydrochloric acid hydrolysis. The separations were performed at a preparative scale with two-phase solvents composed of ethyl acetate-ethanol-water (5 : 1 : 5, v/v/v) for arctiin, and n-hexane-ethyl acetate-ethanol-water (4 : 4 : 3 : 4, v/v/v/v) for arctigenin. From 500 mg of crude extract sample, 122.3 mg of arctiin and 45.7 mg of arctigenin were obtained with the purity of 98.46 and 96.57%, and the recovery of 94.3 and 81.6%, respectively. Their structures were determined by comparison with the high-performance liquid chromatography retention time of standard substance as well as UV, FT-IR, electrospray ion source (ESI)-MS, (1)H-NMR and (13)C-NMR spectrum. According to the antioxidant activity assay, arctigenin had stronger 1,1-diphenyl-2-picrylhydrazyl free radicals scavenging activity. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

A simplified bioprocess for human alpha-fetoprotein production from inclusion bodies.

PubMed

Leong, Susanna S J; Middelberg, Anton P J

2007-05-01

A simple and effective Escherichia coli (E. coli) bioprocess is demonstrated for the preparation of recombinant human alpha-fetoprotein (rhAFP), a pharmaceutically promising protein that has important immunomodulatory functions. The new rhAFP process employs only unit operations that are easy to scale and validate, and reduces the complexity embedded in existing inclusion body processing methods. A key requirement in the establishment of this process was the attainment of high purity rhAFP prior to protein refolding because (i) rhAFP binds easily to hydrophobic contaminants once refolded, and (ii) rhAFP aggregates during renaturation, in a contaminant- dependent way. In this work, direct protein extraction from cell suspension was coupled with a DNA precipitation-centrifugation step prior to purification using two simple chromatographic steps. Refolding was conducted using a single-step, redox-optimized dilution refolding protocol, with refolding success determined by reversed phase HPLC analysis, ELISA, and circular dichroism spectroscopy. Quantitation of DNA and protein contaminant loads after each unit operation showed that contaminant levels were reduced to levels comparable to traditional flowsheets. Protein microchemical modification due to carbamylation in this urea-based process was identified and minimized, yielding a final refolded and purified product that was significantly purified from carbamylated variants. Importantly, this work conclusively demonstrates, for the first time, that a chemical extraction process can substitute the more complex traditional inclusion body processing flowsheet, without compromising product purity and yield. This highly intensified and simplified process is expected to be of general utility for the preparation of other therapeutic candidates expressed as inclusion bodies. (c) 2006 Wiley Periodicals, Inc.

Choice of optimal working fluid for binary power plants at extremely low temperature brine

NASA Astrophysics Data System (ADS)

Tomarov, G. V.; Shipkov, A. A.; Sorokina, E. V.

2016-12-01

The geothermal energy development problems based on using binary power plants utilizing lowpotential geothermal resources are considered. It is shown that one of the possible ways of increasing the efficiency of heat utilization of geothermal brine in a wide temperature range is the use of multistage power systems with series-connected binary power plants based on incremental primary energy conversion. Some practically significant results of design-analytical investigations of physicochemical properties of various organic substances and their influence on the main parameters of the flowsheet and the technical and operational characteristics of heat-mechanical and heat-exchange equipment for binary power plant operating on extremely-low temperature geothermal brine (70°C) are presented. The calculation results of geothermal brine specific flow rate, capacity (net), and other operation characteristics of binary power plants with the capacity of 2.5 MW at using various organic substances are a practical interest. It is shown that the working fluid selection significantly influences on the parameters of the flowsheet and the operational characteristics of the binary power plant, and the problem of selection of working fluid is in the search for compromise based on the priorities in the field of efficiency, safety, and ecology criteria of a binary power plant. It is proposed in the investigations on the working fluid selection of the binary plant to use the plotting method of multiaxis complex diagrams of relative parameters and characteristic of binary power plants. Some examples of plotting and analyzing these diagrams intended to choose the working fluid provided that the efficiency of geothermal brine is taken as main priority.

Using a 3D CAD plant model to simplify process hazard reviews

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

Tolpa, G.

A Hazard and Operability (HAZOP) review is a formal predictive procedure used to identify potential hazard and operability problems associated with certain processes and facilities. The HAZOP procedure takes place several times during the life cycle of the facility. Replacing plastic models, layout and detail drawings with a 3D CAD electronic model, provides access to process safety information and a detailed level of plant topology that approaches the visualization capability of the imagination. This paper describes the process that is used for adding the use of a 3D CAD model to flowsheets and proven computer programs for the conduct ofmore » hazard and operability reviews. Using flowsheets and study nodes as a road map for the review the need for layout and other detail drawings is all but eliminated. Using the 3D CAD model again for a post-P and ID HAZOP supports conformance to layout and safety requirements, provides superior visualization of the plant configuration and preserves the owners equity in the design. The response from the review teams are overwhelmingly in favor of this type of review over a review that uses only drawings. Over the long term the plant model serves more than just process hazards analysis. Ongoing use of the model can satisfy the required access to process safety information, OHSA documentation and other legal requirements. In this paper extensive instructions address the logic for the process hazards analysis and the preparation required to assist anyone who wishes to add the use of a 3D model to their review.« less

[Process strategy for ethanol production from lignocellulose feedstock under extremely low water usage and high solids loading conditions].

PubMed

Zhang, Jian; Chu, Deqiang; Yu, Zhanchun; Zhang, Xiaoxi; Deng, Hongbo; Wang, Xiusheng; Zhu, Zhinan; Zhang, Huaiqing; Dai, Gance; Bao, Jie

2010-07-01

The massive water and steam are consumed in the production of cellulose ethanol, which correspondingly results in the significant increase of energy cost, waster water discharge and production cost as well. In this study, the process strategy under extremely low water usage and high solids loading of corn stover was investigated experimentally and computationally. The novel pretreatment technology with zero waste water discharge was developed; in which a unique biodetoxification method using a kerosene fungus strain Amorphotheca resinae ZN1 to degrade the lignocellulose derived inhibitors was applied. With high solids loading of pretreated corn stover, high ethanol titer was achieved in the simultaneous saccharification and fermentation process, and the scale-up principles were studied. Furthermore, the flowsheet simulation of the whole process was carried out with the Aspen plus based physical database, and the integrated process developed was tested in the biorefinery mini-plant. Finally, the core technologies were applied in the cellulose ethanol demonstration plant, which paved a way for the establishment of an energy saving and environment friendly technology of lignocellulose biotransformation with industry application potential.

Circulation Plasma Centrifuge with Product Flow

NASA Astrophysics Data System (ADS)

Borisevich, V. D.; Potanin, E. P.

2018-05-01

We have analyzed the isotope separation in a high-frequency plasma circulating centrifuge operating with a product flow. The rotation of a weakly ionized plasma is ensured by a rotating magnetic field, while the countercurrent flow (circulation) is produced by a traveling magnetic field. We have calculated the dependences of the enrichment factor and the separative power of the centrifuge on a product flow. The optimal characteristics of the separation unit have been determined.

Experimental investigation of heat transfer characteristics of guar-based polymer solutions and gels

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

Azouz, I.; Vinod, P.S.; Shah, S.N.

1996-12-31

An experimental investigation of the heat transfer characteristics of hydraulic fracturing fluids was conducted at the Fracturing Fluid Characterization Facility (FFCF) of the University of Oklahoma. The facility is equipped with a high pressure fracture simulator, coiled tubing fluid pre-conditioning system, and a full-scale, counter-current, double pipe heat exchanger. The fluids investigated include non-crosslinked and borate-crosslinked guar gum and hydroxypropyl guar (HPG). Results were also obtained for water and were used as a basis for comparison. The effects of flow rate, operating temperature, pH, and various levels of shear pre-conditioning, on the heat transfer behavior of the test fluids weremore » investigated. Results show a significant difference between the heat transfer coefficient of the pure solvent (water) and those of the polymer solutions tested. While all polymer solutions tested exhibited lower heat transfer coefficients than that of the pure solvent, crosslinking appears to enhance the heat transfer characteristics of the polymer fluids. It was also observed that shear preconditioning does not seem to have a significant effect on the heat transfer coefficient of the crosslinked gels. These findings are of great interest to the industry, especially to the petroleum industry where these fluids are commonly used during hydraulic fracturing of hydrocarbon reservoirs.« less

PROCESS DEVELOPMENT QUARTERLY REPORT. II. PILOT PLANT WORK

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

Kuhlman, N. ed.

1957-05-01

Progress is reported on the gross solubility of U in digestions of Mallinokrodt feed materials, studies of variables affecting U purity in a TBP hexane extraction cycle, low-acid flowsheet for TBP--hexane extraction process based on a 440 g U/liter in lM HNO/sub 3/ digest liquor, hacking studies in the pilot plant pumperdecanter system, recovery of U from residues from the dingot process, lowering the H level in dingot metal, forging of dingot bar stock, dingot extrusion, fubrication of UO/sub 2/ fuel elements, and the determination of H content of derby and ingot metal. (W.L.H.)

Countercurrent distribution of biological cells

NASA Technical Reports Server (NTRS)

Brooks, D. E.

1982-01-01

Detailed physiochemical studies of dextran/poly(ethylene glycol) (PEG) two phase systems were carried out to characterize and provide understanding of the properties of the systems which determine cell partition and the electrophoretic behavior of phase drops responsible for electric field driven phase separation. A detailed study of the electrostatic and electrokinetic potentials developed in these systems was carried out. The salt partition was examined both in phase systems and with pure polymer solutions via equilibrium dialysis and mechanism of sulfate, chloride and phosphate partition shown to be exclusion by PEG rather than binding by dextran. Salt partition was shown to have a strong effect on the polymer compositions of the phases as well, an effect which produces large changes in the interfacial tension between them. These effects were characterized and the interfacial tension shown to obey a power law with respect to its dependence on the length of the tie line describing the system composition on a phase diagram. The electrostatic potential differences measured via salt bridges were shown to obey thermodynamic predictions. The electrophoretic mobilities measured were utilized to provide a partial test of Levine's incomplete theory of phase drop electrophoresis. The data were consistent with Levine's expression over a limited range of the variables tested.

Phase-field simulation of counter-current spontaneous imbibition in a fractured heterogeneous porous medium

NASA Astrophysics Data System (ADS)

Rokhforouz, M. R.; Akhlaghi Amiri, H. A.

2017-06-01

Spontaneous imbibition is well-known to be one of the most effective processes of oil recovery in fractured reservoirs. However, the detailed pore-scale mechanisms of the counter-current imbibition process and the effects of different fluid/rock parameters on this phenomenon have not yet been deeply addressed. This work presents the results of a new pore-level numerical study of counter-current spontaneous imbibition, using coupled Cahn-Hilliard phase field and Navier-Stokes equations, solved by a finite element method. A 2D fractured medium was constructed consisting of a nonhomogeneous porous matrix, in which the grains were represented by an equilateral triangular array of circles with different sizes and initially saturated with oil, and a fracture, adjacent to the matrix, initially saturated with water and supported by low rate water inflow. Through invasion of water into the matrix, oil drops were expelled one by one from the matrix to the fracture, and in the matrix, water progressed by forming capillary fingerings, with characteristics corresponding to the experimental observations. The effects of wettability, viscosity ratio, and interfacial tension were investigated. In strongly water-wet matrix, with grain contact angles of θ < π/8, different micro-scale mechanisms were successfully captured, including oil film thinning and rupture, fluids' contact line movement, water bridging, and oil drop detachment. It was notified that there was a specific grain contact angle for this simulated model, θ = π/4, above it, matrix oil recovery was negligible by imbibition, while below it, the imbibition rate and oil recovery were significantly increased by decreasing the contact angle. In simulated mixed wet models, water, coming from the fracture, just invaded the neighboring water-wet grains; the water front was stopped moving as it met the oil-wet grains or wide pores/throats. Increasing water-oil interfacial tension, in the range of 0.005-0.05 N/m, resulted in both higher rate of imbibition and higher ultimate oil recovery. Changing the water-oil viscosity ratio (M), in the range of 0.1-10, had a negligible effect on the imbibition rate, while due to co-effects of capillary fingering and viscous mobility ratio, the model with M = 1 had relatively higher ultimate oil recovery.

Experimental validation of a Lyapunov-based controller for the plasma safety factor and plasma pressure in the TCV tokamak

NASA Astrophysics Data System (ADS)

Mavkov, B.; Witrant, E.; Prieur, C.; Maljaars, E.; Felici, F.; Sauter, O.; the TCV-Team

2018-05-01

In this paper, model-based closed-loop algorithms are derived for distributed control of the inverse of the safety factor profile and the plasma pressure parameter β of the TCV tokamak. The simultaneous control of the two plasma quantities is performed by combining two different control methods. The control design of the plasma safety factor is based on an infinite-dimensional setting using Lyapunov analysis for partial differential equations, while the control of the plasma pressure parameter is designed using control techniques for single-input and single-output systems. The performance and robustness of the proposed controller is analyzed in simulations using the fast plasma transport simulator RAPTOR. The control is then implemented and tested in experiments in TCV L-mode discharges using the RAPTOR model predicted estimates for the q-profile. The distributed control in TCV is performed using one co-current and one counter-current electron cyclotron heating actuation.

Simulation-Assisted Evaluation of Grinding Circuit Flowsheet Design Alternatives: Aghdarreh Gold Ore Processing Plant / Ocena Alternatywnych Schematów Technologicznych Procesu Rozdrabniania W Zakładach Przeróbki Rud Złota W Aghdarreh, Z Wykorzystaniem Metod Symulacji

NASA Astrophysics Data System (ADS)

Farzanegan, A.; Ghalaei, A. Ebtedaei

2015-03-01

The run of mine ore from Aghdarreh gold mine must be comminuted to achieve the desired degree of liberation of gold particles. Currently, comminution circuits include a single-stage crushing using a jaw crusher and a single-stage grinding using a Semi-Autogenous Grinding (SAG) mill in closed circuit with a hydrocyclone package. The gold extraction is done by leaching process using cyanidation method through a series of stirred tanks. In this research, an optimization study of Aghdarreh plant grinding circuit performance was done to lower the product particle size (P80) from 70 μm to approximately 40 μm by maintaining current throughput using modeling and simulation approach. After two sampling campaigns from grinding circuit, particle size distribution data were balanced using NorBal software. The first and second data sets obtained from the two sampling campaigns were used to calibrate necessary models and validate them prior to performing simulation trials using MODSIM software. Computer simulations were performed to assess performance of two proposed new circuit flowsheets. The first proposed flowsheet consists of existing SAG mill circuit and a new proposed ball mill in closed circuit with a new second hydrocyclone package. The second proposed flowsheet consists of existing SAG mill circuit followed by a new proposed ball mill in closed circuit with the existing hydrocyclone package. In all simulations, SAGT, CYCL and MILL models were selected to simulate SAG mill, Hydrocyclone packages and ball mill units. SAGT and MILL models both are based on population balance model of grinding process. CYCL model is based on Plitt's empirical model of classification process in hydrocyclone units. It was shown that P80 can be reduced to about 40 μm and 42 μm for the first and second proposed circuits, respectively. Based on capital and operational costs, it can be concluded that the second proposed circuit is a more suitable option for plant grinding flowsheet modification. Surowy urobek z kopalni rud złota Aghdarreh musi najpierw zostać poddany rozdrobnieniu, aby zapewnić efektywniejsze uwalnianie cząsteczek złota. W chwili obecnej obiegi rozdrabniania obejmują kruszenie jednostopniowe z wykorzystaniem kruszarek szczękowych oraz kruszenie jednostopniowe z użyciem kruszarek półautomatycznych w obiegu zamkniętym z hydrocyklonem. Odzysk złota odbywa się przy zastosowaniu procesu ługowania, z zastosowaniem metody cyjankowej w szeregu mieszalników. W pracy tej przeprowadzono optymalizację procesu rozdrabniania rud w zakładach przeróbczych Aghdarreh prowadzonego w celu zmniejszenia rozmiarów uzyskiwanych cząsteczek złota (Ps0) z 70 μm do ok. 40 μm poprzez zapewnienie ciągłości procesu, z wykorzystaniem metod modelowania i symulacji. Na podstawie dwóch zestawów próbek z ciągu technologicznego rozdrabniania, rozkłady wielkości cząstek zostały statystycznie zrównoważone z wykorzystaniem oprogramowania NorBal. Pierwszy i drugi zbiór danych otrzymanych na podstawie dwóch zestawów próbek wykorzystany został do kalibracji i walidacji modeli, przed przystąpieniem do właściwych badań symulacyjnych z użyciem oprogramowania MODSIM. Symulacje komputerowe przeprowadzono w celu oceny wydajności dwóch proponowanych ciągów technologicznych. Pierwszy ciąg obejmuje istniejące kruszarki półautomatyczne i nowo proponowaną kruszarkę kulową pracującą w obiegu zamkniętym z hydrocyklonem. Drugi rozważany ciąg stanowi istniejąca kruszarka półautomatyczna, następnie proponowana kruszarka kulowa pracująca w obiegu zamkniętym z istniejącym hydrocyklonem. We wszystkich symulacjach bazowano na modelach SAGT, CYCL i MILL do symulacji pracy kruszarek półautomatycznych, pakietu hydrocyklonu oraz pojedynczych kruszarek. Modele SAGT i MILL oparte są na modelu zrównoważonej populacji w procesie rozdrabniania. Model CYCL opiera się na empirycznym modelu klasyfikacji Plitta zastosowanym do hydrocyklonów. Wykazano, że rozmiar cząstek zmniejszony został odpowiednio do 40 μm i 42 μm dla pierwszego i drugiego analizowanego obiegu. Uwzględniając nakłady kapitałowe oraz koszty operacyjne, wyciągnąć można więc wniosek, ze drugi proponowany układ jest korzystniejszą opcją modyfikacji istniejącego ciągu technologicznego rozdrabniania.

Simulated countercurrent moving bed chromatographic reactor and method for use thereof

DOEpatents

Carr, Robert W.; Tonkovich, Anna Lee Y.

2001-01-01

A method and apparatus for continuously reacting a feed gas to form a product and separating the product from unreacted feed gas is provided. The apparatus includes a plurality of compartments and means for connecting the compartments in a series, with the last compartment in the series being connected to the first compartment in the series to provide a closed loop. Each compartment may include an upstream reaction zone and a downstream separation zone.

Waste heat driven absorption refrigeration process and system

DOEpatents

Wilkinson, William H.

1982-01-01

Absorption cycle refrigeration processes and systems are provided which are driven by the sensible waste heat available from industrial processes and other sources. Systems are disclosed which provide a chilled water output which can be used for comfort conditioning or the like which utilize heat from sensible waste heat sources at temperatures of less than 170.degree. F. Countercurrent flow equipment is also provided to increase the efficiency of the systems and increase the utilization of available heat.

Wire-packed heat exchangers for dilution refrigerators.

PubMed

Polturak, E; Rappaport, M; Rosenbaum, R

1978-03-01

Very simple wire-packed step heat exchangers for dilution refrigerators are described. No sintering is used in fabrication. Flow impedances and thermal resistance between the liquid and the copper wires are low. A refrigerator with five wire-packed heat exchangers in addition to a countercurrent heat exchanger attains a temperature of 11.4 mK with a single mixing chamber and 6.1 mK with two mixing chambers. High cooling power is achieved at modest (3)He circulation rates.

Carbon wastewater treatment process

NASA Technical Reports Server (NTRS)

Humphrey, M. F.; Simmons, G. M.; Dowler, W. L.

1974-01-01

A new powdered-carbon treatment process is being developed for the elimination of the present problems, associated with the disposal of biologically active sewage waste solids, and with water reuse. This counter-current flow process produces an activated carbon, which is obtained from the pyrolysis of the sewage solids, and utilizes this material to remove the adulterating materials from the water. Additional advantages of the process are the elimination of odors, the removal of heavy metals, and the potential for energy conservation.

Screening, separation, and evaluation of xanthine oxidase inhibitors from Paeonia lactiflora using chromatography combined with a multi-mode microplate reader.

PubMed

Wang, Jing; Shi, Dongfang; Zheng, Meizhu; Ma, Bing; Cui, Jing; Liu, Chunming; Liu, Chengyu

2017-11-01

Natural products have become one of the most important resources for discovering novel xanthine oxidase inhibitors, which are commonly employed in the treatment of hyperuricemia and gout. However, to date, few reports exist regarding the use of monoterpene glycosides as xanthine oxidase inhibitors. Thus, we herein report the use of ultrafiltration coupled with liquid chromatography in the screening of monoterpene glycoside xanthine oxidase inhibitors from the extract of Paeonia lactiflora (P. lactiflora), and both high-performance counter-current chromatography and medium-pressure liquid chromatography were employed to separate the main constituents. Furthermore, the xanthine oxidase inhibitory activities and the mechanisms of inhibition of the isolated compounds were evaluated using a multi-mode microplate reader by Molecular Devices. As a result, three monoterpene glycosides were separated by combined high-performance counter-current chromatography and medium-pressure liquid chromatography in purities of 90.4, 98.0, and 86.3%, as determined by liquid chromatography. These three compounds were identified as albiflorin, paeoniflorin, and 1-O-β-ᴅ-glucopyranosyl-8-O-benzoylpaeonisuffrone by electrospray ionization tandem mass spectrometry, and albiflorin and paeoniflorin were screened as potential xanthine oxidase inhibitors by ultrafiltration with liquid chromatography. The evaluation results of xanthine oxidase inhibitory activity corresponded with the screening results, as only albiflorin and paeoniflorin exhibited xanthine oxidase inhibitory activity. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Isolation and purification of series bioactive components from Hypericum perforatum L. by counter-current chromatography.

PubMed

Cao, Xueli; Wang, Qiaoe; Li, Yan; Bai, Ge; Ren, Hong; Xu, Chunming; Ito, Yoichiro

2011-03-01

Counter-current chromatography (CCC) combined with pre-separation by ultrasonic solvent extraction was successively used for the separation of series bioactive compounds from the crude extract of Hypericum perforatum L. The petroleum ether extract was separated by the solvent system of n-heptane-methanol-acetonitrile (1.5:0.5:0.5, v/v) and n-heptane-methanol (1.5:1, v/v) in gradient elution, yielding a phloroglucinol compound, hyperforin with HPLC purity over 98%. The ethyl acetate extract was separated by using the solvent system composed of hexane-ethyl acetate-methanol-water (1:1:1:1 and 1:3:1:3, v/v) in gradient through both reverse phase and normal phase elution mode, yielding a naphthodianthrone compound, hypericin with HPLC purity about 95%. The n-butanol extract was separated with the solvent system composed of n-butanol-ethyl acetate-water (1:4:5 and 1.5:3.5:5, v/v) in elution and back-extrusion mode, yielding two of flavones, rutin and hyperoside, with HPLC purity over 95%. HPLC-MS, reference sample and UV spectrum were selectively used in separation to search for target compounds from HPLC-DAD profiles of different sub-extracts. The structures of isolated compounds were further identified by ESI-MS, ¹HNMR and ¹³CNMR. Copyright © 2011 Elsevier B.V. All rights reserved.

Energy-efficient membrane separations in the sweetener industry. Final report

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

Ray, R.J.

1986-02-14

Objective was to investigate the use of membrane processes as energy-efficient alternatives to certain conventional separation processes now in use in the corn-sweetener industry. Three applications of membranes were studied during the program: the concentration of corn steep water by reverse osmosis; the concentration of dilute wastes, called ''sweetwater,'' by a combination of reverse osmosis and countercurrent reverse osmosis; and the enrichment of corn syrup in fructose by a process involving selective complexation of fructose by membrane filtration. Laboratory experiments were conducted for all three applications, and the results were used to conduct technical and economic analyses of the process.more » Calculations indicate that the use of reverse osmosis in combination with conventional mechanical-vapor-recompression evaporation to concentrate steep water, offers savings of a factor of 2.5 in capital costs and a factor of 4.5 in operating costs over currently used evaporation alone. In the concentration of sweetwater by reverse osmosis and countercurrent reverse osmosis, capital costs would be about the same as those for evaporation, but operating costs would only be about one-half those of evaporation. For the fructose-enrichment scheme, preliminary results indicate that the savings in energy alone for the membrane process would be about $0.01/lb of sweetener produced by the process, or about $20 million annually, for the corn-sweetener industry.« less

Use of limonene in countercurrent chromatography: a green alkane substitute.

PubMed

Faure, Karine; Bouju, Elodie; Suchet, Pauline; Berthod, Alain

2013-05-07

Counter-current chromatography (CCC) is a preparative separation technique working with the two liquid phases of a biphasic liquid system. One phase is used as the mobile phase when the other, the stationary phase, is held in place by centrifugal fields. Limonene is a biorenewable cycloterpene solvent coming from orange peel waste. It was evaluated as a possible substitute for heptane in CCC separations. The limonene/methanol/water and heptane/methanol/water phase diagrams are very similar at room temperature. The double bonds of the limonene molecule allows for possible π-π interactions with solutes rendering limonene slightly more polar than heptane giving small differences in solute partition coefficients in the two systems. The 24% higher limonene density is a difference with heptane that has major consequences in CCC. The polar and apolar phases of the limonene/methanol/water 10/9/1 v/v have -0.025 g/cm(3) density difference (lower limonene phase) compared to +0.132 g/cm(3) with heptane (upper heptane phase). This precludes the use of this limonene system with hydrodynamic CCC columns that need significant density difference to retain a liquid stationary phase. It is an advantage with hydrostatic CCC columns because density difference is related to the working pressure drop: limonene allows one to work with high centrifugal fields and moderate pressure drop. Limonene has the capability to be a "green" alternative to petroleum-based solvents in CCC applications.

Hepatoprotective Flavonoids in Opuntia ficus-indica Fruits by Reducing Oxidative Stress in Primary Rat Hepatocytes

PubMed Central

Kim, Jung Wha; Kim, Tae Bum; Kim, Hyun Woo; Park, Sang Wook; Kim, Hong Pyo; Sung, Sang Hyun

2017-01-01

Background: Liver disorder was associated with alcohol consumption caused by hepatic cellular damages. Opuntia ficus-indica fruit extracts (OFIEs), which contain betalain pigments and polyphenols including flavonoids, have been introduced as reducing hangover symptoms and liver protective activity. Objective: To evaluate hepatoprotective activity of OFIEs and isolated compounds by high-speed countercurrent chromatography (HSCCC). Materials and Methods: The extract of O. ficus-indica fruits was fractionated into methylene chloride and n-butanol. The n-butanol fraction was isolated by HSCCC separation (methylene chloride-methanol-n-butanol-water, 5:4:3:5, v/v/v/v). The hepatoprotective activity of OFIEs and isolated compounds was evaluated on rat primary hepatocytes against ethanol-induced toxicity. Antioxidative parameters such as glutathione reductase and glutathione peroxidase (GSH-Px) enzymes and the GSH content were measured. Results: Two flavonoids, quercetin 3-O-methyl ester (1) and (+)-taxifolin, and two flavonoid glycosides, isorhamnetin 3-O-β-d-glucoside (3) and narcissin (4), were isolated from the n-butanol fraction by HSCCC separation. Among them, compound 2 significantly protected rat primary hepatocytes against ethanol exposure by preserving antioxidative properties of GR and GSH-Px. Conclusions: OFIEs and (+)-taxifolin were suggested to reduce hepatic damage by alcoholic oxidative stress. SUMMARY Hepatoprotective Flavonoids were isolated from Opuntia ficus-indica by high -speed countercurrent chromatography (HSCCC). PMID:28839374

Countercurrent chromatography separation of saponins by skeleton type from Ampelozizyphus amazonicus for off-line ultra-high-performance liquid chromatography/high resolution accurate mass spectrometry analysis and characterisation.

PubMed

de Souza Figueiredo, Fabiana; Celano, Rita; de Sousa Silva, Danila; das Neves Costa, Fernanda; Hewitson, Peter; Ignatova, Svetlana; Piccinelli, Anna Lisa; Rastrelli, Luca; Guimarães Leitão, Suzana; Guimarães Leitão, Gilda

2017-01-20

Ampelozizyphus amazonicus Ducke (Rhamnaceae), a medicinal plant used to prevent malaria, is a climbing shrub, native to the Amazonian region, with jujubogenin glycoside saponins as main compounds. The crude extract of this plant is too complex for any kind of structural identification, and HPLC separation was not sufficient to resolve this issue. Therefore, the aim of this work was to obtain saponin enriched fractions from the bark ethanol extract by countercurrent chromatography (CCC) for further isolation and identification/characterisation of the major saponins by HPLC and MS. The butanol extract was fractionated by CCC with hexane - ethyl acetate - butanol - ethanol - water (1:6:1:1:6; v/v) solvent system yielding 4 group fractions. The collected fractions were analysed by UHPLC-HRMS (ultra-high-performance liquid chromatography/high resolution accurate mass spectrometry) and MS n . Group 1 presented mainly oleane type saponins, and group 3 showed mainly jujubogenin glycosides, keto-dammarane type triterpene saponins and saponins with C 31 skeleton. Thus, CCC separated saponins from the butanol-rich extract by skeleton type. A further purification of group 3 by CCC (ethyl acetate - ethanol - water (1:0.2:1; v/v)) and HPLC-RI was performed in order to obtain these unusual aglycones in pure form. Copyright © 2016 Elsevier B.V. All rights reserved.

The Secretion of Oxygen into the Swim-Bladder of Fish

PubMed Central

Wittenberg, Jonathan B.; Schwend, Mary J.; Wittenberg, Beatrice A.

1964-01-01

The secretion of carbon dioxide accompanying the secretion of oxygen into the swim-bladder of the bluefish is examined in order to distinguish among several theories which have been proposed to describe the operation of the rete mirabile, a vascular countercurrent exchange organ. Carbon dioxide may comprise 27 per cent of the gas secreted, corresponding to a partial pressure of 275 mm Hg. This is greater than the partial pressure that would be generated by acidifying arterial blood (about 55 mm Hg). The rate of secretion is very much greater than the probable rate of metabolic formation of carbon dioxide in the gas-secreting complex. It is approximately equivalent to the probable rate of glycolytic generation of lactic acid in the gas gland. It is concluded that carbon dioxide brought into the swim-bladder is liberated from blood by the addition of lactic acid. The rete mirabile must act to multiply the primary partial pressure of carbon dioxide produced by acidification of the blood. The function of the rete mirabile as a countercurrent multiplier has been proposed by Kuhn, W., Ramel, A., Kuhn, H. J., and Marti, E., Experientia, 1963, 19, 497. Our findings provide strong support for their theory. The unique structure of the gas-secreting complex of the swim-bladder of the bluefish, Pomatomus saltatrix L., is described. PMID:14225261

THE SECRETION OF OXYGEN INTO THE SWIM-BLADDER OF FISH. 3. THE ROLE OF CARBON DIOXIDE.

PubMed

WITTENBERG, J B; SCHWEND, M J; WITTENBERG, B A

1964-11-01

The secretion of carbon dioxide accompanying the secretion of oxygen into the swim-bladder of the bluefish is examined in order to distinguish among several theories which have been proposed to describe the operation of the rete mirabile, a vascular countercurrent exchange organ. Carbon dioxide may comprise 27 per cent of the gas secreted, corresponding to a partial pressure of 275 mm Hg. This is greater than the partial pressure that would be generated by acidifying arterial blood (about 55 mm Hg). The rate of secretion is very much greater than the probable rate of metabolic formation of carbon dioxide in the gas-secreting complex. It is approximately equivalent to the probable rate of glycolytic generation of lactic acid in the gas gland. It is concluded that carbon dioxide brought into the swim-bladder is liberated from blood by the addition of lactic acid. The rete mirabile must act to multiply the primary partial pressure of carbon dioxide produced by acidification of the blood. The function of the rete mirabile as a countercurrent multiplier has been proposed by Kuhn, W., Ramel, A., Kuhn, H. J., and Marti, E., Experientia, 1963, 19, 497. Our findings provide strong support for their theory. The unique structure of the gas-secreting complex of the swim-bladder of the bluefish, Pomatomus saltatrix L., is described.

Efficient counter-current chromatographic isolation and structural identification of two new cinnamic acids from Echinacea purpurea.

PubMed

Lu, Ying; Li, JiaYin; Li, MiLu; Hu, Xia; Tan, Jun; Liu, Zhong Hua

2012-10-01

Two new cinnamic acids, 2-O-caffeoyl-3-O-isoferuloyltartaric (3), and 2, 3-di-O-isoferuloyltartaric acid (5), along with three known caffeic acids, cichoric acid (1), 2-O-caffeoyl-3-O-feruloyltartaric acid (2) and 2-O-caffeoyl-3-O-p-coumaroyltartaric acid (4), have been successfully isolated and purified from Echinacea purpurea. In this study, we investigated an efficient method for the preparative isolation and purification of cinnamic acids from E. purpurea by high-speed counter-current chromatography (HSCCC). The separation was performed using a two-phase solvent composed of n-hexane-ethyl-acetate-methanol-0.5% aqueous acetic acid (1:3:1:4, v/v). The upper phase was used as the stationary phase and the lower phase as the mobile phase, with a flow rate of 1.6 mL/min. From 250 mg of crude extracts, 65.1 mg of 1, 8.3 mg of 2, 4.0 mg of 3, 4.5 mg of 4, and 4.3 mg of 5 were isolated in one-step, with purities of 98.5%, 97.7%, 94.6%, 94.3%, and 98.6%, respectively, as evaluated by HPLC-DAD. The chemical structures were identified by electro spray ionization mass spectrometry (ESI-MS) and one- and two-dimensional NMR spectra. HSCCC was very efficient for the separation and purification of the cinnamic acids from

Preparative separation of phenolic compounds from Halimodendron halodendron by high-speed counter-current chromatography.

PubMed

Wang, Jihua; Gao, Haifeng; Zhao, Jianglin; Wang, Qi; Zhou, Ligang; Han, Jianguo; Yu, Zhu; Yang, Fuyu

2010-08-31

Three phenolic compounds, p-hydroxybenzoic acid (1), isorhamnetin-3-O-β-D-rutinoside (2), and 3,3'-di-O-methylquercetin (5), along with a phenolic mixture were successfully separated from the ethyl acetate crude extract of Halimodendron halodendron by high-speed counter-current chromatography (HSCCC) with chloroform-methanol-water-acetic acid (4:3:2:0.05, v/v) as the two-phase solvent system. The phenolic mixture from HSCCC was further separated by preparative HPLC and purified by Sephadex LH-20 to afford quercetin (3) and 3-O-methylquercetin (4). Seven hundred mg of ethyl acetate crude extract was separated by HSCCC to obtain six fractions which were then analyzed by high performance liquid chromatography (HPLC). The HSCCC separation obtained total of 80 mg of the mixture of quercetin (3) and 3-O-methylquercetin (4) (26.43% and 71.89%, respectively) in fraction 2, 14 mg of 3,3'-di-O-methylquercetin (5) at 95.14% of purity in fraction 3, 15 mg of p-hydroxybenzoic acid (1) at 92.83% of purity in fraction 5, 12 mg of isorhamnetin-3-O-β-D-rutinoside (2) at 97.99% of purity in fraction 6. This is the first time these phenolic compounds have been obtained from H. halodendron, and their chemical structures identified by means of physicochemical and spectrometric analysis.

Application and comparison of high performance liquid chromatography and high speed counter-current chromatography in enantioseparation of (±)-2-phenylpropionic acid.

PubMed

Tong, Shengqiang; Zheng, Ye; Yan, Jizhong

2013-03-15

High performance liquid chromatography (HPLC) and high speed counter-current chromatography (HSCCC) were applied and compared in enantioseparation of 2-phenylpropionic acid (2-PPA) when hydroxypropyl-β-cyclodextrin (HP-β-CD) was used as chiral mobile phase additive. For HPLC, the enantioseparation was achieved on ODS C(18) reverse phase column and the mobile phase was 25 mmol L(-1) HP-β-CD aqueous buffer solution (pH 4.0, adjusted with triethylamine): methanol: glacial acetic acid (85:15:0.5 (v/v/v)). For HSCCC, the two-phase solvent system was composed of n-hexane-ethyl acetate-0.1 mol L(-1) phosphate buffer solution pH2.67 (5:5:10 for isocratic elution and 8:2:10 for recycling elution (v/v/v)) added with 0.1 mol L(-1) HP-β-CD. The key parameters, such as a substitution degree of HP-β-CD, the concentration of HP-β-CD, pH value of the aqueous phase and the temperature were optimized for both separation methods. Using the optimum conditions a complete HSCCC enantioseparation of 40 mg of 2-propylpropionic acid in a recycling elution mode gave 15-18 mg of (+)-2-PPA and (-)-2-PPA enantiomers with 95-98% purity and 85-93% recovery. Copyright © 2013 Elsevier B.V. All rights reserved.

More than 170 polyunsaturated tocopherol-related compounds in a vitamin E capsule: Countercurrent chromatographic enrichment, gas chromatography/mass spectrometry analysis and preliminary identification of the potential artefacts.

PubMed

Hammann, Simon; Kröpfl, Alexander; Vetter, Walter

2016-12-09

Tocopherols and tocotrienols (usually summed up as vitamin E) are a class of structurally related natural antioxidants. Commonly, only some of the eight classic representatives (four tocopherols and four tocotrienols) are found with varied composition in food. In this study we fractionated 230mg oil from commercial vitamin E supplement capsules by countercurrent chromatography (CCC) and subsequent analysis by gas chromatography with mass spectrometry (GC/MS) of silylated CCC fractions showed that these eight isomers represented only about 70% of total tocopherol compounds. Detailed analysis enabled the detection of 161T 3 isomers (α-, γ- and δ-T 3 ) along with 18 tetra- and several penta-unsaturated isomers (tocools), two tocomonoenol isomers, and several degradation products with shorter isoprenoid side chain (apo-tocools). Altogether, over 170 tocool compounds, most likely artefacts which originated from an inappropriate oil refining process were described in this study. Silver ion high performance liquid chromatography (Ag + -HPLC) was used to separate one fraction rich in γ-T 3 into four peaks each consisting of at least five peaks according to GC/MS. About ten γ-T 3 isomers were also detected in rice bran oils from one producer bought retail in Germany. Copyright © 2016 Elsevier B.V. All rights reserved.

Isolation and purification of series bioactive components from Hypericum Perforatum L. by high-speed counter-current chromatography

PubMed Central

Cao, Xueli; Wang, Qiaoe; Li, Yan; Bai, Ge; Ren, Hong; Ito, Yiochiro

2011-01-01

High-speed counter-current chromatography (HSCCC) combined with pre-separation by ultrasonic solvent extraction was successively used for the separation of series bioactive compounds from the crude extract of Hypericum perforatum L. The petroleum ether extract was separated by the solvent system of n-heptane-methanol-acetonitrile (1.5:0.5:0.5, v/v) and n-heptane-methanol (1.5:1, v/v) in gradient elution, yielding a phloroglucinol compound, hyperforin with HPLC purity over 98%. The ethyl acetate extract was separated by using the solvent system composed of hexane-ethyl acetate-methanol-water (1:1:1:1 and 1:3:1:3, v/v) in gradient through both reverse phase and normal phase elution mode, yielding a naphthodianthrone compound, hypericin with HPLC purity about 95%. The n-butanol extract was separated with the solvent system composed of n-butanol-ethyl acetate–water (1:4:5 and 1.5:3.5:5, v/v) in elution and back-extrusion mode, yielding two of flavones, rutin and hyperoside, with HPLC purity over 95%. HPLC-MS, reference sample and UV spectrum were selectively used in separation to search for target compounds from HPLC-DAD profiles of different sub-extracts. The structures of isolated compounds were further identified by ESI-MS, 1HNMR and 13CNMR. PMID:21306961

Isolation of strawberry anthocyanins using high-speed counter-current chromatography and the copigmentation with catechin or epicatechin by high pressure processing.

PubMed

Zou, Hui; Ma, Yan; Xu, Zhenzhen; Liao, Xiaojun; Chen, Ailiang; Yang, Shuming

2018-05-01

Three anthocyanins were isolated from strawberry extract by high-speed counter-current chromatography, using a biphasic mixture of tert-butyl methyl ether, n-butanol, acetonitrile, water and trifluoroacetic acid (2.5:2.0:2.5:5.0:1.0%). The anthocyanins were identified as pelargonidin-3-rutinoside, cyanidin-3-glucoside and pelargonidin-3-glucoside with purity of 95.6%, 96.2% and 99.3% respectively. Additionally, the copigmentation reaction rates between pelargonidin-3-glucoside and phenolic acids (catechin or epicatechin) at pH 1.5 and 3.6, pressure 0.1 and 500 MPa, and temperature 60 °C were calculated. The absorbance of pelargonidin-3-glucoside at pH 3.6, with high quantity of phenolic acids was significantly increased by high pressure. The complex of pelargonidin-3-glucoside/catechin has a binding energy of 78.64 kJ/mol at pH 3.6, and 39.13 kJ/mol at pH 1.5; pelargonidin-3-glucoside/epicatechin has a binding energy of 75.34 kJ/mol at pH 1.5 and 54.47 kJ/mol at pH 3.6. The hydrogen bond and van der Waals interaction were the main forces contributing to the structures of complex. Copyright © 2017 Elsevier Ltd. All rights reserved.

Two-zone countercurrent smelter system and process

DOEpatents

Cox, J.H.; Fruehan, R.J.; Elliott, J.F.

1995-01-03

A process for continuously smelting iron ore by use of coal to yield molten iron or semi-steel is disclosed. The process comprises the steps of establishing a melt covered by slag; inducing the slag and the molten iron to flow countercurrently to one another, toward opposite ends of the smelter; maintaining iron oxide-reducing conditions in that zone of the smelter towards which the slag flows; maintaining carbon-oxidizing conditions in that zone of the smelter towards which the molten iron flows; continuously or semicontinuously tapping the slag from the reducing zone end of the smelter; continuously or semicontinuously tapping the molten iron from the oxidizing zone end of the smelter; and adding to both zones iron ore, coal, oxygen, and flux at addition rates sufficient to keep the molten iron in the reducing zone substantially saturated with carbon, maintain in the slag being tapped an FeO content of about 5 weight percent or less, and maintain in the molten iron being tapped a carbon content of about 0.5 to 5 weight percent. A slag dam preferably is included in the smelter, to impede the backflow of the slag from the reducing zone to the oxidizing zone. A metal bath dam with one or more flow-through portals also is preferably used, submerged below the slag dam, to impede the backflow of the hot metal. 8 figures.

Two-zone countercurrent smelter system and process

DOEpatents

Cox, James H.; Fruehan, Richard J.; Elliott, deceased, John F.

1995-01-01

A process for continuously smelting iron ore by use of coal to yield molten iron or semi-steel is disclosed. The process comprises the steps of establishing a melt covered by slag; inducing the slag and the molten iron to flow countercurrently to one another, toward opposite ends of the smelter; maintaining iron oxide-reducing conditions in that zone of the smelter towards which the slag flows; maintaining carbon-oxidizing conditions in that zone of the smelter towards which the molten iron flows; continuously or semicontinuously tapping the slag from the reducing zone end of the smelter; continuously or semicontinuously tapping the molten iron from the oxidizing zone end of the smelter; and adding to both zones iron ore, coal, oxygen, and flux at addition rates sufficient to keep the molten iron in the reducing zone substantially saturated with carbon, maintain in the slag being tapped an FeO content of about 5 weight percent or less, and maintain in the molten iron being tapped a carbon content of about 0.5 to 5 weight percent. A slag dam preferably is included in the smelter, to impede the backflow of the slag from the reducing zone to the oxidizing zone. A metal bath dam with one or more flow-through portals also is preferably used, submerged below the slag dam, to impede the backflow of the hot metal.

Schinus terebinthifolius countercurrent chromatography (Part II): Intra-apparatus scale-up and inter-apparatus method transfer.

PubMed

Costa, Fernanda das Neves; Vieira, Mariana Neves; Garrard, Ian; Hewitson, Peter; Jerz, Gerold; Leitão, Gilda Guimarães; Ignatova, Svetlana

2016-09-30

Countercurrent chromatography (CCC) is being widely used across the world for purification of various materials, especially in natural product research. The predictability of CCC scale-up has been successfully demonstrated using specially designed instruments of the same manufacturer. The reality is that the most of CCC users do not have access to such instruments and do not have enough experience to transfer methods from one CCC column to another. This unique study of three international teams is based on innovative approach to simplify the scale-up between different CCC machines using fractionation of Schinus terebinthifolius berries dichloromethane extract as a case study. The optimized separation methodology, recently developed by the authors (Part I), was repeatedly performed on CCC columns of different design available at most research laboratories across the world. Hexane - ethyl acetate - methanol - water (6:1:6:1, v/v/v/v) was used as solvent system with masticadienonic and 3β-masticadienolic acids as target compounds to monitor stationary phase retention and calculate peak resolution. It has been demonstrated that volumetric, linear and length scale-up transfer factors based on column characteristics can be directly applied to different i.d., volume and length columns independently on instrument make in an intra-apparatus scale-up and inter-apparatus method transfer. Copyright © 2016 Elsevier B.V. All rights reserved.

Annual and longitudinal variations of the Pacific North Equatorial Countercurrent

NASA Technical Reports Server (NTRS)

Lolk, Nina K.

1992-01-01

The climatological annual cycle of the Pacific North Equatorial Countercurrent (NECC) simulated by an ocean general circulation model (OGCM) was studied. The longitudinal variation of transports, degree of geostrophy, and the relationship between Ekman pumping and vertical displacement of the thermocline were emphasized. The longitudinal variation was explored using six sections along 150 deg E, 180 deg, 160 deg W, 140 deg W, 125 deg W, and 110 deg W. A primitive equation OGCM of the Pacific Ocean was run for three years and the fields used were from the third year. The fields consisted of zonal, meridional, and vertical current components and temperature and salinity averaged every three days. The model was forced with the Hellerman and Rosenstein climatological wind stress. The mean annual eastward transport (19.9 Sv) was largest at 160 deg W. The maximum-current boundaries along 160 deg W were 9.2 deg N (1.0 deg), 5.1 deg N (1.1 deg), and 187 m (90.6 m). The annual-cycle amplitude of the NECC was greatest between 160 deg W and 140 deg W. Although the NECC is geostrophic to the first order, deviations from geostrophy were found in the boreal spring and summer near the southern boundary and near the surface. Meridional local acceleration played a role between 3 deg N-5 deg N.

Downhole steam generator having a downhole oxidant compressor

DOEpatents

Fox, Ronald L.

1983-01-01

Apparatus and method for generation of steam in a borehole for penetration into an earth formation wherein a downhole oxidant compressor is used to compress relatively low pressure (atmospheric) oxidant, such as air, to a relatively high pressure prior to mixing with fuel for combustion. The multi-stage compressor receives motive power through a shaft driven by a gas turbine powered by the hot expanding combustion gases. The main flow of compressed oxidant passes through a velocity increasing nozzle formed by a reduced central section of the compressor housing. An oxidant bypass feedpipe leading to peripheral oxidant injection nozzles of the combustion chamber are also provided. The downhole compressor allows effective steam generation in deep wells without need for high pressure surface compressors. Feedback preheater means are provided for preheating fuel in a preheat chamber. Preheating of the water occurs in both a water feed line running from aboveground and in a countercurrent water flow channel surrounding the combustor assembly. The countercurrent water flow channels advantageously serve to cool the combustion chamber wall. The water is injected through slotted inlets along the combustion chamber wall to provide an unstable boundary layer and stripping of the water from the wall for efficient steam generation. Pressure responsive doors are provided at the steam outlet for closing and sealing the combustion chamber from entry of reservoir fluids in the event of a flameout.

[Preparative isolation and purification of the active components from Viticis Fructus by high-speed counter-current chromatography].

PubMed

Guan, Renjun; Wang, Daijie; Yu, Zongyuan; Wang, Xiao; Lan, Tianfeng

2010-11-01

Vitex trifolia L. var. simplicifolia Cham. is widely distributed in Asia, and its fruits are used as a folk medicine for headaches, colds, migraine, eyepain, etc. In order to effectively separate high-purity active components from the seeds of Vitex trifolia L. var. simplicifolia Cham., a high-speed counter-current chromatography (HSCCC) procedure was performed to separate four components from the crude extract of the fruits. A two-phase solvent system composed of light petroleum-ethyl acetate-methanol-water (3:6: 3.6: 3, v/v/v/ v) was used. Within 230 min, 23 mg of 4-hydroxybenzoic acid, 15 mg of 3,6,7-trimethylquercetagetin, 24 mg of casticin and 5 mg of artemetin were obtained from 250 mg of the crude extract of Viticis Fructus in one-step elution under the conditions of a flow rate of 1.5 mL/min, 800 r/min and the detection wavelength of 254 nm. The purities of the four fractions were 93.1%, 97.3%, 98.7% and 98.5%, respectively. The obtained fractions were analyzed by high performance liquid chromatography (HPLC), and identified by electrospray ionization mass spectrometry (ESI-MS), 1H-nuclear magnetic resonance (NMR) and 13C-NMR. The results indicate that HSCCC is a powerful technique for the purification of active components from Viticis Fructus.

Preparation of the monomers of gingerols and 6-shogaol by flash high speed counter-current chromatography.

PubMed

Qiao, Qingliang; Du, Qizhen

2011-09-09

The flash high speed counter-current chromatographic (FHSCCC) separation of gingerols and 6-shogaol was performed on a HSCCC instrument equipped with a 1200-ml column (5 mm tubing i.d.) at a flow rate of 25 ml/min. The performance met the FHSCCC feature that the flow rate of mobile phase (ml) is equal to or greater than the square of the diameter of the column tubing (mm). The separation employed the upper phase of stationary phase of the n-hexane-ethyl acetate-methanol-water (3:2:2:3, v/v) as the stationary phase. A stepwise elution was performed by eluting with the lower phase of n-hexane-ethyl acetate-methanol-water (3:2:2:3, v/v) for first 90 min and the lower phase of the n-hexane-ethyl acetate-methanol-water (3:2:6:5, v/v) for the second 90 min. In each separation 5 g of the ethyl acetate extract of rhizomes of ginger was loaded, yielding 1.96 g of 6-gingerol (98.3%), 0.33 g of 8-gingerol (97.8%), 0.64 g of 6-shogaol (98.8%) and 0.57 g of 10-gingerol (98.2%). The separation can be expected to scale up to industrial separation. Copyright © 2010 Elsevier B.V. All rights reserved.

Development of the Next-Generation Caustic-Side Solvent Extraction (NG-CSSX) Process for Cesium Removal from High-Level Tank Waste

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

Moyer, Bruce A; Bonnesen, Peter V; Delmau, Laetitia Helene

2011-01-01

This paper describes the chemical performance of the Next-Generation Caustic-Side Solvent Extraction (NG-CSSX) process in its current state of development for removal of cesium from the alkaline high-level tank wastes at the Savannah River Site (SRS) in the US Department of Energy (USDOE) complex. Overall, motivation for seeking a major enhancement in performance for the currently deployed CSSX process stems from needs for accelerating the cleanup schedule and reducing the cost of salt-waste disposition. The primary target of the NG-CSSX development campaign in the past year has been to formulate a solvent system and to design a corresponding flowsheet thatmore » boosts the performance of the SRS Modular CSSX Unit (MCU) from a current minimum decontamination factor of 12 to 40,000. The chemical approach entails use of a more soluble calixarene-crown ether, called MaxCalix, allowing the attainment of much higher cesium distribution ratios (DCs) on extraction. Concurrently decreasing the Cs-7SB modifier concentration is anticipated to promote better hydraulics. A new stripping chemistry has been devised using a vitrification-friendly aqueous boric acid strip solution and a guanidine suppressor in the solvent, resulting in sharply decreased DCs on stripping. Results are reported herein on solvent phase behavior and batch Cs distribution for waste simulants and real waste together with a preliminary flowsheet applicable for implementation in the MCU. The new solvent will enable MCU to process a much wider range of salt feeds and thereby extend its service lifetime beyond its design life of three years. Other potential benefits of NG-CSSX include increased throughput of the SRS Salt Waste Processing Facility (SWPF), currently under construction, and an alternative modular near-tank application at Hanford.« less

Next Generation Solvent Performance in the Modular Caustic Side Solvent Extraction Process - 15495

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

Smith, Tara E.; Scherman, Carl; Martin, David

Changes to the Modular Caustic Side Solvent Extraction Unit (MCU) flow-sheet were implemented in the facility. Implementation included changing the scrub and strip chemicals and concentrations, modifying the O/A ratios for the strip, scrub, and extraction contactor banks, and blending the current BoBCalixC6 extractant-based solvent in MCU with clean MaxCalix extractant-based solvent. During the successful demonstration period, the MCU process was subject to rigorous oversight to ensure hydraulic stability and chemical/radionuclide analysis of the key process tanks (caustic wash tank, solvent hold tank, strip effluent hold tank, and decontaminated salt solution hold tank) to evaluate solvent carryover to downstream facilitiesmore » and the effectiveness of cesium removal from the liquid salt waste. Results indicated the extraction of cesium was significantly more effective with an average Decontamination Factor (DF) of 1,129 (range was 107 to 1,824) and that stripping was effective. The contactor hydraulic performance was stable and satisfactory, as indicated by contactor vibration, contactor rotational speed, and flow stability; all of which remained at or near target values. Furthermore, the Solvent Hold Tank (SHT) level and specific gravity was as expected, indicating that solvent integrity and organic hydraulic stability were maintained. The coalescer performances were in the range of processing results under the BOBCalixC6 flow sheet, indicating negligible adverse impact of NGS deployment. After the Demonstration period, MCU began processing via routine operations. Results to date reiterate the enhanced cesium extraction and stripping capability of the Next Generation Solvent (NGS) flow sheet. This paper presents process performance results of the NGS Demonstration and continued operations of MCU utilizing the blended BobCalixC6-MaxCalix solvent under the NGS flowsheet.« less

Discards beneficiation in South Africa

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

Horsfall, D.W.

1995-08-01

The intergrown nature of most South African coals means that in beneficiating them, the preparation engineer rarely has the easy task of carrying out a simple separation between good coal and high density shale or stone. Apart from de-shaling operations, all beneficiation entails rejecting, not only adventitious stone but a large percentage of high ash but strongly combustible middlings material. Typically, a coal preparation plant can only recover about 70-80% of the heat in the run-of-mine coal. The other 20-30% ends up on the discard heap. Over the last decade, extensive studies were carried out to establish the extend tomore » which that discarded heat may be recoverable in marketable grades of coal. Detailed washability studies were carried out on four mines which between them produce almost 60% of the total make of discards. Computer simulations allowed different flowsheet configurations to be assessed to give rewashed coal of various calorific values. The flowsheets were also subjected to factorial establishment of budget capital and operating costs. Finally some initial work was carried out on the potential markets for such products. This paper is concise account of the results of the study for one major mine. Please note that the paper is based almost wholly on the evaluation carried out for the Energy Branch of the Department of Mineral and Energy Affairs (DMEA). The actual work was executed by the van Eck and Lurie Division of E L Bateman and Co. The writer chaired the Beneficiation Sub-Committee set up by the DMEA to oversee and guide the work, and in that capacity was closely connected with the study as it evolved. Other acknowledgements are given at the end of the paper.« less

SME Acceptability Determination For DWPF Process Control (U)

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

Edwards, T.

2017-06-12

The statistical system described in this document is called the Product Composition Control System (PCCS). K. G. Brown and R. L. Postles were the originators and developers of this system as well as the authors of the first three versions of this technical basis document for PCCS. PCCS has guided acceptability decisions for the processing at the Defense Waste Processing Facility (DWPF) at the Savannah River Site (SRS) since the start of radioactive operations in 1996. The author of this revision to the document gratefully acknowledges the firm technical foundation that Brown and Postles established to support the ongoing successfulmore » operation at the DWPF. Their integration of the glass propertycomposition models, developed under the direction of C. M. Jantzen, into a coherent and robust control system, has served the DWPF well over the last 20+ years, even as new challenges, such as the introduction into the DWPF flowsheet of auxiliary streams from the Actinide Removal Process (ARP) and other processes, were met. The purpose of this revision is to provide a technical basis for modifications to PCCS required to support the introduction of waste streams from the Salt Waste Processing Facility (SWPF) into the DWPF flowsheet. An expanded glass composition region is anticipated by the introduction of waste streams from SWPF, and property-composition studies of that glass region have been conducted. Jantzen, once again, directed the development of glass property-composition models applicable for this expanded composition region. The author gratefully acknowledges the technical contributions of C.M. Jantzen leading to the development of these glass property-composition models. The integration of these models into the PCCS constraints necessary to administer future acceptability decisions for the processing at DWPF is provided by this sixth revision of this document.« less

Laboratory Tests on Post-Filtration Precipitation in the WTP Pretreatment Process

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

Russell, Renee L.; Peterson, Reid A.; Rinehart, Donald E.

Pacific Northwest National Laboratory (PNNL) has been tasked by Bechtel National Inc. (BNI) on the River Protection Project-Hanford Tank Waste Treatment and Immobilization Plant (RPP-WTP) project to perform research and development activities to resolve technical issues identified for the Pretreatment Facility (PTF). The Pretreatment Engineering Platform (PEP) was designed, constructed, and operated as part of a plan to respond to issue M12, "Undemonstrated Leaching Processes," of the External Flowsheet Review Team (EFRT) issue response plan (Barnes et al. 2006). The PEP is a 1/4.5-scale test platform designed to simulate the WTP pretreatment caustic leaching, oxidative leaching, ultrafiltration solids concentration, andmore » slurry washing processes. The PEP replicates the WTP leaching processes using prototypic equipment and control strategies. A simplified flow diagram of the PEP system is shown in Figure 1.1. Two operating scenarios are currently being evaluated for the ultrafiltration process (UFP) and leaching operations. The first scenario has caustic leaching performed in the UFP-2 ultrafiltration feed vessels (i.e., vessel UFP-VSL-T02A in the PEP; and vessels UFP-VSL-00002A and B in the WTP PTF). The second scenario has caustic leaching conducted in the UFP-1 ultrafiltration feed preparation vessels (i.e., vessels UFP-VSL-T01A and B in the PEP; vessels UFP-VSL-00001A and B in the WTP PTF).« less

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

Ermanoski, Ivan; Orozco, Adrian

In this report we present the development of a packed particle bed recirculator and heat exchanger. The device is intended to create countercurrent flows of packed particle beds and exchange heat between the flows. The project focused on the design, fabrication, demonstration, and modifications of a simple prototype, in order to attain high levels of heat exchange between particle flows while maintaining an effective particle conveying rate in a scalable package. Despite heat losses in a package not optimized for heat retention, 50% heat recovery was achieved, at a particle conveying efficiency of 40%.

Calculation of prompt loss and toroidal field ripple loss under neutral beam injection on EAST

NASA Astrophysics Data System (ADS)

Wu, Bin; Hao, Baolong; White, Roscoe; Wang, Jinfang; Zang, Qing; Han, Xiaofeng; Hu, Chundong

2017-02-01

Neutral beam injection is a major auxiliary heating method in the EAST experimental campaign. This paper gives detailed calculations of beam loss with different plasma equilibria using the guiding center code ORBIT and NUBEAM/TRANSP. Increasing plasma current can dramatically lower the beam ion prompt loss and ripple loss. Countercurrent beam injection gives a much larger prompt loss fraction than co-injection, and ripple-induced collisionless stochastic diffusion is the dominant loss channel.

Calculation of prompt loss and toroidal field ripple loss under neutral beam injection on EAST

DOE PAGES

Wu, Bin; Hao, Baolong; White, Roscoe; ...

2016-12-09

Here, neutral beam injection is a major auxiliary heating method in the EAST experimental campaign. This paper gives detailed calculations of beam loss with different plasma equilibria using the guiding center code ORBIT and NUBEAM/TRANSP. Increasing plasma current can dramatically lower the beam ion prompt loss and ripple loss. Countercurrent beam injection gives a much larger prompt loss fraction than co-injection, and ripple-induced collisionless stochastic diffusion is the dominant loss channel.

DECONTAMINATION OF NEUTRON-IRRADIATED REACTOR FUEL

DOEpatents

Buyers, A.G.; Rosen, F.D.; Motta, E.E.

1959-12-22

A pyrometallurgical method of decontaminating neutronirradiated reactor fuel is presented. In accordance with the invention, neutron-irradiated reactor fuel may be decontaminated by countercurrently contacting the fuel with a bed of alkali and alkaine fluorides under an inert gas atmosphere and inductively melting the fuel and tracking the resulting descending molten fuel with induction heating as it passes through the bed. By this method, a large, continually fresh surface of salt is exposed to the descending molten fuel which enhances the efficiency of the scrubbing operation.

Generation of noninductive current by electron-Bernstein waves on the COMPASS-D Tokamak.

PubMed

Shevchenko, V; Baranov, Y; O'Brien, M; Saveliev, A

2002-12-23

Electron-Bernstein waves (EBW) were excited in the plasma by mode converted extraordinary (X) waves launched from the high field side of the COMPASS-D tokamak at different toroidal angles. It has been found experimentally that X-mode injection perpendicular to the magnetic field provides maximum heating efficiency. Noninductive currents of up to 100 kA were found to be driven by the EBW mode with countercurrent drive. These results are consistent with ray tracing and quasilinear Fokker-Planck simulations.

Process and apparatus for solvent extraction of oil from oil-containing diatomite ore

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

Karnofsky, G. B.

1980-12-16

A process for solvent extraction of oil from oil bearing diatomite ore and an apparatus for use therewith, wherein the ore is extracted by countercurrent decantation with a hydrocarbon solvent, solvent is recovered from the extract by multiple effect evaporation followed by stripping, and the spent diatomite is contacted with water to displace a major portion of the solvent therefrom, and solvent is recovered from the aqueous slurry of the spent diatomite by stripping with steam at superatmospheric pressure.

Method of independently operating a group of stages within a diffusion cascade

DOEpatents

Benedict, Manson; Fruit, Allen J.; Levey, Horace B.

1976-06-08

1. A method of operating a group of the diffusion stages of a productive diffusion cascade with countercurrent flow, said group comprising a top and a bottom stage, which comprises isolating said group from said cascade, circulating the diffused gas produced in said top stage to the feed of said bottom stage while at the same time circulating the undiffused gas from said bottom stage to the feed of said top stage whereby major changes in

Analytical Study on Thermal and Mechanical Design of Printed Circuit Heat Exchanger

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

Yoon, Su-Jong; Sabharwall, Piyush; Kim, Eung-Soo

2013-09-01

The analytical methodologies for the thermal design, mechanical design and cost estimation of printed circuit heat exchanger are presented in this study. In this study, three flow arrangements of parallel flow, countercurrent flow and crossflow are taken into account. For each flow arrangement, the analytical solution of temperature profile of heat exchanger is introduced. The size and cost of printed circuit heat exchangers for advanced small modular reactors, which employ various coolants such as sodium, molten salts, helium, and water, are also presented.

Calculation of prompt loss and toroidal field ripple loss under neutral beam injection on EAST

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

Wu, Bin; Hao, Baolong; White, Roscoe

Here, neutral beam injection is a major auxiliary heating method in the EAST experimental campaign. This paper gives detailed calculations of beam loss with different plasma equilibria using the guiding center code ORBIT and NUBEAM/TRANSP. Increasing plasma current can dramatically lower the beam ion prompt loss and ripple loss. Countercurrent beam injection gives a much larger prompt loss fraction than co-injection, and ripple-induced collisionless stochastic diffusion is the dominant loss channel.

TECHNETIUM RETENTION IN WTP LAW GLASS WITH RECYCLE FLOW-SHEET DM10 MELTER TESTING VSL-12R2640-1 REV 0

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

Abramowitz, Howard; Brandys, Marek; Cecil, Richard

2012-12-11

Melter tests were conducted to determine the retention of technetium and other volatiles in glass while processing simulated Low Activity Waste (LAW) streams through a DM10 melter equipped with a prototypical off-gas system that concentrates and recycles fluid effiuents back to the melter feed. To support these tests, an existing DM10 system installed at Vitreous State Laboratory (VSL) was modified to add the required recycle loop. Based on the Hanford Tank Waste Treatment and Immobilization Plant (WTP) LAW off-gas system design, suitably scaled versions of the Submerged Bed Scrubber (SBS), Wet Electrostatic Precipitator (WESP), and TLP vacuum evaporator were designed,more » built, and installed into the DM10 system. Process modeling was used to support this design effort and to ensure that issues associated with the short half life of the {sup 99m}Tc radioisotope that was used in this work were properly addressed and that the system would be capable of meeting the test objectives. In particular, this required that the overall time constant for the system was sufficiently short that a reasonable approach to steady state could be achieved before the {sup 99m}Tc activity dropped below the analytical limits of detection. The conceptual design, detailed design, flow sheet development, process model development, Piping and Instrumentation Diagram (P&ID) development, control system design, software design and development, system fabrication, installation, procedure development, operator training, and Test Plan development for the new system were all conducted during this project. The new system was commissioned and subjected to a series of shake-down tests before embarking on the planned test program. Various system performance issues that arose during testing were addressed through a series of modifications in order to improve the performance and reliability of the system. The resulting system provided a robust and reliable platform to address the test objectives.« less

Cost evaluation of cellulase enzyme for industrial-scale cellulosic ethanol production based on rigorous Aspen Plus modeling.

PubMed

Liu, Gang; Zhang, Jian; Bao, Jie

2016-01-01

Cost reduction on cellulase enzyme usage has been the central effort in the commercialization of fuel ethanol production from lignocellulose biomass. Therefore, establishing an accurate evaluation method on cellulase enzyme cost is crucially important to support the health development of the future biorefinery industry. Currently, the cellulase cost evaluation methods were complicated and various controversial or even conflict results were presented. To give a reliable evaluation on this important topic, a rigorous analysis based on the Aspen Plus flowsheet simulation in the commercial scale ethanol plant was proposed in this study. The minimum ethanol selling price (MESP) was used as the indicator to show the impacts of varying enzyme supply modes, enzyme prices, process parameters, as well as enzyme loading on the enzyme cost. The results reveal that the enzyme cost drives the cellulosic ethanol price below the minimum profit point when the enzyme is purchased from the current industrial enzyme market. An innovative production of cellulase enzyme such as on-site enzyme production should be explored and tested in the industrial scale to yield an economically sound enzyme supply for the future cellulosic ethanol production.

Calcination/dissolution chemistry development Fiscal year 1995

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

Delegard, C.H.

1995-09-01

The task {open_quotes}IPC Liaison and Chemistry of Thermal Reconstitution{close_quotes} is a $300,000 program that was conducted in Fiscal Year (FY) 1995 with U.S. Department of Energy (DOE) Office of Research and Development (EM-53) Efficient Separations and Processing Crosscutting Program supported under technical task plan (TTP) RL4-3-20-04. The principal investigator was Cal Delegard of the Westinghouse Hanford Company (WHC). The task encompassed the following two subtasks related to the chemistry of alkaline Hanford Site tank waste: (1) Technical Liaison with the Institute of Physical Chemistry of the Russian Academy of Science (IPC/RAS) and its research into the chemistry of transuranic elementsmore » (TRU) and technetium (Tc) in alkaline media. (2) Laboratory investigation of the chemistry of calcination/dissolution (C/D) (or thermal reconstitution) as an alternative to the present reference Hanford Site tank waste pretreatment flowsheet, Enhanced Sludge Washing (ESW). This report fulfills the milestone for the C/D subtask to {open_quotes}Provide End-of-Year Report on C/D Laboratory Test Results{close_quotes} due 30 September 1995. A companion report, fulfilling the milestone to provide an end-of-year report on the IPC/RAS liaison, also has been prepared.« less

Southward flow on the western flank of the Florida Current

NASA Astrophysics Data System (ADS)

Soloviev, Alexander V.; Hirons, Amy; Maingot, Christopher; Dean, Cayla W.; Dodge, Richard E.; Yankovsky, Alexander E.; Wood, Jon; Weisberg, Robert H.; Luther, Mark E.; McCreary, Julian P.

2017-07-01

A suite of long-term in situ measurements in the Straits of Florida, including the ADCP bottom moorings at an 11-m isobath and 244-m isobath (Miami Terrace) and several ADCP ship transects, have revealed a remarkable feature of the ocean circulation - southward flow on the western, coastal flank of the Florida Current. We have observed three forms of the southward flow - a seasonally varying coastal countercurrent, an undercurrent jet attached to the Florida shelf, and an intermittent undercurrent on the Miami Terrace. According to a 13-year monthly climatology obtained from the near-shore mooring, the coastal countercurrent is a persistent feature from October through January. The southward flow in the form of an undercurrent jet attached to the continental slope was observed during five ship transects from April through September but was not observed during three transects in February, March, and November. This undercurrent jet is well mixed due to strong shear at its top associated with the northward direction of the surface flow (Florida Current) and friction at the bottom. At the same time, no statistically significant seasonal cycle has been observed in the undercurrent flow on the Miami Terrace. Theoretical considerations suggest that several processes could drive the southward current, including interaction between the Florida Current and the shelf, as well as forcing that is independent of the Florida Current. The exact nature of the southward flow on the western flank of the Florida Current is, however, unknown.

Fractionation of technical octabromodiphenyl ether by countercurrent chromatography combined with gas chromatography/mass spectrometry and offline and online (1)H nuclear magnetic resonance spectroscopy.

PubMed

Hammann, Simon; Conrad, Jürgen; Vetter, Walter

2015-06-12

Countercurrent chromatography (CCC) is a technique, which uses two immiscible liquid phases for a separation process in a long and hollow tube. The technique allows the separation of high amounts of sample (50mg to several grams) with a low consumption of solvents. In this study, we fractionated 50mg technical octabromodiphenyl ether (DE-79) and analyzed the fractions by gas chromatography with mass spectrometry (GC/MS) and proton nuclear magnetic resonance ((1)H NMR) spectroscopy. CCC separations were performed with n-hexane/acetonitrile as solvent system in tail-to-head (i.e. the upper phase is mobile) mode. Twelve CCC fractions were studied for the PBDE composition. CCC elution of PBDE congeners was dependent both on the degree of bromination and substitution pattern. Higher brominated congeners eluted faster than lower brominated congeners and isomers with vicinal hydrogen atoms eluted last. In addition to several known PBDE congeners in DE-79, we were able to unequivocally identify BDE 195 in DE-79 and we could verify the presence of BDE 184. Finally, we also established the online hyphenation of CCC with (1)H NMR. The use of deuterated solvents could be avoided by using n-hexane/acetonitrile as two-phase system. By online CCC-(1)H NMR in stop-flow mode we were able to detect eight PBDE congeners in the mixture. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparative isolation and purification of capsaicin and dihydrocapsaicin from Capsici Fructus using supercritical fluid extraction combined with high speed countercurrent chromatography.

PubMed

Yan, Rongwei; Zhao, Leilei; Tao, Junfei; Zou, Yong; Xu, Xinjun

2018-05-01

Supercritical fluid extraction with CO 2 (SFE-CO 2 ) was utilized for extraction of capsaicin (CA) and dihydrocapsaicin (DHCA) from Capsici Fructus, and then a two-step enrichment method for separating capsaicinoids from SFE-CO 2 extracts was developed. The process involved extraction with aqueous methanol and crystallization by alkali extraction and acid precipitation. Finally, a consecutive high-speed countercurrent chromatography (HSCCC) separation method was successfully applied in the purification of CA and DHCA from capsaicinoid crystal. The extraction pressure, extraction temperature and volume of co-solvent were optimized at 33 MPa, 41 °C and 75 mL, respectively, using response surface methodology; the extraction rates of CA and DHCA were about 93.18% and 93.49%, respectively. 407.43 mg capsaicinoid crystal was isolated from the SFE-CO 2 extracts obtained from 100 g capsicum powder by the two-step enrichment method. About 506 mg and 184 mg CA and DHCA with purities up to 98.31% and 96.68%, respectively, were obtained from 1 g capsaicinoid crystal in one HSCCC of three consecutive sample loadings without exchanging any solvent system. This method comprising SFE-CO 2 , a two-step enrichment and HSCCC was efficient, powerful and practical for the large-scale preparation of CA and DHCA from Capsici Fructus with high purity and high yield. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

One-step separation and purification of three lignans and one flavonol from Sinopodophyllum emodi by medium-pressure liquid chromatography and high-speed counter-current chromatography.

PubMed

Wang, Ping; Liu, Yongling; Chen, Tao; Xu, Wenhua; You, Jinmao; Liu, Yongjun; Li, Yulin

2013-01-01

Lignans and flavonols are the primary constituents of Sinopodophyllum emodi and have been used as cathartic, anthelmintic, chemotherapeutic and anti-hypertensive compounds. Although these compounds have been isolated, there have been no reports on the separation of 4'-demethyl podophyllotoxin, podophyllotoxin, deoxypodophyllotoxin and kaempferol in one step by medium-pressure liquid chromatography (MPLC) and high-speed counter-current chromatography (HSCCC). Development of an efficient method for the preparative separation and purification of three lignans and one flavonol from S. emodi. The precipitate of crude extracts was first separated by MPLC into four parts, numbered GJ-1, GJ-2, GJ-3 and GJ-4. GJ-1 was separated and purified by HSCCC using a solvent system composed of n-hexane:ethyl acetate:methanol:water (1.75:1.5:1:0.75, v/v/v/v). The purities of the target compounds were assessed using high-performance liquid chromatography (HPLC) and chemical structures were identified by (1) H-NMR and (13) C-NMR. The HSCCC and MPLC methods were successfully used for the preparative separation and purification of 4'-demethyl podophyllotoxin (8.5 mg, 92.4%), podophyllotoxin (40.1 mg, 92.1%), deoxypodophyllotoxin (4.6 mg, 98.1%), and kaempferol (1.6 mg, 96.7%) from a 100 mg sample. Three lignans (4'-demethyl podophyllotoxin, podophyllotoxin, deoxypodophyllotoxin) and one flavonol (kaempferol) were successfully isolated by HSCCC and MPLC in one step. Copyright © 2013 John Wiley & Sons, Ltd.

[Isolation and preparation of an imidazole alkaloid from radix radix of Aconitum pendulum Busch by semi-preparative high-speed counter-current chromatography].

PubMed

Liu, Yongling; Chen, Tao; Chen, Chen; Zou, Denglang; Li, Yulin

2014-05-01

Aconitum pendulum Busch is rich C19 diterpenoid alkaloids, but there is no report of imidazole alkaloid in Aconitum pendulum Busch. In this study, an imidazole alkaloid named 1H-imidazole-2-carboxylic acid, butyl ester (ICABE) was successfully separated from Aconitum pendulum Busch with semi-preparative high-speed counter-current chromatography (HSCCC). The partition coefficient was measured by HPLC to select the solvent systems for ICABE separation by HSCCC. The separation was performed with a two-phase solvent system composed of n-hexane-chloroform-ethanol-water (10:1 : 13:2, v/v/v/v). The upper phase was used as the stationary phase and the lower phase as the mobile phase. It was operated at a flow rate of 1.8 mL/min. The apparatus was rotated at 850 r/min, and the detection wavelength was set at 230 nm. Under the selected conditions, a high efficiency separation of HSCCC was achieved, and 7.5 mg of ICABE was obtained from 100 mg of the crude sample of Aconitum pendulum in one-step separation within 350 min. The HPLC analysis showed that the purity of the compound was over 98%. The chemical structure was confirmed by UV, 1H-NMR and 13C-NMR. The established method is simple, highly efficient and suitable for large scale separation of ICABE from radix of Aconitum pendulum Busch.

The three-dimensional model for helical columns on type-J synchronous counter-current chromatography.

PubMed

Guan, Y H; van den Heuvel, Remco

2011-08-05

Unlike the existing 2-D pseudo-ring model for helical columns undergoing synchronous type-J planetary motion of counter-current chromatograph (CCC), the 3-D "helix" model developed in this work shows that there is a second normal force (i.e. the binormal force) applied virtually in the axial direction of the helical column. This force alternates in the two opposite directions and intensifies phase mixing with increasing the helix angle. On the contrary, the 2-D spiral column operated on the same CCC device lacks this third-dimensional mixing force. The (principal) normal force quantified by this "helix" model has been the same as that by the pseudo-ring model. With β>0.25, this normal centrifugal force has been one-directional and fluctuates cyclically. Different to the spiral column, this "helix" model shows that the centrifugal force (i.e. the hydrostatic force) does not contribute to stationary phase retention in the helical column. Between the popular helical columns and the emerging spiral columns for type-J synchronous CCC, this work has thus illustrated that the former is associated with better phase mixing yet poor retention for the stationary phase whereas the latter has potential for better retention for the stationary phase yet poor phase mixing. The methodology developed in this work may be regarded as a new platform for designing optimised CCC columns for analytical and engineering applications. Copyright © 2011 Elsevier B.V. All rights reserved.

Calmodulin-stimulated Ca(2+)-ATPases in the vacuolar and plasma membranes in cauliflower.

PubMed

Askerlund, P

1997-07-01

The subcellular locations of Ca(2+)-ATPases in the membranes of cauliflower (Brassica oleracea L.) inflorescences were investigated. After continuous sucrose gradient centrifugation a 111-kD calmodulin (CaM)-stimulated and caM-binding Ca(2+)-ATPase (BCA1; P. Askerlund [1996] Plant Physiol 110: 913-922; S. Malmström, P. Askerlund, M.G. Plamgren [1997] FEBS Lett 400: 324-328) comigrated with vacuolar membrane markers, whereas a 116-kD caM-binding Ca(2+)-ATPase co-migrated with a marker for the plasma membrane. The 116 kD Ca(2+)-ATPase was enriched in plasma membranes obtained by aqueous two-phase partitioning, which is in agreement with a plasma membrane location of this Ca(2+)-ATPase. Countercurrent distribution of a low-density intracellular membrane fraction in an aqueous two-phase system resulted in the separation of the endoplasmic reticulum and vacuolar membranes. The 111-kD Ca(2+)-ATPase co-migrated with a vacuolar membrane marker after countercurrent distribution but not with markers for the endoplasmic reticulum. A vacuolar membrane location of the 111-kD Ca(2+)-AtPase was further supported by experiments with isolated vacuoles from cauliflower: (a) Immunoblotting with an antibody against the 111-kD Ca(2+)-ATPase showed that it was associated with the vacuoles, and (b) ATP-dependent Ca2+ uptake by the intact vacuoles was found to be CaM stimulated and partly protonophore insensitive.

Revisiting resolution in hydrodynamic countercurrent chromatography: tubing bore effect.

PubMed

Berthod, A; Faure, K

2015-04-17

A major challenge in countercurrent chromatography (CCC), the technique that works with a support-free biphasic liquid system, is to retain the liquid stationary phase inside the CCC column (Sf parameter). Two solutions are commercially available: the hydrostatic CCC columns, also called centrifugal partition chromatographs (CPC), with disks of interconnected channels and rotary seals, and the hydrodynamic CCC columns with bobbins of coiled open tube and no rotary seals. It was demonstrated that the amount of liquid stationary phase retained by a coiled tube was higher with larger bore tubing than with small bore tubes. At constant column volume, small bore tubing will be longer producing more efficiency than larger bore tube that will better retain the liquid stationary phase. Since the resolution equation in CCC is depending on both column efficiency and stationary phase retention ratio, the influence of the tubing bore should be studied. This theoretical work showed that there is an optimum tubing bore size depending on solute partition coefficient and mobile phase flow rate. The interesting result of the theoretical study is that larger tubing bores allow for dramatically reduced experiment durations for all solutes: in reversed phase CCC (polar mobile phase), hydrophobic solutes are usually highly retained. These apolar solutes can be separated by the same coil at high flow rates and reduced Sf with similar retention times as polar solutes separated at smaller flow rates and much higher Sf. Copyright © 2015 Elsevier B.V. All rights reserved.

Efficient Preparation of Streptochlorin from Marine Streptomyces sp. SYYLWHS-1-4 by Combination of Response Surface Methodology and High-Speed Counter-Current Chromatography.

PubMed

Li, Lin; He, Shan; Ding, Lijian; Yuan, Ye; Zhu, Peng; Epstein, Slava; Fan, Jianzhong; Wu, Xiaokai; Yan, Xiaojun

2016-05-27

Since first isolated from the lipophilic extract of Streptomyces sp. SF2583, streptochlorin, has attracted a lot of attention because of its various pharmacological properties, such as antibiotic, antiallergic, antitumor, and anti-inflammatory activities. For the efficient preparation of streptochlorin from a producing strain Streptomyces sp. SYYLWHS-1-4, we developed a combinative method by using response surface methodology (RSM) and high-speed counter-current chromatography (HSCCC). In the fermentation process, we used RSM to optimize the condition for the efficient accumulation of streptochlorin, and the optimal parameters were: yeast extract 1.889 g/L, soluble starch 8.636 g/L, K₂HPO₄ 0.359 g/L, CaCl₂ 2.5 g/L, MgSO₄ 0.625 g/L, marine salt 25 g/L, medium volume 50%, initial pH value 7.0, temperature 27.5 °C, which enhanced streptochlorin yield by 17.7-fold. During the purification process, the preparative HSCCC separation was performed using a petroleum ether-ethyl acetate-methanol-water (9:0.8:5:5, v/v/v/v) biphasic solvent system, where 300 mg of crude sample yielded 16.5 mg streptochlorin with over 95% purity as determined by UPLC. Consequently, the combination method provided a feasible strategy for highly effective preparation of streptochlorin, which ensured the supply of large amounts of streptochlorin for in vivo pharmacological assessments or other requirements.

At-line hyphenation of high-speed countercurrent chromatography with Sephadex LH-20 column chromatography for bioassay-guided separation of antioxidants from vine tea (Ampelopsis grossedentata).

PubMed

Ma, Ruyi; Zhou, Rongrong; Tong, Runna; Shi, Shuyun; Chen, Xiaoqing

2017-01-01

Vine tea (Ampelopsis grossedentata), a widely used healthy tea, beverage and herbal medicine, exhibited strong antioxidant activity. However, systematic purification of antioxidants, especially for those with similar structures or polarities, is a challenging work. Here, we present a novel at-line hyphenation of high-speed countercurrent chromatography with Sephadex LH-20 column chromatography (HSCCC-Sephadex LH-20 CC) for rapid and efficient separation of antioxidants from vine tea target-guided by 1,1-diphenyl-2-picryl-hydrazyl radical-high performance liquid chromatography (DPPH-HPLC) experiment. A makeup pump, a six-port switching valve and a trapping column were served as interface. The configuration had no operational time and mobile phase limitations between two dimensional chromatography and showed great flexibility without tedious sample-handling procedure. Seven targeted antioxidants were firstly separated by stepwise HSCCC using petroleum ether-ethyl acetate-methanol-water (4:9:4:9, v/v/v/v) and (4:9:5:8, v/v/v/v) as solvent systems, and then co-eluted antioxidants were on-line trapped, concentrated and desorbed to Sephadex LH-20 column for further off-line purification by methanol. It is noted that six elucidated antioxidants with purity over 95% exhibited stronger activity than ascorbic acid (VC). More importantly, this at-line hyphenated strategy could sever as a rapid and efficient pathway for systematic purification of bioactive components from complex matrix. Copyright © 2016 Elsevier B.V. All rights reserved.

Preparative isolation and purification of four flavonoids from the petals of Nelumbo nucifera by high-speed counter-current chromatography.

PubMed

Xingfeng, Guo; Daijie, Wang; Wenjuan, Duan; Jinhua, Du; Xiao, Wang

2010-01-01

Flavonoids, the primary constituents of the petals of Nelumbo nucifera, are known to have antioxidant properties and antibacterial bioactivities. However, efficient methods for the preparative isolation and purification of flavonoids from this plant are not currently available. To develop an efficient method for the preparative isolation and purification of flavonoids from the petals of N. nucifera by high-speed counter-current chromatography (HSCCC). Following an initial clean-up step on a polyamide column, HSCCC was utilised to separate and purify flavonoids. Purities and identities of the isolated compounds were established by HPLC-PAD, ESI-MS, (1)H-NMR and (13)C-NMR. The separation was performed using a two-phase solvent system composed of ethyl acetate-methanol-water-acetic acid (4 : 1 : 5 : 0.1, by volume), in which the upper phase was used as the stationary phase and the lower phase was used as the mobile phase at a flow-rate of 1.0 mL/min in the head-to-tail elution mode. Ultimately, 5.0 mg syringetin-3-O-beta-d-glucoside, 6.5 mg quercetin-3-O-beta-d-glucoside, 12.8 mg isorhamnetin-3-O-beta-d-glucoside and 32.5 mg kaempferol-3-O-beta-d-glucoside were obtained from 125 mg crude sample. The combination of HSCCC with a polyamide column is an efficient method for the preparative separation and purification of flavonoids from the petals of N. nucifera. (c) 2009 John Wiley & Sons, Ltd.

Permeability evolution of shale during spontaneous imbibition

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

Chakraborty, N.; Karpyn, Z. T.; Liu, S.

Shales have small pore and throat sizes ranging from nano to micron scales, low porosity and limited permeability. The poor permeability and complex pore connectivity of shales pose technical challenges to (a) understanding flow and transport mechanisms in such systems and, (b) in predicting permeability changes under dynamic saturation conditions. This paper presents quantitative experimental evidence of the migration of water through a generic shale core plug using micro CT imaging. In addition, in-situ measurements of gas permeability were performed during counter-current spontaneous imbibition of water in nano-darcy permeability Marcellus and Haynesville core plugs. It was seen that water blocksmore » severely reduced the effective permeability of the core plugs, leading to losses of up to 99.5% of the initial permeability in experiments lasting 30 days. There was also evidence of clay swelling which further hindered gas flow. When results from this study were compared with similar counter-current gas permeability experiments reported in the literature, the initial (base) permeability of the rock was found to be a key factor in determining the time evolution of effective gas permeability during spontaneous imbibition. With time, a recovery of effective permeability was seen in the higher permeability rocks, while becoming progressively detrimental and irreversible in tighter rocks. Finally, these results suggest that matrix permeability of ultra-tight rocks is susceptible to water damage following hydraulic fracturing stimulation and, while shut-in/soaking time helps clearing-up fractures from resident fluid, its effect on the adjacent matrix permeability could be detrimental.« less

Permeability evolution of shale during spontaneous imbibition

DOE PAGES

Chakraborty, N.; Karpyn, Z. T.; Liu, S.; ...

2017-01-05

Shales have small pore and throat sizes ranging from nano to micron scales, low porosity and limited permeability. The poor permeability and complex pore connectivity of shales pose technical challenges to (a) understanding flow and transport mechanisms in such systems and, (b) in predicting permeability changes under dynamic saturation conditions. This paper presents quantitative experimental evidence of the migration of water through a generic shale core plug using micro CT imaging. In addition, in-situ measurements of gas permeability were performed during counter-current spontaneous imbibition of water in nano-darcy permeability Marcellus and Haynesville core plugs. It was seen that water blocksmore » severely reduced the effective permeability of the core plugs, leading to losses of up to 99.5% of the initial permeability in experiments lasting 30 days. There was also evidence of clay swelling which further hindered gas flow. When results from this study were compared with similar counter-current gas permeability experiments reported in the literature, the initial (base) permeability of the rock was found to be a key factor in determining the time evolution of effective gas permeability during spontaneous imbibition. With time, a recovery of effective permeability was seen in the higher permeability rocks, while becoming progressively detrimental and irreversible in tighter rocks. Finally, these results suggest that matrix permeability of ultra-tight rocks is susceptible to water damage following hydraulic fracturing stimulation and, while shut-in/soaking time helps clearing-up fractures from resident fluid, its effect on the adjacent matrix permeability could be detrimental.« less

Modeling of heat transfer in a vascular tissue-like medium during an interstitial hyperthermia process.

PubMed

Hassanpour, Saeid; Saboonchi, Ahmad

2016-12-01

This paper aims to evaluate the role of small vessels in heat transfer mechanisms of a tissue-like medium during local intensive heating processes, for example, an interstitial hyperthermia treatment. To this purpose, a cylindrical tissue with two co- and counter-current vascular networks and a central heat source is introduced. Next, the energy equations of tissue, supply fluid (arterial blood), and return fluid (venous blood) are derived using porous media approach. Then, a 2D computer code is developed to predict the temperature of blood (fluid phase) and tissue (solid phase) by conventional volume averaging method and a more realistic solution method. In latter method, despite the volume averaging the blood of interconnect capillaries is separated from the arterial and venous blood phases. It is found that in addition to blood perfusion rate, the arrangement of vascular network has considerable effects on the pattern and amount of the achieved temperature. In contrast to counter-current network, the co-current network of vessels leads to considerable asymmetric pattern of temperature contours and relocation of heat affected zone along the blood flow direction. However this relocation can be prevented by changing the site of hyperthermia heat source. The results show that the cooling effect of co-current blood vessels during of interstitial heating is more efficient. Despite much anatomical dissimilarities, these findings can be useful in designing of protocols for hyperthermia cancer treatment of living tissue. Copyright © 2016 Elsevier Ltd. All rights reserved.

Thermal and single frequency counter-current ultrasound pretreatments of sodium caseinate: enzymolysis kinetics and thermodynamics, amino acids composition, molecular weight distribution and antioxidant peptides.

PubMed

Abdualrahman, Mohammed Adam Y; Ma, Haile; Zhou, Cunshan; Yagoub, Abu ElGasim A; Hu, Jiali; Yang, Xue

2016-12-01

Due to the disadvantages of traditional enzymolysis, pretreatments are crucial to enhance protein enzymolysis. Enzymolysis kinetics and thermodynamics, amino acids composition, molecular weight distribution, fluorescence spectroscopy and antioxidant activity of thermal (HT) and single frequency counter-current ultrasound (SCFU) pretreated sodium caseinate (NaCas) were studied. Enzymolysis of untreated NaCas (control) improved significantly (P < 0.05) by SFCU and followed by HT. Values of the Michaelis-Menten constant (K M ) of SFCU and HT were 0.0212 and 0.0250, respectively. HT and SFCU increased (P < 0.05) the reaction rate constant (k) by 38.64 and 90.91%, respectively at 298 K. k values decreased with increasing temperature. The initial activation energy (46.39 kJ mol -1 ) reduced (P < 0.05) by HT (39.66 kJ mol -1 ) and further by SFCU (33.42 kJ mol -1 ). SFCU-pretreated NaCas hydrolysates had the highest contents of hydrophobic, aromatic, positively and negatively charged amino acids. Medium-sized peptides (5000-1000 Da) are higher in SFCU (78.11%) than HT and the control. SFCU induced molecular unfolding of NaCas proteins. Accordingly, SFCU-pretreated NaCas hydrolysate exhibited the highest scavenging activity on DPPH and hydroxyl radicals, reducing power, and iron chelating ability. SFCU pretreatment would be a useful tool for production of bioactive peptides from NaCas hydrolysate. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Separation of cyclic lipopeptide puwainaphycins from cyanobacteria by countercurrent chromatography combined with polymeric resins and HPLC.

PubMed

Cheel, José; Urajová, Petra; Hájek, Jan; Hrouzek, Pavel; Kuzma, Marek; Bouju, Elodie; Faure, Karine; Kopecký, Jiří

2017-02-01

Puwainaphycins are a recently described group of β-amino fatty acid cyclic lipopeptides of cyanobacterial origin that possess interesting biological activities. Therefore, the development of an efficient method for their isolation from natural sources is necessary. Following the consecutive adsorption of the crude extract on Amberlite XAD-16 and XAD-7 resins, countercurrent chromatography (CCC) was applied to separate seven puwainaphycin variants from a soil cyanobacterium (Cylindrospermum alatosporum CCALA 988). The resin-enriched extract was first fractionated by CCC into fractions I and II with use of the n-hexane-ethyl acetate-ethanol-water (1:5:1:5, v/v/v/v) system at a flow rate of 2 mL min -1 and a rotational speed of 1400 rpm. The CCC separation of fraction I, with use of the ethyl acetate-ethanol-water (5:1:5, v/v/v) system, afforded compounds 1 and 2. The CCC separation of fraction II, with use of the n-hexane-ethyl acetate-ethanol-water (1:5:1:5, v/v/v/v) system, afforded compounds 3-7. In both cases, the lower phases were used as mobile phases at a flow rate of 1 mL min -1 with a rotational speed of 1400 rpm and a temperature of 28 °C. The CCC target fractions obtained were repurified by semipreparative high-performance liquid chromatography (HPLC), leading to compounds 1-7 with purities of 95 %, 95 %, 99 %, 99 %, 95 %, 99 %, and 90 % respectively, as determined by HPLC-electrospray ionization high-resolution mass spectrometry (ESI-HRMS). The chemical identity of the isolated puwainaphycins (compounds 1-7) was confirmed by ESI-HRMS and NMR analyses. Three new puwainaphycin variants (compounds 1, 2, and 5) are reported for the first time. This study provides a new approach for the isolation of puwainaphycins from cyanobacterial biomass. Graphical Abstract Separation of cyclic lipopeptide puwainaphycins from cyanobacteria by countercurrent chromatography combined with polymeric resins and HPLC. Compounds 1 (12-hydroxy-4-methyl-Ahtea-Puw-F), 2 (11-chloro-4-methyl-Ahdoa-Puw-F), 3 (4-methyl-Ahdoa-Puw-F), 4 (4-methyl-Ahdoa-Puw-G), 5 (12-chloro-4-methyl-Ahtea-Puw-F), 6 (4-methyl-Ahtea-Puw-F) and 7 (4-methyl-Ahtea-Puw-G). Ahtea: 3-amino-2-hydroxy tetradecanoic acid. Ahdoa: 3-amino-2-hydroxy dodecanoic acid.

Experimental Demonstration of the Thermochemical Reduction of Ceria in a Solar Aerosol Reactor

PubMed Central

2016-01-01

We report on the experimental demonstration of an aerosol solar reactor for the thermal reduction of ceria, as part of a thermochemical redox cycle for splitting H2O and CO2. The concept utilizes a cavity-receiver enclosing an array of alumina tubes, each containing a downward gravity-driven aerosol flow of ceria particles countercurrent to an inert sweep gas flow for intrinsic separation of reduced ceria and oxygen. A 2 kWth lab-scale prototype with a single tube was tested under radiative fluxes approaching 4000 suns, yielding reaction extents of up to 53% of the thermodynamic equilibrium at 1919 K within residence times below 1 s. Upon thermal redox cycling, fresh primary particles of 2.44 μm mean size initially formed large agglomerates of 1000 μm mean size, then sintered into stable particles of 150 μm mean size. The reaction extent was primarily limited by heat transfer for large particles/agglomerates (mean size > 200 μm) and by the gas phase advection of product O2 for smaller particles. PMID:27853339

Comparison of 2-Octanol and Tributyl Phosphate in Recovery of Tungsten from Sulfuric-Phosphoric Acid Leach Solution of Scheelite

NASA Astrophysics Data System (ADS)

Liao, Yulong; Zhao, Zhongwei

2018-04-01

Tungsten was recovered from sulfuric-phosphoric acid leach solution of scheelite using 2-octanol and tributyl phosphate (TBP). Approximately 76% of the tungsten and less than 6.2% of the iron were extracted when using 70% 2-octanol, showing good selectivity for tungsten over iron; the tungsten extraction could not be significantly enhanced using a three-stage countercurrent simulation test. Moreover, more than 99.2% of the W and 91.0% of the Fe were extracted when using 70% TBP, showing poor selectivity, but after pretreating the leach solution with iron powder, less than 5.5% of the Fe was extracted. The loaded phases were stripped using deionized water and ammonia solution. The maximum stripping rate of tungsten from loaded 2-octanol was 45.6% when using water, compared with only 13.1% from loaded TBP. Tungsten was efficiently stripped from loaded phases using ammonia solution without formation of Fe(OH)3 precipitate. Finally, a flow sheet for recovery of tungsten with TBP is proposed.

Experimental Demonstration of the Thermochemical Reduction of Ceria in a Solar Aerosol Reactor.

PubMed

Welte, Michael; Barhoumi, Rafik; Zbinden, Adrian; Scheffe, Jonathan R; Steinfeld, Aldo

2016-10-12

We report on the experimental demonstration of an aerosol solar reactor for the thermal reduction of ceria, as part of a thermochemical redox cycle for splitting H 2 O and CO 2 . The concept utilizes a cavity-receiver enclosing an array of alumina tubes, each containing a downward gravity-driven aerosol flow of ceria particles countercurrent to an inert sweep gas flow for intrinsic separation of reduced ceria and oxygen. A 2 kW th lab-scale prototype with a single tube was tested under radiative fluxes approaching 4000 suns, yielding reaction extents of up to 53% of the thermodynamic equilibrium at 1919 K within residence times below 1 s. Upon thermal redox cycling, fresh primary particles of 2.44 μm mean size initially formed large agglomerates of 1000 μm mean size, then sintered into stable particles of 150 μm mean size. The reaction extent was primarily limited by heat transfer for large particles/agglomerates (mean size > 200 μm) and by the gas phase advection of product O 2 for smaller particles.

Recovering and recycling Hg from chlor-alkali plant wastewater sludge

NASA Astrophysics Data System (ADS)

Twidwell, L. G.; Thompson, R. J.

2001-01-01

Montana Tech of the University of Montana and Universal Dynamics of British Columbia have developed a hydrometallurgical process for recovering and recycling mercury from chlorine plant wastewater sludge materials (U.S. Environmental Protection Agency [EPA]hazardous-waste classification K106). The hydrometallurgical process is also applicable for the treatment of mercury-contaminated soils (EPA hazardous waste classification D009) and other mercury-bearing waste materials. The process, which is capable of lowering the mercury content in the K106 solids from 10% to <50 mg/kg Hg, has been commercialized and utilized at three U.S. plants. This paper describes the fundamental chemistry of the process, the flowsheet being used, and operating plant case histories.

Observations of the California Countercurrent.

DTIC Science & Technology

1984-06-01

m S. P. Tucker Approved for public release; distribut ion tin] imi ted. UnCLASS IFIED W S4(CWftIY CLASSIVICATIOkO r 7.1% PAGE "Wh., Owe Ent.,eai...Idtinity by block number) - -R6sults from moored current meters, 150-350 m , Uru describec~for ai region over the continental slope off Cape San Martin...from ,.ored current net e r 15) - 35q m , are z2-CUS.eJ tar a region over th1e continental _sioLp, .2 "a,, .San rrtin, Cali orn ra . .I nLlarv 1979 to

Opposed slant tube diabatic sorber

DOEpatents

Erickson, Donald C.

2004-01-20

A sorber comprised of at least three concentric coils of tubing contained in a shell with a flow path for liquid sorbent in one direction, a flow path for heat transfer fluid which is in counter-current heat exchange relationship with sorbent flow, a sorbate vapor port in communication with at least one of sorbent inlet or exit ports, wherein each coil is coiled in opposite direction to those coils adjoining it, whereby the opposed slant tube configuration is achieved, with structure for flow modification in the core space inside the innermost coil.

Biparticle fluidized bed reactor

DOEpatents

Scott, Charles D.; Marasco, Joseph A.

1995-01-01

A fluidized bed reactor system utilizes a fluid phase, a retained fluidized primary particulate phase, and a migratory second particulate phase. The primary particulate phase is a particle such as a gel bead containing an immobilized biocatalyst. The secondary particulate phase, continuously introduced and removed in either cocurrent or countercurrent mode, acts in a secondary role such as a sorbent to continuously remove a product or by-product constituent from the fluid phase. Introduction and removal of the sorbent phase is accomplished through the use of feed screw mechanisms and multivane slurry valves.

Biparticle fluidized bed reactor

DOEpatents

Scott, Charles D.; Marasco, Joseph A.

1996-01-01

A fluidized bed reactor system which utilizes a fluid phase, a retained fluidized primary particulate phase, and a migratory second particulate phase. The primary particulate phase is a particle such as a gel bead containing an immobilized biocatalyst. The secondary and tertiary particulate phases, continuously introduced and removed simultaneously in the cocurrent and countercurrent mode, act in a role such as a sorbent to continuously remove a product or by-product constituent from the fluid phase. Means for introducing and removing the sorbent phases include feed screw mechanisms and multivane slurry valves.

Biparticle fluidized bed reactor

DOEpatents

Scott, C.D.; Marasco, J.A.

1995-04-25

A fluidized bed reactor system utilizes a fluid phase, a retained fluidized primary particulate phase, and a migratory second particulate phase. The primary particulate phase is a particle such as a gel bead containing an immobilized biocatalyst. The secondary particulate phase, continuously introduced and removed in either cocurrent or countercurrent mode, acts in a secondary role such as a sorbent to continuously remove a product or by-product constituent from the fluid phase. Introduction and removal of the sorbent phase is accomplished through the use of feed screw mechanisms and multivane slurry valves. 3 figs.

Biparticle fluidized bed reactor

DOEpatents

Scott, C.D.

1993-12-14

A fluidized bed reactor system which utilizes a fluid phase, a retained fluidized primary particulate phase, and a migratory second particulate phase is described. The primary particulate phase is a particle such as a gel bead containing an immobilized biocatalyst. The secondary particulate phase, continuously introduced and removed in either cocurrent or countercurrent mode, acts in a secondary role such as a sorbent to continuously remove a product or by-product constituent from the fluid phase. Introduction and removal of the sorbent phase is accomplished through the use of feed screw mechanisms and multivane slurry valves. 3 figures.

Biparticle fluidized bed reactor

DOEpatents

Scott, C.D.; Marasco, J.A.

1996-02-27

A fluidized bed reactor system is described which utilizes a fluid phase, a retained fluidized primary particulate phase, and a migratory second particulate phase. The primary particulate phase is a particle such as a gel bead containing an immobilized biocatalyst. The secondary and tertiary particulate phases, continuously introduced and removed simultaneously in the cocurrent and countercurrent mode, act in a role such as a sorbent to continuously remove a product or by-product constituent from the fluid phase. Means for introducing and removing the sorbent phases include feed screw mechanisms and multivane slurry valves. 3 figs.

Biparticle fluidized bed reactor

DOEpatents

Scott, Charles D.

1993-01-01

A fluidized bed reactor system which utilizes a fluid phase, a retained fluidized primary particulate phase, and a migratory second particulate phase. The primary particulate phase is a particle such as a gel bead containing an immobilized biocatalyst. The secondary particulate phase, continuously introduced and removed in either cocurrent or countercurrent mode, acts in a secondary role such as a sorbent to continuously remove a product or by-product constituent from the fluid phase. Introduction and removal of the sorbent phase is accomplished through the use of feed screw mechanisms and multivane slurry valves.

Calculation of wind-driven surface currents in the North Atlantic Ocean

NASA Technical Reports Server (NTRS)

Rees, T. H.; Turner, R. E.

1976-01-01

Calculations to simulate the wind driven near surface currents of the North Atlantic Ocean are described. The primitive equations were integrated on a finite difference grid with a horizontal resolution of 2.5 deg in longitude and latitude. The model ocean was homogeneous with a uniform depth of 100 m and with five levels in the vertical direction. A form of the rigid-lid approximation was applied. Generally, the computed surface current patterns agreed with observed currents. The development of a subsurface equatorial countercurrent was observed.

Parasitic momentum flux in the tokamak core

DOE PAGES

Stoltzfus-Dueck, T.

2017-03-06

A geometrical correction to the E × B drift causes an outward flux of co-current momentum whenever electrostatic potential energy is transferred to ion parallel flows. The robust, fully nonlinear symmetry breaking follows from the free-energy flow in phase space and does not depend on any assumed linear eigenmode structure. The resulting rotation peaking is counter-current and scales as temperature over plasma current. Lastly, this peaking mechanism can only act when fluctuations are low-frequency enough to excite ion parallel flows, which may explain some recent experimental observations related to rotation reversals.

Process and apparatus for solvent extraction of oil from oil-containing diatomite ore

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

Karnofsky, G.B.

1979-09-11

A process is described for solvent extraction of oil-bearing diatomite ore. An apparatus is provided for use therewith, wherein the ore is extracted by countercurrent decantation with a hydrocarbon solvent. The solvent is recovered from the extract by multiple effect evaporation followed by stripping, and the spent diatomite is contacted with water to displace a major portion of the solvent therefrom. The solvent is recovered from the aqueous slurry of the spent diatomite by stripping with steam at superatmospheric pressure. 17 claims.

Open-type miniature heat pipes

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

Vasiliev, L.L.

1994-01-01

The hypothesis that systems of thermoregulation, similar to open-type micro heat pipes, exist in nature (soils, living organisms, plants) and in a number of technological processes (drying, thermodynamic cycles on solid adsorbents) is considered. The hydrodynamics and heat transfer in such thermoregulation systems differ from the hydrodynamics and heat transfer in classical heat pipes, since their geometrical dimensions are extremely small (dozens of microns), adhesion forces are powerful, the effect of the field of capillary and gravitational forces is significant, and strong interaction between counter-current flows of vapor and liquid takes place.

The proportions of different lecithins in the livers of rats deficient in essential fatty acids

PubMed Central

Collins, F. D.

1966-01-01

1. Lecithin was prepared from the livers of rats deficient in essential fatty acids and analysed by means of countercurrent distribution. Thin-layer chromatography showed that only lecithin was present. 2. The distributions of phosphorus and the fatty acids at the 3 and 2 positions were determined. 3. It has been shown that 26% of the fatty acids in the 3 position were unsaturated and that most of the Δ5,8,11-eicosatrienoic acid and the arachidonic acids occur as the stearoyl or oleoyl lecithins. PMID:5965328

Overflows and Upper Ocean Interaction: A Mechanism for the Azores Current

DTIC Science & Technology

2006-09-01

at WHOI. They all saw my ups and downs and I enjoyed their presence in the office during the weekend and late at night. Taka Ito and Masa Sugiyama, my...Countercurrent forms near 380 N with a transport of 2 Sv. This location is 1 degree further north compared to the two-layer model (Figure 3-2) but... 380 N (see Section 1.4.3 for details). Although the origin and the transport of this current is still unclear, the study suggests the formation of

AFS-2 FLOWSHEET MODIFICATIONS TO ADDRESS THE INGROWTH OF PU(VI) DURING METAL DISSOLUTION

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

Crapse, K.; Rudisill, T.; O'Rourke, P.

2014-07-02

In support of the Alternate Feed Stock Two (AFS-2) PuO{sub 2} production campaign, Savannah River National Laboratory (SRNL) conducted a series of experiments concluding that dissolving Pu metal at 95°C using a 6–10 M HNO{sub 3} solution containing 0.05–0.2 M KF and 0–2 g/L B could reduce the oxidation of Pu(IV) to Pu(VI) as compared to dissolving Pu metal under the same conditions but at or near the boiling temperature. This flowsheet was demonstrated by conducting Pu metal dissolutions at 95°C to ensure that PuO{sub 2} solids were not formed during the dissolution. These dissolution parameters can be used formore » dissolving both Aqueous Polishing (AP) and MOX Process (MP) specification materials. Preceding the studies reported herein, two batches of Pu metal were dissolved in the H-Canyon 6.1D dissolver to prepare feed solution for the AFS-2 PuO{sub 2} production campaign. While in storage, UV-visible spectra obtained from an at-line spectrophotometer indicated the presence of Pu(VI). Analysis of the solutions also showed the presence of Fe, Ni, and Cr. Oxidation of Pu(IV) produced during metal dissolution to Pu(VI) is a concern for anion exchange purification. Anion exchange requires Pu in the +4 oxidation state for formation of the anionic plutonium(IV) hexanitrato complex which absorbs onto the resin. The presence of Pu(VI) in the anion feed solution would require a valence adjustment step to prevent losses. In addition, the presence of Cr(VI) would result in absorption of chromate ion onto the resin and could limit the purification of Pu from Cr which may challenge the purity specification of the final PuO{sub 2} product. Initial experiments were performed to quantify the rate of oxidation of Pu(IV) to Pu(VI) (presumed to be facilitated by Cr(VI)) as functions of the HNO{sub 3} concentration and temperature in simulated dissolution solutions containing Cr, Fe, and Ni. In these simulated Pu dissolutions studies, lowering the temperature from near boiling to 95 °C reduced the oxidation rate of Pu(IV) to Pu(VI). For 8.1 M HNO{sub 3} simulated dissolution solutions, at near boiling conditions >35% Pu(VI) was present in 50 h while at 95 °C <10% Pu(VI) was present at 50 h. At near boiling temperatures, eliminating the presence of Cr and varying the HNO{sub 3} concentration in the range of 7–8.5 M had little effect on the rate of conversion of Pu(IV) to Pu(VI). HNO{sub 3} oxidation of Pu(IV) to Pu(VI) in a pure solution has been reported previously. Based on simulated dissolution experiments, this study concluded that dissolving Pu metal at 95°C using a 6 to 10 M HNO{sub 3} solution 0.05–0.2 M KF and 0–2 g/L B could reduce the rate of oxidation of Pu(IV) to Pu(VI) as compared to near boiling conditions. To demonstrate this flowsheet, two small-scale experiments were performed dissolving Pu metal up to 6.75 g/L. No Pu-containing residues were observed in the solutions after cooling. Using Pu metal dissolution rates measured during the experiments and a correlation developed by Holcomb, the time required to completely dissolve a batch of Pu metal in an H-Canyon dissolver using this flowsheet was estimated to require nearly 5 days (120 h). This value is reasonably consistent with an estimate based on the Batch 2 and 3 dissolution times in the 6.1D dissolver and Pu metal dissolution rates measured in this study and by Rudisill et al. Data from the present and previous studies show that the Pu metal dissolution rate decreases by a factor of approximately two when the temperature decreased from boiling (112 to 116°C) to 95°C. Therefore, the time required to dissolve a batch of Pu metal in an H-Canyon dissolver at 95°C would likely double (from 36 to 54 h) and require 72 to 108 h depending on the surface area of the Pu metal. Based on the experimental studies, a Pu metal dissolution flowsheet utilizing 6–10 M HNO{sub 3} containing 0.05–0.2 M KF (with 0–2 g/L B) at 95°C is recommended to reduce the oxidation of Pu(IV) to Pu(VI) as compared to near boiling conditions. The time required to completely dissolve a batch of Pu metal will increase, however, by approximately a factor of two as compared to initial dissolutions at near boiling (assuming the KF concentration is maintained at nominally 0.1 M). By lowering the temperature to 95°C under otherwise the same operating parameters as previous dissolutions, the Pu(VI) concentration should not exceed 15% after a 120 h heating cycle. Increasing the HNO{sub 3} concentration and lowering Pu concentration are expected to further limit the amount of Pu(VI) formed.« less

Direct current hybrid breakers: A design and its realization

NASA Astrophysics Data System (ADS)

Atmadji, Ali Mahfudz Surya

2000-12-01

The use of semiconductors for electric power circuit breakers instead of conventional breakers remains a utopia when designing fault current interrupters for high power networks. The major problems concerning power semiconductor circuit breakers are the excessive heat losses and their sensitivity to transients. However, conventional breakers are capable of dealing with such matters. A combination of the two methods, or so-called `hybrid breakers', would appear to be a solution; however, hybrid breakers use separate parallel branches for conducting the main current and interrupting the short-circuit current. Such breakers are intended for protecting direct current (DC) traction systems. In this thesis hybrid switching techniques for current limitation and purely solidstate current interruption are investigated for DC breakers. This work analyzes the transient behavior of hybrid breakers and compares their operations with conventional breakers and similar solid-state devices in DC systems. Therefore a hybrid breaker was constructed and tested in a specially designed high power test circuit. A vacuum breaker was chosen as the main breaker in the main conducting path; then a commutation path was connected across the vacuum breaker where it provided current limitation and interruption. The commutation path operated only during any current interruption and the process required additional circuits. These included a certain energy storage, overvoltage suppressor and commutation switch. So that when discharging this energy, a controlled counter-current injection could be produced. That counter-current opposed the main current in the breaker by superposition in order to create a forced current-zero. One-stage and two-stage commutation circuits have been treated extensively. This study project contains both theoretical and experimental investigations. A direct current shortcircuit source was constructed capable of delivering power equivalent to a fault. It supplied a direct voltage of 1kVDC which was rectified having been obtained from a 3-phase lOkV/380V supply. The source was successfully tested to deliver a fault current of 7kA with a time constant of 5ms. The hybrid breaker that was developed could provide protection for 750VDC traction systems. The breaker was equipped with a fault- recognizing circuit based on a current level triggering. An electronic circuit was built for this need and was included in the system. It monitored the system continuously and took action by generating trip signals when a fault was recognized. Interruption was followed by a suitable timing of the fast contact separation in the main breaker and the current-zero creation. An electrodynamically driven mechanism was successfully tested having a dead-time of 300μs to separate the main breaker contacts. Furthermore, a maximum peak current injection of RA at a frequency of 500Hz could be obtained in order to produce an artificial current-zero in the vacuum breaker. A successful current interruption with a prospective value of RA was achieved by the hybrid switching technique. In addition, measures were taken to prevent overvoltages. Experimentally, the concept of a hybrid breaker was compared with the functioning of all mechanical (air breaker) and all electronical (IGCT breaker) versions. Although a single stage interrupting method was verified experimentally, two two-stage interrupting methods were analyzed theoretically.

Establishment of the roadmap for chlorination process development for zirconium recovery and recycle

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

Collins, E.D.; Del Cul, G.D.; Spencer, B.B.

Process development studies are being conducted to recover, purify, and reuse the zirconium (about 98.5% by mass) in used nuclear fuel (UNF) zirconium alloy cladding. Feasibility studies began in FY 2010 using empty cladding hulls that were left after fuel dissolution or after oxidation to a finely divided oxide powder (voloxidation). In FY 2012, two industrial teams (AREVA and Shaw-Westinghouse) were contracted by the Department of Energy Office of Nuclear Energy (NE) to provide technical assistance to the project. In FY 2013, the NE Fuel Cycle Research and Development Program requested development of a technology development roadmap to guide futuremore » work. The first step in the roadmap development was to assess the starting point, that is, the current state of the technology and the end goal. Based on previous test results, future work is to be focused on first using chlorine as the chlorinating agent and secondly on the use of a process design that utilizes a chlorination reactor and dual ZrCl{sub 4} product salt condensers. The likely need for a secondary purification step was recognized. Completion of feasibility testing required an experiment on the chemical decladding flowsheet option. This was done during April 2013. The roadmap for process development will continue through process chemistry optimization studies, the chlorinated reactor design configuration, product salt condensers, and the off-gas trapping of tritium or other volatile fission products from the off-gas stream. (authors)« less

ASPEN simulation of a fixed-bed integrated gasification combined-cycle power plant

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

Stone, K.R.

1986-03-01

A fixed-bed integrated gasification combined-cycle (IGCC) power plant has been modeled using the Advanced System for Process ENgineering (ASPEN). The ASPEN simulation is based on a conceptual design of a 509-MW IGCC power plant that uses British Gas Corporation (BGC)/Lurgi slagging gasifiers and the Lurgi acid gas removal process. The 39.3-percent thermal efficiency of the plant that was calculated by the simulation compares very favorably with the 39.4 percent that was reported by EPRI. The simulation addresses only thermal performance and does not calculate capital cost or process economics. Portions of the BGC-IGCC simulation flowsheet are based on the SLAGGERmore » fixed-bed gasifier model (Stefano May 1985), and the Kellogg-Rust-Westinghouse (KRW) iGCC, and the Texaco-IGCC simulations (Stone July 1985) that were developed at the Department of Energy (DOE), Morgantown Energy Technology Center (METC). The simulation runs in 32 minutes of Central Processing Unit (CPU) time on the VAX-11/780. The BGC-IGCC simulation was developed to give accurate mass and energy balances and to track coal tars and environmental species such as SO/sub x/ and NO/sub x/ for a fixed-bed, coal-to-electricity system. This simulation is the third in a series of three IGCC simulations that represent fluidized-bed, entrained-flow, and fixed-bed gasification processes. Alternate process configurations can be considered by adding, deleting, or rearranging unit operation blocks. The gasifier model is semipredictive; it can properly respond to a limited range of coal types and gasifier operating conditions. However, some models in the flowsheet are based on correlations that were derived from the EPRI study, and are therefore limited to coal types and operating conditions that are reasonably close to those given in the EPRI design. 4 refs., 7 figs., 2 tabs.« less

Analysis of maximum allowable fragment heights during dissolution of high flux isotope reactor fuel in an h-canyon dissolver

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

Daniel, G.; Rudisill, T.

2017-07-17

As part of the Spent Nuclear Fuel (SNF) processing campaign, H-Canyon is planning to begin dissolving High Flux Isotope Reactor (HFIR) fuel in late FY17 or early FY18. Each HFIR fuel core contains inner and outer fuel elements which were fabricated from uranium oxide (U 3O 8) dispersed in a continuous Al phase using traditional powder metallurgy techniques. Fuels fabricated in this manner, like other SNF’s processed in H-Canyon, dissolve by the same general mechanisms with similar gas generation rates and the production of H 2. The HFIR fuel cores will be dissolved using a flowsheet developed by the Savannahmore » River National Laboratory (SRNL) in either the 6.4D or 6.1D dissolver using a unique insert. Multiple cores will be charged to the same dissolver solution maximizing the concentration of dissolved Al. The recovered U will be down-blended into low-enriched U for subsequent use as commercial reactor fuel. During the development of the HFIR fuel dissolution flowsheet, the cycle time for the initial core was estimated at 28 to 40 h. Once the cycle is complete, H-Canyon personnel will open the dissolver and probe the HFIR insert wells to determine the height of any fuel fragments which did not dissolve. Before the next core can be charged to the dissolver, an analysis of the potential for H 2 gas generation must show that the combined surface area of the fuel fragments and the subsequent core will not generate H 2 concentrations in the dissolver offgas which exceeds 60% of the lower flammability limit (LFL) of H 2 at 200 °C. The objective of this study is to identify the maximum fuel fragment height as a function of the Al concentration in the dissolving solution which will provide criteria for charging successive HFIR cores to an H-Canyon dissolver.« less

Solvent system selectivities in countercurrent chromatography using Salicornia gaudichaudiana metabolites as practical example with off-line electrospray mass-spectrometry injection profiling.

PubMed

Costa, Fernanda das Neves; Jerz, Gerold; Figueiredo, Fabiana de Souza; Winterhalter, Peter; Leitão, Gilda Guimarães

2015-03-13

For the development of an efficient two-stage isolation process for high-speed countercurrent chromatography (HSCCC) with focus on principal metabolites from the ethyl acetate extract of the halophyte plant Salicornia gaudichaudiana, separation selectivities of two different biphasic solvent systems with similar polarities were evaluated using the elution and extrusion approach. Efficiency in isolation of target compounds is determined by the solvent system selectivity and their chronological use in multiple separation steps. The system n-hexane-ethyl acetate-methanol-water (0.5:6:0.5:6, v/v/v/v) resulted in a comprehensive separation of polyphenolic glycosides. The system n-hexane-n-butanol-water (1:1:2, v/v/v) was less universal but was highly efficient in the fractionation of positional isomers such as di-substituted cinnamic acid quinic acid derivatives. Multiple metabolite detection performed on recovered HSCCC tube fractions was done with rapid mass-spectrometry profiling by sequential off-line injections to electrospray mass-spectrometry (ESI-MS/MS). Selective ion traces of metabolites delivered reconstituted preparative HSCCC runs. Molecular weight distribution of target compounds in single HSCCC tube fractions and MS/MS fragment data were available. Chromatographic areas with strong co-elution effects and fractions of pure recoverable compounds were visualized. In total 11 metabolites have been identified and monitored. Result of this approach was a fast isolation protocol for S. gaudichaudiana metabolites using two solvent systems in a strategic sequence. The process could easily be scaled-up to larger lab-scale or industrial recovery. Copyright © 2015 Elsevier B.V. All rights reserved.

Combination of Sonodynamic and Photodynamic Therapy against Cancer Would Be Effective through Using a Regulated Size of Nanoparticles

PubMed Central

Miyoshi, N.; Kundu, S. K.; Tuziuti, T.; Yasui, K.; Shimada, I.; Ito, Y.

2016-01-01

Nanoparticles have been used for many functional materials in nano-sciences and photo-catalyzing surface chemistry. The titanium oxide nanoparticles will be useful for the treatment of tumor by laser and/or ultrasound as the sensitizers in nano-medicine. We have studied the combination therapy of photo- and sono-dynamic therapies in an animal tumor model. Oral-administration of two sensitizers titanium oxide, 0.2%-TiO2 nanoparticles for sono-dynamic and 1 mM 5-aminolevulinic acid for photodynamic therapies have resulted in the best combination therapeutic effects for the cancer treatment. Our light microscopic and Raman spectroscopic studies revealed that the titanium nanoparticles were distributed inside the blood vessel of the cancer tissue (1–3 μm sizes). Among these nanoparticles with a broad size distribution, only particular-sized particles could penetrate through the blood vessel of the cancer tissue, while other particles may only exhibit the side effects in the model mouse. Therefore, it may be necessary to separate the optimum size particles. For this purpose we have separated TiO2 nanoparticles by countercurrent chromatography with a flat coiled column (1.6 mm ID) immersed in an ultrasonic bath (42 KHz). Separation was performed with a two-phase solvent system composed of 1-butanol-acetic acid-water at a volume ratio of 4:1:5 at a flow rate of 0.1 ml/min. Countercurrent chromatographic separation yielded fractions containing particle aggregates at 31 and 4400 nm in diameter. PMID:27088115

Flavonoids from the flowers of Impatiens glandulifera Royle isolated by high performance countercurrent chromatography.

PubMed

Vieira, Mariana N; Winterhalter, Peter; Jerz, Gerold

2016-01-01

Impatiens glandulifera Royle (Balsaminaceae) is an annual herb from the Himalaya region, currently widespread along European river systems and one of the most important neophyte invading plants in Germany. Exploring the effects of allelopathic plant chemicals is important for the understanding of its ecological impacts in the process of suppression of indigenous plant species. To investigate the chemical composition of Impatiens glandulifera flowers (IGFs) using high performance countercurrent chromatography (HPCCC). The flowers of Impatiens glandulifera were manually separated and extracted with ethanol. LC-ESI-MS/MS was used to characterise the crude extract of IGF. The various flavonoids detected were isolated by HPCCC using of methyl tert-butyl ether-acetonitrile-water (2:2:3, v/v/v). The combination of the data provided by preparative ESI-MS/MS metabolite profiling, LC-ESI-MS/MS, UV-vis and 1D/2D-NMR spectroscopic analysis was used to elucidate the structures of the isolated compounds. HPCCC runs led to the direct isolation of pure dihydromyricetin (ampelopsin), eriodictyol-7-O-glucoside, kaempferol-3-O-glucoside (astragalin) and kaempferol-3-O-6"-malonyl-glucoside, as well as the pre-purification of kaempferol-3-O-rhamno-rhamnosyldiglucoside, quercetin-3-O-galactoside (hyperoside), quercetin and kaempferol in a single step. This is the first report on the flavonoid composition of the species Impatiens glandulifera. The developed protocol was successfully used to isolate the main flavonoids from the crude extract of IGFs. This combined HPCCC and HPLC procedure could be applied to the fast fractionation and recovery of flavonoid derivatives of other plant extracts. Copyright © 2016 John Wiley & Sons, Ltd.

Preparative isolation and purification of three stilbene glycosides from the tibetan medicinal plant Rheum tanguticum maxim. Ex Balf. by high-speed counter-current chromatography.

PubMed

Zhao, Xiao-Hui; Han, Fa; Li, Yu-Lin; Yue, Hui-Lan

2013-02-01

Stilbene glycosides are the primary constituents of Rheum tanguticum Maxim. ex Balf., to which different bioactivities has been attributed, including: anti-HIV, anti-oxidant, anti-tumour, anti-malarial, and anti-allergy activity. However, effective methods for the isolation and purification of stilbene glycosides, such as trans-rhapontin, cis-rhapontin and trans-desoxyrhaponticin, from this herb are not currently available. To develop an efficient method for the preparative isolation and purification of three stilbene glycosides from Rheum tanguticum Maxim. ex Balf. via high-speed counter-current chromatography (HSCCC). A solvent system composed of chloroform:n-butanol:methanol:water (4:1:3:2, v/v/v/v) was developed for the separation. The upper phase was used as the stationary phase, and the lower phase was used as the mobile phase. The flow rate was 1.8 mL/min. The apparatus was controlled at 800 rpm and 25 °C, and the effluent was monitored at 280 nm. Chemical constituents were analysed by high-performance liquid chromatography (HPLC), and their structures were identified by ¹H- and ¹³C-NMR. Under the optimised conditions, 25.5 mg trans-rhapontin, 16.0 mg cis-rhapontin and 20.5 mg trans-desoxyrhaponticin were separated from 80 mg crude sample; the isolates had purities of 99.6, 97.2 and 99.2%, respectively. A simple and efficient HSCCC method has been optimised for the preparative separation of stilbene glycosides from Rheum tanguticum Maxim. ex Balf. Copyright © 2012 John Wiley & Sons, Ltd.

Studies on polar high-speed counter-current chromatographic systems in separation of amaranthine-type betacyanins from Celosia species.

PubMed

Spórna-Kucab, Aneta; Milo, Angelika; Kumorkiewicz, Agnieszka; Wybraniec, Sławomir

2018-01-15

Betacyanins, natural plant pigments exhibiting antioxidant and chemopreventive properties, were extracted from Celosia spicata (Thouars) Spreng. inflorescences and separated by high-speed counter-current chromatography (HSCCC) in two polar solvent systems composed of: TBME - 1-BuOH - ACN - H 2 O (0.7% HFBA, 2:2:1:5, v/v/v/v) (system I) and EtOH - ACN - 1-PrOH - (NH 4 ) 2 SO 4satd.soln - H 2 O (0.5:0.5:0.5:1.2:1, v/v/v/v/v) (system II). The systems were used in the head-to-tail (system I) and tail-to-head (system II) mode. The flow rate of the mobile phase was 2.0 ml/min and the column rotation speed was 860 rpm. The retention of the stationary phase was 73.5% (system I) and 80.0% (system II). For the identification of separated betacyanins in the crude extract as well as in the HSCCC fractions, LC-DAD-ESI-MS/MS analyses were performed. Depending on the target compounds, each of the systems exhibit meaningfully different selectivity and applicability. For the pairs of amaranthines (1/1') and betanins (2/2'), the best choice is the system II, but the acylated amaranthine pairs (3/3' and 4/4') can be resolved only in the ion-pair system I. For the indication of the most suitable solvent system for Celosia plumosa hort., Celosia cristata L. and Celosia spicata (Thouars) Spreng. species, the profiles of betacyanins in different plant parts were studied. Copyright © 2017. Published by Elsevier B.V.

Ion-pair high-speed countercurrent chromatography in fractionation of a high-molecular weight variation of acyl-oligosaccharide linked betacyanins from purple bracts of Bougainvillea glabra.

PubMed

Wybraniec, Sławomir; Jerz, Gerold; Gebers, Nadine; Winterhalter, Peter

2010-02-15

The natural pigment composition of purple bracts of Bougainvillea glabra (Nyctaginaceae) consists of a highly complex mixture of betacyanins solely differing by the substitution with a variety of acyl-oligoglycoside units. This study was focused on a two-dimensional chromatography approach, a combination of preparative high-speed countercurrent chromatography (HSCCC) and analytical C18-HPLC with ESI-DAD-MS/MS detection which finally enabled a more detailed view into the pigment profile and elucidated the existence of an overwhelming amount of varying betacyanin structures occurring in Bougainvillea bracts. The detected molecular weights of the pigments reached so far unknown high values and ranged up to maximum values of 1653 and 1683 Da for the largest molecules due to oligosaccharide linkage and multiple acyl substitutions. The preparative IP-HSCCC separation yielded 15 complex fractions containing betacyanins of enhanced polarity as well as structures with highly increased lipophilicity. Betacyanin structures extended by large oligosaccharide chains with bigger number of glycoside units and also carrying a reduced number of hydroxycinnamic acid substitutions were characteristic for polar pigments occurring mainly in the early eluting CCC fractions. IP-HSCCC was proven to be extremely effective for fractionating this complex crude betalain pigment extract into more defined 'polarity-windows'. Structural analysis by analytical LC-ESI-MS/MS in the positive ionization mode detected a total sum of 146 different betacyanin pigments in the CCC fractions of reduced complexity. Copyright 2010 Elsevier B.V. All rights reserved.

Isolation and identification of phenolic compounds from rum aged in oak barrels by high-speed countercurrent chromatography/high-performance liquid chromatography-diode array detection-electrospray ionization mass spectrometry and screening for antioxidant activity.

PubMed

Regalado, Erik L; Tolle, Sebastian; Pino, Jorge A; Winterhalter, Peter; Menendez, Roberto; Morales, Ana R; Rodríguez, José L

2011-10-14

Beverages, especially wines are well-known to contain a variety of health-beneficial bioactive substances, mainly of phenolic nature which frequently exhibit antioxidant activity. Significant information is available about the separation and identification of polyphenols from some beverages by chromatographic and spectroscopic techniques, but considerably poor is chemical data related to the polyphenolic content in rums. In this paper, a method involving the all-liquid chromatographic technique of high-speed countercurrent chromatography (HSCCC) combined with high-performance liquid chromatography coupled with diode-array detection and electrospray ionization mass spectrometry (HPLC-DAD-ESI-MS(n)) has been successfully applied for separation and identification of phenolic compounds in an aged rum. Besides, the phenolic fraction (PF) was assayed for its antioxidant effects using three different free radical in vitro assays (DPPH·, RO(2)· and spontaneous lipid peroxidation (LPO) on brain homogenates) and on ferric reducing antioxidant power (FRAP). Results showed that PF potently scavenged DPPH and strongly scavenged peroxyl radicals compared to ascorbic acid and butylated hydroxytoluene (BHT); and almost equally inhibited LPO on brain homogenates subjected to spontaneous LPO when compared to quercetin. Moreover, PF also exhibited strong reducing power. This chemical analysis illustrates the rich array of phenols in the aged rum and represents a rapid and suitable method for the isolation and identification of phenolic compounds from mixtures of considerable complexity, achieving high purity and reproducibility with the use of two separation steps. Copyright © 2011 Elsevier B.V. All rights reserved.

MEMBRANE PROCESS TO SEQUESTER CO2 FROM POWER PLANT FLUE GAS

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

Tim Merkel; Karl Amo; Richard Baker

2009-03-31

The objective of this project was to assess the feasibility of using a membrane process to capture CO2 from coal-fired power plant flue gas. During this program, MTR developed a novel membrane (Polaris™) with a CO2 permeance tenfold higher than commercial CO2-selective membranes used in natural gas treatment. The Polaris™ membrane, combined with a process design that uses a portion of combustion air as a sweep stream to generate driving force for CO2 permeation, meets DOE post-combustion CO2 capture targets. Initial studies indicate a CO2 separation and liquefaction cost of $20 - $30/ton CO2 using about 15% of the plantmore » energy at 90% CO2 capture from a coal-fired power plant. Production of the Polaris™ CO2 capture membrane was scaled up with MTR’s commercial casting and coating equipment. Parametric tests of cross-flow and countercurrent/sweep modules prepared from this membrane confirm their near-ideal performance under expected flue gas operating conditions. Commercial-scale, 8-inch diameter modules also show stable performance in field tests treating raw natural gas. These findings suggest that membranes are a viable option for flue gas CO2 capture. The next step will be to conduct a field demonstration treating a realworld power plant flue gas stream. The first such MTR field test will capture 1 ton CO2/day at Arizona Public Service’s Cholla coal-fired power plant, as part of a new DOE NETL funded program.« less

RELAP5 Analyses of OECD/NEA ROSA-2 Project Experiments on Intermediate-Break LOCAs at Hot Leg or Cold Leg

NASA Astrophysics Data System (ADS)

Takeda, Takeshi; Maruyama, Yu; Watanabe, Tadashi; Nakamura, Hideo

Experiments simulating PWR intermediate-break loss-of-coolant accidents (IBLOCAs) with 17% break at hot leg or cold leg were conducted in OECD/NEA ROSA-2 Project using the Large Scale Test Facility (LSTF). In the hot leg IBLOCA test, core uncovery started simultaneously with liquid level drop in crossover leg downflow-side before loop seal clearing (LSC) induced by steam condensation on accumulator coolant injected into cold leg. Water remained on upper core plate in upper plenum due to counter-current flow limiting (CCFL) because of significant upward steam flow from the core. In the cold leg IBLOCA test, core dryout took place due to rapid liquid level drop in the core before LSC. Liquid was accumulated in upper plenum, steam generator (SG) U-tube upflow-side and SG inlet plenum before the LSC due to CCFL by high velocity vapor flow, causing enhanced decrease in the core liquid level. The RELAP5/MOD3.2.1.2 post-test analyses of the two LSTF experiments were performed employing critical flow model in the code with a discharge coefficient of 1.0. In the hot leg IBLOCA case, cladding surface temperature of simulated fuel rods was underpredicted due to overprediction of core liquid level after the core uncovery. In the cold leg IBLOCA case, the cladding surface temperature was underpredicted too due to later core uncovery than in the experiment. These may suggest that the code has remaining problems in proper prediction of primary coolant distribution.

Small-scale, hydrogen-oxidizing-denitrifying bioreactor for treatment of nitrate-contaminated drinking water.

PubMed

Smith, Richard L; Buckwalter, Seanne P; Repert, Deborah A; Miller, Daniel N

2005-05-01

Nitrate removal by hydrogen-coupled denitrification was examined using flow-through, packed-bed bioreactors to develop a small-scale, cost effective system for treating nitrate-contaminated drinking-water supplies. Nitrate removal was accomplished using a Rhodocyclus sp., strain HOD 5, isolated from a sole-source drinking-water aquifer. The autotrophic capacity of the purple non-sulfur photosynthetic bacterium made it particularly adept for this purpose. Initial tests used a commercial bioreactor filled with glass beads and countercurrent, non-sterile flow of an autotrophic, air-saturated, growth medium and hydrogen gas. Complete removal of 2 mM nitrate was achieved for more than 300 days of operation at a 2-h retention time. A low-cost hydrogen generator/bioreactor system was then constructed from readily available materials as a water treatment approach using the Rhodocyclus strain. After initial tests with the growth medium, the constructed system was tested using nitrate-amended drinking water obtained from fractured granite and sandstone aquifers, with moderate and low TDS loads, respectively. Incomplete nitrate removal was evident in both water types, with high-nitrite concentrations in the bioreactor output, due to a pH increase, which inhibited nitrite reduction. This was rectified by including carbon dioxide in the hydrogen stream. Additionally, complete nitrate removal was accomplished with wastewater-impacted surface water, with a concurrent decrease in dissolved organic carbon. The results of this study using three chemically distinct water supplies demonstrate that hydrogen-coupled denitrification can serve as the basis for small-scale remediation and that pilot-scale testing might be the next logical step.

Small-scale, hydrogen-oxidizing-denitrifying bioreactor for treatment of nitrate-contaminated drinking water

USGS Publications Warehouse

Smith, R.L.; Buckwalter, S.P.; Repert, D.A.; Miller, D.N.

2005-01-01

Nitrate removal by hydrogen-coupled denitrification was examined using flow-through, packed-bed bioreactors to develop a small-scale, cost effective system for treating nitrate-contaminated drinking-water supplies. Nitrate removal was accomplished using a Rhodocyclus sp., strain HOD 5, isolated from a sole-source drinking-water aquifer. The autotrophic capacity of the purple non-sulfur photosynthetic bacterium made it particularly adept for this purpose. Initial tests used a commercial bioreactor filled with glass beads and countercurrent, non-sterile flow of an autotrophic, air-saturated, growth medium and hydrogen gas. Complete removal of 2 mM nitrate was achieved for more than 300 days of operation at a 2-h retention time. A low-cost hydrogen generator/bioreactor system was then constructed from readily available materials as a water treatment approach using the Rhodocyclus strain. After initial tests with the growth medium, the constructed system was tested using nitrate-amended drinking water obtained from fractured granite and sandstone aquifers, with moderate and low TDS loads, respectively. Incomplete nitrate removal was evident in both water types, with high-nitrite concentrations in the bioreactor output, due to a pH increase, which inhibited nitrite reduction. This was rectified by including carbon dioxide in the hydrogen stream. Additionally, complete nitrate removal was accomplished with wastewater-impacted surface water, with a concurrent decrease in dissolved organic carbon. The results of this study using three chemically distinct water supplies demonstrate that hydrogen-coupled denitrification can serve as the basis for small-scale remediation and that pilot-scale testing might be the next logical step.

Spectroscopic methods of process monitoring for safeguards of used nuclear fuel separations

NASA Astrophysics Data System (ADS)

Warburton, Jamie Lee

To support the demonstration of a more proliferation-resistant nuclear fuel processing plant, techniques and instrumentation to allow the real-time, online determination of special nuclear material concentrations in-process must be developed. An ideal materials accountability technique for proliferation resistance should provide nondestructive, realtime, on-line information of metal and ligand concentrations in separations streams without perturbing the process. UV-Visible spectroscopy can be adapted for this precise purpose in solvent extraction-based separations. The primary goal of this project is to understand fundamental URanium EXtraction (UREX) and Plutonium-URanium EXtraction (PUREX) reprocessing chemistry and corresponding UV-Visible spectroscopy for application in process monitoring for safeguards. By evaluating the impact of process conditions, such as acid concentration, metal concentration and flow rate, on the sensitivity of the UV-Visible detection system, the process-monitoring concept is developed from an advanced application of fundamental spectroscopy. Systematic benchtop-scale studies investigated the system relevant to UREX or PUREX type reprocessing systems, encompassing 0.01-1.26 M U and 0.01-8 M HNO3. A laboratory-scale TRansUranic Extraction (TRUEX) demonstration was performed and used both to analyze for potential online monitoring opportunities in the TRUEX process, and to provide the foundation for building and demonstrating a laboratory-scale UREX demonstration. The secondary goal of the project is to simulate a diversion scenario in UREX and successfully detect changes in metal concentration and solution chemistry in a counter current contactor system with a UV-Visible spectroscopic process monitor. UREX uses the same basic solvent extraction flowsheet as PUREX, but has a lower acid concentration throughout and adds acetohydroxamic acid (AHA) as a complexant/reductant to the feed solution to prevent the extraction of Pu. By examining UV-Visible spectra gathered in real time, the objective is to detect the conversion from the UREX process, which does not separate Pu, to the PUREX process, which yields a purified Pu product. The change in process chemistry can be detected in the feed solution, aqueous product or in the raffinate stream by identifying the acid concentration, metal distribution and the presence or absence of AHA. A fiber optic dip probe for UV-Visible spectroscopy was integrated into a bank of three counter-current centrifugal contactors to demonstrate the online process monitoring concept. Nd, Fe and Zr were added to the uranyl nitrate system to explore spectroscopic interferences and identify additional species as candidates for online monitoring. This milestone is a demonstration of the potential of this technique, which lies in the ability to simultaneously and directly monitor the chemical process conditions in a reprocessing plant, providing inspectors with another tool to detect nuclear material diversion attempts. Lastly, dry processing of used nuclear fuel is often used as a head-end step before solvent extraction-based separations such as UREX or TRUEX. A non-aqueous process, used fuel treatment by dry processing generally includes chopping of used fuel rods followed by repeated oxidation-reduction cycles and physical separation of the used fuel from the cladding. Thus, dry processing techniques are investigated and opportunities for online monitoring are proposed for continuation of this work in future studies.