Science.gov

Sample records for liquid waste quantification

  1. The Sonophysics and Sonochemistry of Liquid Waste Quantification and Remediation

    SciTech Connect

    Matula, Thomas J.

    1998-06-01

    This research is being conducted to (a) perform an in-depth and comprehensive study of the fundamentals of acoustic cavitation and nonlinear bubble dynamics, (b) elucidate the fundamental physics of sonochemical reactions, (c) examine the potential of sonoluminescence to quantify and monitor the presence of alkali metals and other elements in waste liquids, (d) design and evaluate more effective sonochemical reactors for waste remediation, and (e) determine the optimal acoustical parameters in the use of sonochemistry for liquid-waste-contaminant remediation. So far cells have been designed for multibubble sonoluminescence (MBSL) and single-bubble sonoluminescence (SBSL) spectroscopy experiments. Positive results have been obtained in both systems using a Raman system which covers the wavelength range from 790 to 1,070 nm. Further progress from year-1 involved the use of the newly discovered technique of changing the pressure head above the cavitation field to increase the light emission from MBSL. A second method for changing the pressure head involves pressure-jumping, whereby the pressure in the head space above the solution is quickly increased to a new steady value.

  2. THE SONOPHYSICS AND SONOCHEMISTRY OF LIQUID WASTE QUANTIFICATION AND REMEDIATION

    EPA Science Inventory

    When an ultrasonic field of moderate to large intensity is applied to a liquid, the liquid often fails under the action of the dynamic tensile stress applied by the ultrasound. Consequently, the vapor cavity that is formed during the rarefaction portion of the sound field can thu...

  3. The sonophysics and sonochemistry of liquid waste quantification and remediation. 1998 annual progress report

    SciTech Connect

    Matula, T.J.

    1998-06-01

    'To perform an in-depth and comprehensive study of the fundamentals of acoustic cavitation and nonlinear bubble dynamics, to elucidate the fundamental physics of sonochemical reactions, to examine the potential of sonoluminescence to quantify and to monitor the presence of alkali metals and other elements in waste liquids, to design and to evaluate more effective sonochemical reactors for waste remediation, and to determine the optimal acoustical parameters in the use of sonochemistry for liquid-waste-contaminant remediation. This report summarizes work performed during year 2 of a 3-year project. The goals included performing near-IR spectroscopy of sonoluminescence. Cells have been designed for multi-bubble sonoluminescence (MBSL) and single-bubble sonoluminescence (SBSL) spectroscopy experiments. The MBSL cells are designed around a 20 kHz acoustic horn with replaceable titanium tips from Sonics and Materials. The horn is pressure-fitted into a stainless steel cell via O-rings and a compression ring, to seal the cell up to 100 psi for pressure experiments. The cell is thermostated by circulating coolant in a jacket, as well as flowing the cell fluid (at 4L/min.) through a temperature control bath. Several ports are located on the cell for gas ports (one for headspace, another for bubbling), a pressure transducer, a thermocouple, a needle hydrophone, and a septum port for addition or withdrawal of samples. The total volume is approximately 80 mL with a 10 mL head space. Directly opposite the horn tip is a 2 cm quartz window against which a fiber optic bundle is placed. Light collected through the fiber optic is imaged onto one of several detection systems.'

  4. FINAL REPORT. THE SONOPHYSICS AND SONOCHEMISTRY OF LIQUID WASTE QUANTIFICATION AND REMEDIATION

    EPA Science Inventory

    The objective of this proposal was to study the physics and chemistry of acoustic cavitation--thatis, the formation, growth, and violent collapse of bubbles--for its eventual application as both an analytical tool for toxic waste identification and monitoring, as well as a cost-...

  5. High-performance liquid chromatography method for the simultaneous quantification of retinol, alpha-tocopherol, and cholesterol in shrimp waste hydrolysate.

    PubMed

    López-Cervantes, J; Sánchez-Machado, D I; Ríos-Vázquez, N J

    2006-02-10

    This study presents an HPLC method for the simultaneous quantification of retinol, alpha-tocopherol, and cholesterol in shrimp waste hydrolysate lipid fraction. The method includes microscale saponification and extraction with n-hexane. Liposoluble vitamins and cholesterol were quantified by HPLC with UV detection (HPLC-UV), on a 25 cm x 0.46 cm SS Exil ODS 5 microm column, mobile phase 68:28:4 (v/v/v) methanol:acetonitrile:water; flow rate 1.4 ml/min; column temperature 36 degrees C. The detection was operated using two channels of a diode-array spectrophotometer, 325 nm for retinol and 208 nm for alpha-tocopherol and cholesterol. With these conditions, the overall recovery was 95.7, 100.8, and 98.0% for retinol, alpha-tocopherol, and cholesterol, respectively. The method precision (relative standard deviation) was 1.83% for retinol, 2.32% for alpha-tocopherol, and 1.98% for cholesterol. This method was used to quantify the cited analytes in the hydrolysate obtained during lactic acid fermentation of shrimp waste. This hydrolysate may be a valuable supplement of nutrients in fish production. PMID:16439259

  6. Immobilization of organic liquid wastes

    SciTech Connect

    Greenhalgh, W.O.

    1985-08-07

    This report describes a portland cement immobilization process for the disposal treatment of radioactive organic liquid wastes which would be generated in a a FFTF fuels reprocessing line. An incineration system already on-hand was determined to be too costly to operate for the 100 to 400 gallons per year organic liquid. Organic test liquids were dispersed into an aqueous phosphate liquid using an emulsifier. A total of 109 gallons of potential and radioactive aqueous immiscible organic liquid wastes from Hanford 300 Area operations were solidified with portland cement and disposed of as solid waste during a 3-month test program with in-drum mixers. Waste packing efficiencies varied from 32 to 40% and included pump oils, mineral spirits, and TBP-NPH type solvents.

  7. Method for treating liquid wastes

    SciTech Connect

    Katti, Kattesh V.; Volkert, Wynn A.; Singh, Prahlad; Ketring, Alan R.

    1995-01-01

    The method of treating liquid waste in a media is accomplished by exposing the media to phosphinimines and sequestering .sup.99 Tc from the media by the phosphinimine (PN) functionalities. The system for treating the liquid waste in the media includes extraction of .sup.99 TcO.sub.4.sup.- from aqueous solutions into organic solvents or mixed organic/polar media, extraction of .sup.99 Tc from solutions on a solid matrix by using a container containing PN functionalities on solid matrices including an inlet and outlet for allowing flow of media through an immobilized phosphinimine ligand system contained within the container. Also, insoluble suspensions of phosphinimine functionalities on solid matrices in liquid solutions or present on supported liquid membranes (SLM) can be used to sequester .sup.99 Tc from those liquids.

  8. Method for treating liquid wastes

    SciTech Connect

    Katti, K.V.; Volkert, W.A.; Singh, P.; Ketring, A.R.

    1995-12-26

    The method of treating liquid waste in a media is accomplished by exposing the media to phosphinimines and sequestering {sup 99}Tc from the media by the phosphinimine (PN) functionalities. The system for treating the liquid waste in the media includes extraction of {sup 99}TcO{sub 4}{sup {minus}} from aqueous solutions into organic solvents or mixed organic/polar media, extraction of {sup 99}Tc from solutions on a solid matrix by using a container containing PN functionalities on solid matrices including an inlet and outlet for allowing flow of media through an immobilized phosphinimine ligand system contained within the container. Also, insoluble suspensions of phosphinimine functionalities on solid matrices in liquid solutions or present on supported liquid membranes (SLM) can be used to sequester {sup 99}Tc from those liquids. 6 figs.

  9. Investigations of Some Liquid Matrixes for Analyte Quantification by MALDI

    NASA Astrophysics Data System (ADS)

    Moon, Jeong Hee; Park, Kyung Man; Ahn, Sung Hee; Lee, Seong Hoon; Kim, Myung Soo

    2015-06-01

    Sample inhomogeneity is one of the obstacles preventing the generation of reproducible mass spectra by MALDI and to their use for the purpose of analyte quantification. As a potential solution to this problem, we investigated MALDI with some liquid matrixes prepared by nonstoichiometric mixing of acids and bases. Out of 27 combinations of acids and bases, liquid matrixes could be produced from seven. When the overall spectral features were considered, two liquid matrixes using α-cyano-4-hydroxycinnamic acid as the acid and 3-aminoquinoline and N,N-diethylaniline as bases were the best choices. In our previous study of MALDI with solid matrixes, we found that three requirements had to be met for the generation of reproducible spectra and for analyte quantification: (1) controlling the temperature by fixing the total ion count, (2) plotting the analyte-to-matrix ion ratio versus the analyte concentration as the calibration curve, and (3) keeping the matrix suppression below a critical value. We found that the same requirements had to be met in MALDI with liquid matrixes as well. In particular, although the liquid matrixes tested here were homogeneous, they failed to display spot-to-spot spectral reproducibility unless the first requirement above was met. We also found that analyte-derived ions could not be produced efficiently by MALDI with the above liquid matrixes unless the analyte was sufficiently basic. In this sense, MALDI processes with solid and liquid matrixes should be regarded as complementary techniques rather than as competing ones.

  10. Electrochemical treatment of liquid wastes

    SciTech Connect

    Hobbs, D.T.

    1997-10-01

    Under this task, electrochemical treatment processes are being evaluated and developed for the destruction of organic compounds and nitrates/nitrites and the removal of other hazardous species from liquid wastes stored throughout the DOE complex. This technology targets the (1) destruction of nitrates, nitrites and organic compounds; (2) removal of radionuclides; and (3) removal of RCRA metals. The development program consists of five major tasks: (1) evaluation of electrochemical reactors for the destruction and removal of hazardous waste components, (2) development and validation of engineering process models, (3) radioactive laboratory-scale tests, (4) demonstration of the technology in an engineering-scale reactor, and (5) analysis and evaluation of test data. The development program team is comprised of individuals from national laboratories, academic institutions, and private industry. Possible benefits of this technology include: (1) improved radionuclide separation as a result of the removal of organic complexants, (2) reduction in the concentrations of hazardous and radioactive species in the waste (e.g., removal of nitrate, mercury, chromium, cadmium, {sup 99}Tc, and {sup 106}Ru), (3) reduction in the size of the off-gas handling equipment for the vitrification of low-level waste (LLW) by reducing the source of NO{sub x} emissions, (4) recovery of chemicals of value (e.g. sodium hydroxide), and (5) reduction in the volume of waste requiring disposal.

  11. A Spanish model for quantification and management of construction waste.

    PubMed

    Solís-Guzmán, Jaime; Marrero, Madelyn; Montes-Delgado, Maria Victoria; Ramírez-de-Arellano, Antonio

    2009-09-01

    Currently, construction and demolition waste (C&D waste) is a worldwide issue that concerns not only governments but also the building actors involved in construction activity. In Spain, a new national decree has been regulating the production and management of C&D waste since February 2008. The present work describes the waste management model that has inspired this decree: the Alcores model implemented with good results in Los Alcores Community (Seville, Spain). A detailed model is also provided to estimate the volume of waste that is expected to be generated on the building site. The quantification of C&D waste volume, from the project stage, is essential for the building actors to properly plan and control its disposal. This quantification model has been developed by studying 100 dwelling projects, especially their bill of quantities, and defining three coefficients to estimate the demolished volume (CT), the wreckage volume (CR) and the packaging volume (CE). Finally, two case studies are included to illustrate the usefulness of the model to estimate C&D waste volume in both new construction and demolition projects. PMID:19523801

  12. A Spanish model for quantification and management of construction waste

    SciTech Connect

    Solis-Guzman, Jaime Marrero, Madelyn; Montes-Delgado, Maria Victoria; Ramirez-de-Arellano, Antonio

    2009-09-15

    Currently, construction and demolition waste (C and D waste) is a worldwide issue that concerns not only governments but also the building actors involved in construction activity. In Spain, a new national decree has been regulating the production and management of C and D waste since February 2008. The present work describes the waste management model that has inspired this decree: the Alcores model implemented with good results in Los Alcores Community (Seville, Spain). A detailed model is also provided to estimate the volume of waste that is expected to be generated on the building site. The quantification of C and D waste volume, from the project stage, is essential for the building actors to properly plan and control its disposal. This quantification model has been developed by studying 100 dwelling projects, especially their bill of quantities, and defining three coefficients to estimate the demolished volume (CT), the wreckage volume (CR) and the packaging volume (CE). Finally, two case studies are included to illustrate the usefulness of the model to estimate C and D waste volume in both new construction and demolition projects.

  13. Radioactive liquid waste treatment facility

    SciTech Connect

    Black, R.L.

    1984-07-01

    The Radioactive Liquid Waste Treatment Facility (RLWTF) at Argonne National Laboratory-West (ANL-W) in Idaho provides improved treatment for low-level aqueous waste compared to conventional systems. A unique, patented evaporated system is used in the RLWTF. SHADE (shielded hot air drum evaporator, US Patent No. 4,305,780) is a low-cost disposable unit constructed from standard components and is self-shielded. The results of testing and recent operations indicate that evaporation rates of 2 to 6 gph (8 to 23 L/h) can be achieved with a single unit housed in a standard 30-gal (114-L) drum container. The operating experience has confirmed the design evaporation rate of 60,000 gal (227,000 L) per year, using six SHADE's. 2 references, 2 figures, 2 tables.

  14. Electrochemical treatment of liquid wastes

    SciTech Connect

    Hobbs, D.

    1996-10-01

    Electrochemical treatment processes are being evaluated and developed for the destruction of organic compounds and nitrates/nitrites and the removal of other hazardous species from liquid wastes stored throughout the DOE complex. This activity consists of five major tasks: (1) evaluation of different electrochemical reactors for the destruction and removal of hazardous waste components, (2) development and validation of engineering process models, (3) radioactive laboratory-scale tests, (4) demonstration of the technology in an engineering-scale size reactor, and (5) analysis and evaluation of testing data. The development program team is comprised of individuals from federal, academic, and private industry. Work is being carried out in DOE, academic, and private industrial laboratories.

  15. Reduction of INTEC Analytical Radioactive Liquid Waste

    SciTech Connect

    Johnson, Virgil James; Hu, Jian Sheng; Chambers, Andrea

    1999-06-01

    This report details the evaluation of the reduction in radioactive liquid waste from the analytical laboratories sent to the Process Effluent Waste system (deep tanks). The contributors are the Analytical Laboratories Department (ALD), the Waste Operations Department, the laboratories at CPP-637, and natural run off. Other labs were contacted to learn of methods used and if any new technologies had emerged. A waste generation database was made from the current methods in use in the ALD. From this database, methods were targeted to reduce waste. Individuals were contacted on ways to reduce waste. The results are: a new method generating much less waste, several methods being handled differently, some cleaning processes being changed to reduce waste, and changes to reduce chemicals to waste.

  16. Reduction of INTEC Analytical Radioactive Liquid Wastes

    SciTech Connect

    V. J. Johnson; J. S. Hu; A. G. Chambers

    1999-06-01

    This report details the evaluation of the reduction in radioactive liquid waste from the analytical laboratories sent to the Process Effluent Waste system (deep tanks). The contributors are the Analytical Laboratories Department (ALD), the Waste Operations Department, the laboratories at CPP-637, and natural run off. Other labs were contacted to learn the methods used and if any new technologies had emerged. A waste generation database was made from the current methods in used in the ALD. From this database, methods were targeted to reduce waste. Individuals were contacted on ways to reduce waste. The results are: a new method generating much less waste, several methods being handled differently, some cleaning processes being changed to reduce waste, and changes to reduce chemicals to waste.

  17. 20 CFR 654.406 - Excreta and liquid waste disposal.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 20 Employees' Benefits 3 2013-04-01 2013-04-01 false Excreta and liquid waste disposal. 654.406... Excreta and liquid waste disposal. (a) Facilities shall be provided and maintained for effective disposal of excreta and liquid waste. Raw or treated liquid waste shall not be discharged or allowed...

  18. 20 CFR 654.406 - Excreta and liquid waste disposal.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 20 Employees' Benefits 3 2010-04-01 2010-04-01 false Excreta and liquid waste disposal. 654.406... Excreta and liquid waste disposal. (a) Facilities shall be provided and maintained for effective disposal of excreta and liquid waste. Raw or treated liquid waste shall not be discharged or allowed...

  19. 20 CFR 654.406 - Excreta and liquid waste disposal.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 20 Employees' Benefits 3 2012-04-01 2012-04-01 false Excreta and liquid waste disposal. 654.406... Excreta and liquid waste disposal. (a) Facilities shall be provided and maintained for effective disposal of excreta and liquid waste. Raw or treated liquid waste shall not be discharged or allowed...

  20. 20 CFR 654.406 - Excreta and liquid waste disposal.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 20 Employees' Benefits 3 2014-04-01 2014-04-01 false Excreta and liquid waste disposal. 654.406... Excreta and liquid waste disposal. (a) Facilities shall be provided and maintained for effective disposal of excreta and liquid waste. Raw or treated liquid waste shall not be discharged or allowed...

  1. 20 CFR 654.406 - Excreta and liquid waste disposal.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 20 Employees' Benefits 3 2011-04-01 2011-04-01 false Excreta and liquid waste disposal. 654.406... Excreta and liquid waste disposal. (a) Facilities shall be provided and maintained for effective disposal of excreta and liquid waste. Raw or treated liquid waste shall not be discharged or allowed...

  2. Method for solidifying liquid radioactive wastes

    DOEpatents

    Berreth, Julius R.

    1976-01-01

    The quantity of nitrous oxides produced during the solidification of liquid radioactive wastes containing nitrates and nitrites can be substantially reduced by the addition to the wastes of a stoichiometric amount of urea which, upon heating, destroys the nitrates and nitrites, liberating nontoxic N.sub.2, CO.sub.2 and NH.sub.3.

  3. Solid and Liquid Waste Drying Bag

    NASA Technical Reports Server (NTRS)

    Litwiller, Eric (Inventor); Hogan, John A. (Inventor); Fisher, John W. (Inventor)

    2009-01-01

    Method and system for processing waste from human activities, including solids, liquids and vapors. A fluid-impermeable bag, lined with a liquid-impermeable but vapor-permeable membrane, defining an inner bag, is provided. A vacuum force is provided to extract vapors so that the waste is moved toward a selected region in the inner bag, extracted vapors, including the waste vapors and vaporized portions of the waste liquids are transported across the membrane, and most or all of the solids remain within the liner. Extracted vapors are filtered, and sanitized components thereof are isolated and optionally stored. The solids remaining within the liner are optionally dried and isolated for ultimate disposal.

  4. Bioprocessing of a stored mixed liquid waste

    SciTech Connect

    Wolfram, J.H.; Rogers, R.D.; Finney, R.

    1995-12-31

    This paper describes the development and results of a demonstration for a continuous bioprocess for mixed waste treatment. A key element of the process is an unique microbial strain which tolerates high levels of aromatic solvents and surfactants. This microorganism is the biocatalysis of the continuous flow system designed for the processing of stored liquid scintillation wastes. During the past year a process demonstration has been conducted on commercial formulation of liquid scintillation cocktails (LSC). Based on data obtained from this demonstration, the Ohio EPA granted the Mound Applied Technologies Lab a treatability permit allowing the limited processing of actual mixed waste. Since August 1994, the system has been successfully processing stored, {open_quotes}hot{close_quotes} LSC waste. The initial LSC waste fed into the system contained 11% pseudocumene and detectable quantities of plutonium. Another treated waste stream contained pseudocumene and tritium. Data from this initial work shows that the hazardous organic solvent, and pseudocumene have been removed due to processing, leaving the aqueous low level radioactive waste. Results to date have shown that living cells are not affected by the dissolved plutonium and that 95% of the plutonium was sorbed to the biomass. This paper discusses the bioprocess, rates of processing, effluent, and the implications of bioprocessing for mixed waste management.

  5. 40 CFR 761.269 - Sampling liquid PCB remediation waste.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Sampling liquid PCB remediation waste... with § 761.61(a)(2) § 761.269 Sampling liquid PCB remediation waste. (a) If the liquid is single phase... liquid is multi-phasic, separate the phases, and collect and analyze a sample from each liquid...

  6. 40 CFR 761.269 - Sampling liquid PCB remediation waste.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Sampling liquid PCB remediation waste... with § 761.61(a)(2) § 761.269 Sampling liquid PCB remediation waste. (a) If the liquid is single phase... liquid is multi-phasic, separate the phases, and collect and analyze a sample from each liquid...

  7. 40 CFR 761.269 - Sampling liquid PCB remediation waste.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 31 2011-07-01 2011-07-01 false Sampling liquid PCB remediation waste... with § 761.61(a)(2) § 761.269 Sampling liquid PCB remediation waste. (a) If the liquid is single phase... liquid is multi-phasic, separate the phases, and collect and analyze a sample from each liquid...

  8. 40 CFR 761.269 - Sampling liquid PCB remediation waste.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Sampling liquid PCB remediation waste... with § 761.61(a)(2) § 761.269 Sampling liquid PCB remediation waste. (a) If the liquid is single phase... liquid is multi-phasic, separate the phases, and collect and analyze a sample from each liquid...

  9. 40 CFR 761.269 - Sampling liquid PCB remediation waste.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 32 2012-07-01 2012-07-01 false Sampling liquid PCB remediation waste... with § 761.61(a)(2) § 761.269 Sampling liquid PCB remediation waste. (a) If the liquid is single phase... liquid is multi-phasic, separate the phases, and collect and analyze a sample from each liquid...

  10. Liquid low level waste management expert system

    SciTech Connect

    Ferrada, J.J.; Abraham, T.J. ); Jackson, J.R. )

    1991-01-01

    An expert system has been developed as part of a new initiative for the Oak Ridge National Laboratory (ORNL) systems analysis program. This expert system will aid in prioritizing radioactive waste streams for treatment and disposal by evaluating the severity and treatability of the problem, as well as the final waste form. The objectives of the expert system development included: (1) collecting information on process treatment technologies for liquid low-level waste (LLLW) that can be incorporated in the knowledge base of the expert system, and (2) producing a prototype that suggests processes and disposal technologies for the ORNL LLLW system. 4 refs., 9 figs.

  11. Process equipment waste and process waste liquid collection systems

    SciTech Connect

    Not Available

    1990-06-01

    The US DOE has prepared an environmental assessment for construction related to the Process Equipment Waste (PEW) and Process Waste Liquid (PWL) Collection System Tasks at the Idaho Chemical Processing Plant. This report describes and evaluates the environmental impacts of the proposed action (and alternatives). The purpose of the proposed action would be to ensure that the PEW and PWL collection systems, a series of enclosed process hazardous waste, and radioactive waste lines and associated equipment, would be brought into compliance with applicable State and Federal hazardous waste regulations. This would be accomplished primarily by rerouting the lines to stay within the buildings where the lined floors of the cells and corridors would provide secondary containment. Leak detection would be provided via instrumented collection sumps locate din the cells and corridors. Hazardous waste transfer lines that are routed outside buildings will be constructed using pipe-in-pipe techniques with leak detection instrumentation in the interstitial area. The need for the proposed action was identified when a DOE-sponsored Resource Conservation and Recovery Act (RCRA) compliance assessment of the ICPP facilities found that singly-contained waste lines ran buried in the soil under some of the original facilities. These lines carried wastes with a pH of less than 2.0, which were hazardous waste according to the RCRA standards. 20 refs., 7 figs., 1 tab.

  12. 324 Bldg Liquid Waste Handling System Functional Design Criteria

    SciTech Connect

    HAM, J.E.

    1999-12-16

    The 324 Building in the 300 Area of the Hanford Site, is preparing to design, construct, and operate the Liquid Waste Handling System (LWHS). The system will include transfer, collection, treatment, and disposal of radiological and mixed liquid waste.

  13. Development of characterization protocol for mixed liquid radioactive waste classification

    SciTech Connect

    Zakaria, Norasalwa; Wafa, Syed Asraf; Wo, Yii Mei; Mahat, Sarimah

    2015-04-29

    Mixed liquid organic waste generated from health-care and research activities containing tritium, carbon-14, and other radionuclides posed specific challenges in its management. Often, these wastes become legacy waste in many nuclear facilities and being considered as ‘problematic’ waste. One of the most important recommendations made by IAEA is to perform multistage processes aiming at declassification of the waste. At this moment, approximately 3000 bottles of mixed liquid waste, with estimated volume of 6000 litres are currently stored at the National Radioactive Waste Management Centre, Malaysia and some have been stored for more than 25 years. The aim of this study is to develop a characterization protocol towards reclassification of these wastes. The characterization protocol entails waste identification, waste screening and segregation, and analytical radionuclides profiling using various analytical procedures including gross alpha/ gross beta, gamma spectrometry, and LSC method. The results obtained from the characterization protocol are used to establish criteria for speedy classification of the waste.

  14. Future radioactive liquid waste streams study

    SciTech Connect

    Rey, A.S.

    1993-11-01

    This study provides design planning information for the Radioactive Liquid Waste Treatment Facility (RLWTF). Predictions of estimated quantities of Radioactive Liquid Waste (RLW) and radioactivity levels of RLW to be generated are provided. This information will help assure that the new treatment facility is designed with the capacity to treat generated RLW during the years of operation. The proposed startup date for the RLWTF is estimated to be between 2002 and 2005, and the life span of the facility is estimated to be 40 years. The policies and requirements driving the replacement of the current RLW treatment facility are reviewed. Historical and current status of RLW generation at Los Alamos National Laboratory are provided. Laboratory Managers were interviewed to obtain their insights into future RLW activities at Los Alamos that might affect the amount of RLW generated at the Lab. Interviews, trends, and investigation data are analyzed and used to create scenarios. These scenarios form the basis for the predictions of future RLW generation and the level of RLW treatment capacity which will be needed at LANL.

  15. Quantification of methane and nitrous oxide emissions from various waste treatment facilities by tracer dilution method

    NASA Astrophysics Data System (ADS)

    Mønster, Jacob; Rella, Chris; Jacobson, Gloria; Kjeldsen, Peter; Scheutz, Charlotte

    2013-04-01

    Urban activities generate solid and liquid waste, and the handling and aftercare of the waste results in the emission of various compounds into the surrounding environment. Some of these compounds are emitted as gasses into the atmosphere, including methane and nitrous oxide. Methane and nitrous oxide are strong greenhouse gases and are considered to have 25 and 298 times the greenhouse gas potential of carbon dioxide on a hundred years term (Solomon et al. 2007). Global observations of both gasses have shown increasing concentrations that significantly contribute to the greenhouse gas effect. Methane and nitrous oxide are emitted from both natural and anthropogenic sources and inventories of source specific fugitive emissions from the anthropogenic sources of methane and nitrous oxide of are often estimated on the basis of modeling and mass balance. Though these methods are well-developed, actual measurements for quantification of the emissions is a very useful tool for verifying the modeling and mass balance as well as for validation initiatives done for lowering the emissions of methane and nitrous oxide. One approach to performing such measurements is the tracer dilution method (Galle et al. 2001, Scheutz et al. 2011), where the exact location of the source is located and a tracer gas is released at this source location at a known flow. The ratio of downwind concentrations of the tracer gas and the methane and nitrous oxide gives the emissions rates of the greenhouse gases. This tracer dilution method can be performed using both stationary and mobile measurements and in both cases, real-time measurements of both tracer and quantified gas are required, placing high demands on the analytical detection method. To perform the methane and nitrous oxide measurements, two robust instruments capable of real-time measurements were used, based on cavity ring-down spectroscopy and operating in the near-infrared spectral region. One instrument measured the methane and

  16. Quantification of Tea Flavonoids by High Performance Liquid Chromatography

    ERIC Educational Resources Information Center

    Freeman, Jessica D.; Niemeyer, Emily D.

    2008-01-01

    We have developed a laboratory experiment that uses high performance liquid chromatography (HPLC) to quantify flavonoid levels in a variety of commercial teas. Specifically, this experiment analyzes a group of flavonoids known as catechins, plant-derived polyphenolic compounds commonly found in many foods and beverages, including green and black…

  17. Waste generated in high-rise buildings construction: a quantification model based on statistical multiple regression.

    PubMed

    Parisi Kern, Andrea; Ferreira Dias, Michele; Piva Kulakowski, Marlova; Paulo Gomes, Luciana

    2015-05-01

    Reducing construction waste is becoming a key environmental issue in the construction industry. The quantification of waste generation rates in the construction sector is an invaluable management tool in supporting mitigation actions. However, the quantification of waste can be a difficult process because of the specific characteristics and the wide range of materials used in different construction projects. Large variations are observed in the methods used to predict the amount of waste generated because of the range of variables involved in construction processes and the different contexts in which these methods are employed. This paper proposes a statistical model to determine the amount of waste generated in the construction of high-rise buildings by assessing the influence of design process and production system, often mentioned as the major culprits behind the generation of waste in construction. Multiple regression was used to conduct a case study based on multiple sources of data of eighteen residential buildings. The resulting statistical model produced dependent (i.e. amount of waste generated) and independent variables associated with the design and the production system used. The best regression model obtained from the sample data resulted in an adjusted R(2) value of 0.694, which means that it predicts approximately 69% of the factors involved in the generation of waste in similar constructions. Most independent variables showed a low determination coefficient when assessed in isolation, which emphasizes the importance of assessing their joint influence on the response (dependent) variable. PMID:25704604

  18. [Utilization of organic resources in paper pulp waste liquid].

    PubMed

    Lin, Qiaojia; Liu, Jinghong; Yang, Guidi; Huang, Biao

    2005-04-01

    In this paper, one hundred percent of condensed sulfate paper pulp waste liquid was used as the raw material of adhesive, and the activation of its lignin as well as the improving effects of phenol formaldehyde resin and polyfunctional aqueous polymer isocyanate (PAPI) were studied. The results showed that adding formaldehyde to the waste liquid could increase the reactivity of contained lignin, and adding 30% phenol formaldehyde resin or 20% PAPI could make the waste liquid in place of pure phenol formaldehyde resin for producing class I plywood. Furthermore, the cost could be reduced by 55.5% and 49.0%, respectively, in comparing with pure phenol formaldehyde resin. This approach fully used the organic resources in paper pulp waste liquid, reduced environment pollution at the same time, and had unexceptionable economic, social and ecological benefits. The feasibility of preparing adhesives from paper pulp waste liquid was also analyzed by infrared spectrum. PMID:16011170

  19. Existing data on the 216-Z liquid waste sites

    SciTech Connect

    Owens, K.W.

    1981-05-01

    During 36 years of operation at the Hanford Site, the ground has been used for disposal of liquid and solid transuranic and/or low-level wastes. Liquid waste was disposed in surface and subsurface cribs, trenches, French drains, reverse wells, ditches and ponds. Disposal structures associated with Z Plant received liquid waste from plutonium finishing and reclamation, waste treatment and laboratory operations. The nineteen 216-Z sites have received 83% of the plutonium discharged to 325 liquid waste facilities at the Hanford Site. The purpose of this document is to support the Hanford Defense Waste Environmental Impact Statement by drawing the existing data together for the 216-Z liquid waste disposal sites. This document provides an interim reference while a sitewide Waste Information Data System (WIDS) is developed and put on line. Eventually these and additional site data for all Hanford waste disposal sites will be available on WIDS. Compilation of existing data is the first step in evaluating the need and developing the technology for long-term management of these waste sites. The scope of this document is confined to data describing the status of the 216-Z waste sites as of December 31, 1979. Information and sketches are taken from existing documents and drawings.

  20. Natural diatomite process for removal of radioactivity from liquid waste.

    PubMed

    Osmanlioglu, Ahmet Erdal

    2007-01-01

    Diatomite has a number of unique physical properties and has found diversified industrial utilization. The filtration characteristics are particularly significant in the purification of liquids. The purpose of this study was to test natural diatomaceous earth (diatomite) as an alternative material that could be used for removal of radioactivity from liquid waste. A pilot-scale column-type device was designed. Natural diatomite samples were ground, sieved and prepared to use as sorption media. In this study, real waste liquid was used as radioactive liquid having special conditions. The liquid waste contained three radionuclides (Cs-137, Cs-134 and Co-60). Following the treatment by diatomite, the radioactivity of liquid waste was reduced from the initial 2.60 Bq/ml to less than 0.40 Bq/ml. The results of this study show that most of the radioactivity was removed from the solution by processing with diatomite. PMID:17049259

  1. Cement encapsulation of low-level waste liquids. Final report

    SciTech Connect

    Baker, M.N.; Houston, H.M.

    1999-01-01

    Pretreatment of liquid high-level radioactive waste at the West Valley Demonstration Project (WVDP) was essential to ensuring the success of high-level waste (HLW) vitrification. By chemically separating the HLW from liquid waste, it was possible to achieve a significant reduction in the volume of HLW to be vitrified. In addition, pretreatment made it possible to remove sulfates, which posed several processing problems, from the HLW before vitrification took place.

  2. Waste characterization for radioactive liquid waste evaporators at Argonne National Laboratory - West.

    SciTech Connect

    Christensen, B. D.

    1999-02-15

    Several facilities at Argonne National Laboratory - West (ANL-W) generate many thousand gallons of radioactive liquid waste per year. These waste streams are sent to the AFL-W Radioactive Liquid Waste Treatment Facility (RLWTF) where they are processed through hot air evaporators. These evaporators remove the liquid portion of the waste and leave a relatively small volume of solids in a shielded container. The ANL-W sampling, characterization and tracking programs ensure that these solids ultimately meet the disposal requirements of a low-level radioactive waste landfill. One set of evaporators will process an average 25,000 gallons of radioactive liquid waste, provide shielding, and reduce it to a volume of six cubic meters (container volume) for disposal. Waste characterization of the shielded evaporators poses some challenges. The process of evaporating the liquid and reducing the volume of waste increases the concentrations of RCIU regulated metals and radionuclides in the final waste form. Also, once the liquid waste has been processed through the evaporators it is not possible to obtain sample material for characterization. The process for tracking and assessing the final radioactive waste concentrations is described in this paper, The structural components of the evaporator are an approved and integral part of the final waste stream and they are included in the final waste characterization.

  3. Concepts for detritiation of waste liquids

    SciTech Connect

    King, C.M. ); Van Brunt, V.; Garber, A.R. ); King, R.B. . Dept. of Chemistry)

    1991-01-01

    Tritium is formed in thermal nuclear reactors both by neutron activation of elements such as deuterium and lithium and by ternary fission in the fuel. It is a weak beta-emitter with a short half-life, 12.3 years, and its radiological significance in reactor discharges is very low. In heavy-water-cooled and -moderated reactors, such as the SRS reactors, the tritium concentration in the moderator is sufficiently high to cause a potential hazard to operators, so research and development programs have been carried out on processes to remove the tritium. Detritiation of light water has also been the subject of major R D efforts world-wide, because reprocessing operations can generate significant quantities of tritium in liquid waste, and high concentrations of tritium may arise in some aqueous streams in future fusion reactors. This paper presents a review of some of the methods that have been proposed, studied, and developed for removal of tritium from light and heavy water, along with some new concepts for aqueous detritiation directly from liquid oxide (HTO) bearing feed streams.

  4. Concepts for detritiation of waste liquids

    SciTech Connect

    King, C.M.; Van Brunt, V.; Garber, A.R.; King, R.B.

    1991-12-31

    Tritium is formed in thermal nuclear reactors both by neutron activation of elements such as deuterium and lithium and by ternary fission in the fuel. It is a weak beta-emitter with a short half-life, 12.3 years, and its radiological significance in reactor discharges is very low. In heavy-water-cooled and -moderated reactors, such as the SRS reactors, the tritium concentration in the moderator is sufficiently high to cause a potential hazard to operators, so research and development programs have been carried out on processes to remove the tritium. Detritiation of light water has also been the subject of major R&D efforts world-wide, because reprocessing operations can generate significant quantities of tritium in liquid waste, and high concentrations of tritium may arise in some aqueous streams in future fusion reactors. This paper presents a review of some of the methods that have been proposed, studied, and developed for removal of tritium from light and heavy water, along with some new concepts for aqueous detritiation directly from liquid oxide (HTO) bearing feed streams.

  5. DETERMINATION AND QUANTIFICATION OF NON-AQUEOUS PHASE LIQUID MIXTURES IN ENVIRONMENTAL MEDIA

    SciTech Connect

    Rucker, G

    2006-09-22

    It is important to recognize the presence of Non-Aqueous Phase Liquids (NAPLs) in soils at a waste site in order to design and construct a successful remediation system. NAPLs often manifest as a complex, multi-component mixture of organic compounds that can occur in environmental media, such as vadose zone soil, where the mixture will partition and equilibrate with soil particles, pore vapor, and pore water. Complex organic mixtures can greatly complicate the determination and quantification of NAPL in soil due to inter-media transfer. NAPL thresholds can also change because of mixture physical properties and can disguise the presence of NAPL. A unique analytical method and copyrighted software have been developed at the Department of Energy's Savannah River Site that facilitates solution of this problem. The analytical method uses a classic chemistry approach and applies the principals of solubility limit theory, Raoult's Law, and equilibrium chemistry to derive an accurate estimation of NAPL presence and quantity. The method is unique because it calculates an exact result that is mass balanced for each physical state, chemical mixture component, and mixture characteristics. The method is also unique because the solution can be calculated on both a wet weight and dry weight basis--a factor which is often overlooked. The software includes physical parameters for 300 chemicals in a database that self-loads into the model to save time. The method accommodates up to 20 different chemicals in a multi-component mixture analysis. A robust data display is generated including important parameters of the components and mixture including: NAPL thresholds for individual chemical components within the mixture, mass distribution in soil for each physical state, molar fractions, density, vapor pressure, solubility, mass balance, media concentrations, residual saturation, and modest graphing capabilities. This method and software are power tools to simplify otherwise tedious

  6. Newly Generated Liquid Waste Processing Alternatives Study, Volume 1

    SciTech Connect

    Landman, William Henry; Bates, Steven Odum; Bonnema, Bruce Edward; Palmer, Stanley Leland; Podgorney, Anna Kristine; Walsh, Stephanie

    2002-09-01

    This report identifies and evaluates three options for treating newly generated liquid waste at the Idaho Nuclear Technology and Engineering Center of the Idaho National Engineering and Environmental Laboratory. The three options are: (a) treat the waste using processing facilities designed for treating sodium-bearing waste, (b) treat the waste using subcontractor-supplied mobile systems, or (c) treat the waste using a special facility designed and constructed for that purpose. In studying these options, engineers concluded that the best approach is to store the newly generated liquid waste until a sodium-bearing waste treatment facility is available and then to co-process the stored inventory of the newly generated waste with the sodium-bearing waste. After the sodium-bearing waste facility completes its mission, two paths are available. The newly generated liquid waste could be treated using the subcontractor-supplied system or the sodium-bearing waste facility or a portion of it. The final decision depends on the design of the sodium-bearing waste treatment facility, which will be completed in coming years.

  7. Treatability Variance for Containerised Liquids in Mixed Debris Waste - 12101

    SciTech Connect

    Alstatt, Catherine M.

    2012-07-01

    The TRU Waste Processing Center (TWPC) is a Department of Energy facility whose mission is to receive and process for appropriate disposal legacy Contact Handled (CH) and Remote Handled (RH) waste, including debris waste stored at various DOE Oak Ridge facilities. Acceptable Knowledge (AK) prepared for the waste characterizes the waste as mixed waste, meaning it is both radioactive and regulated under the Resource Conservation and Recovery Act (RCRA). The AK also indicates that a number of the debris waste packages contain small amounts of containerised liquids. The documentation indicates liquid wastes generated in routine lab operations were typically collected for potential recovery of valuable isotopes. However, during activities associated with decontamination and decommissioning (D and D), some containers with small amounts of liquids were placed into the waste containers with debris waste. Many of these containers now hold from 2.5 milliliters (ml) to 237 ml of liquid; a few contain larger volumes. At least some of these containers were likely empty at the time of generation, but documentation of this condition is lacking. Since WIPP compliant AK is developed on a waste stream basis, rather than an individual container basis, and includes every potential RCRA hazardous constituent within the waste stream, it is insufficient for the purpose of characterizing individual containers of liquid. Debris waste is defined in 40 CFR 268.2(g) as 'solid material exceeding a 60 mm particle size that is intended for disposal and that is: a manufactured object; or plant or animal matter; or natural geologic material'. The definition further states that intact containers of hazardous waste that are not ruptured and that retain at least 75% of their original volume are not debris. The prescribed treatment is removal of intact containers from the debris waste, and treatment of their contents to meet specific Land Disposal Restrictions (LDR) standards. This is true for

  8. Quantification of feather structure, wettability and resistance to liquid penetration

    PubMed Central

    Srinivasan, Siddarth; Chhatre, Shreerang S.; Guardado, Jesus O.; Park, Kyoo-Chul; Parker, Andrew R.; Rubner, Michael F.; McKinley, Gareth H.; Cohen, Robert E.

    2014-01-01

    Birds in the cormorant (Phalacrocoracidae) family dive tens of metres into water to prey on fish while entraining a thin layer of air (a plastron film) within the microstructures of their feathers. In addition, many species within the family spread their wings for long periods of time upon emerging from water. To investigate whether wetting and wing-spreading are related to feather structure, microscopy and photographic studies have previously been used to extract structural parameters for barbs and barbules. In this work, we describe a systematic methodology to characterize the quasi-hierarchical topography of bird feathers that is based on contact angle measurements using a set of polar and non-polar probing liquids. Contact angle measurements on dip-coated feathers of six aquatic bird species (including three from the Phalacrocoracidae family) are used to extract two distinguishing structural parameters, a dimensionless spacing ratio of the barbule (D*) and a characteristic length scale corresponding to the spacing of defect sites. The dimensionless spacing parameter can be used in conjunction with a model for the surface topography to enable us to predict a priori the apparent contact angles of water droplets on feathers as well as the water breakthrough pressure required for the disruption of the plastron on the feather barbules. The predicted values of breakthrough depths in water (1–4 m) are towards the lower end of typical diving depths for the aquatic bird species examined here, and therefore a representative feather is expected to be fully wetted in a typical deep dive. However, thermodynamic surface energy analysis based on a simple one-dimensional cylindrical model of the feathers using parameters extracted from the goniometric analysis reveals that for water droplets on feathers of all six species under consideration, the non-wetting ‘Cassie–Baxter’ composite state represents the global energy minimum of the system. By contrast, for other

  9. QUANTIFICATION OF MUNICIPAL DISPOSAL METHODS FOR INDUSTRIALLY GENERATED HAZARDOUS WASTES

    EPA Science Inventory

    Estimations of the amounts of industrial hazardous wastes being disposed of according to various methods of disposal were generated for significant portions of the five following SIC codes: 28, Chemical and Allied Products; 29, Petroleum Refining and Related Industries; 30, Rubbe...

  10. Detection of free liquid in containers of solidified radioactive waste

    DOEpatents

    Greenhalgh, W.O.

    Nondestructive detection of the presence of free liquid within a sealed enclosure containing solidified waste is accomplished by measuring the levels of waste at two diametrically opposite locations while slowly tilting the enclosure toward one of said locations. When the measured level remains constant at the other location, the measured level at said one location is noted and any measured difference of levels indicates the presence of liquid on the surface of the solifified waste. The absence of liquid in the enclosure is verified when the measured levels at both locations are equal.

  11. Detection of free liquid in containers of solidified radioactive waste

    DOEpatents

    Greenhalgh, Wilbur O.

    1985-01-01

    A method of nondestructively detecting the presence of free liquid within a sealed enclosure containing solidified waste by measuring the levels of waste at two diametrically opposite locations while slowly tilting the enclosure toward one of said locations. When the measured level remains constant at the other location, the measured level at said one location is noted and any measured difference of levels indicates the presence of liquid on the surface of the solidified waste. The absence of liquid in the enclosure is verified when the measured levels at both locations are equal.

  12. Methodology for quantification of waste generated in Spanish railway construction works.

    PubMed

    de Guzmán Báez, Ana; Villoria Sáez, Paola; del Río Merino, Mercedes; García Navarro, Justo

    2012-05-01

    In the last years, the European Union (EU) has been focused on the reduction of construction and demolition (C&D) waste. Specifically, in 2006, Spain generated roughly 47million tons of C&D waste, of which only 13.6% was recycled. This situation has lead to the drawing up of many regulations on C&D waste during the past years forcing EU countries to include new measures for waste prevention and recycling. Among these measures, the mandatory obligation to quantify the C&D waste expected to be originated during a construction project is mandated. However, limited data is available on civil engineering projects. Therefore, the aim of this research study is to improve C&D waste management in railway projects, by developing a model for C&D waste quantification. For this purpose, we develop two equations which estimate in advance the amount, both in weight and volume, of the C&D waste likely to be generated in railway construction projects, including the category of C&D waste generated for the entire project. PMID:22321896

  13. Methodology for quantification of waste generated in Spanish railway construction works

    SciTech Connect

    Guzman Baez, Ana de; Garcia Navarro, Justo

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer Two equations for C and D waste estimation in railway construction works are developed. Black-Right-Pointing-Pointer Mixed C and D waste is the most generated category during railway construction works. Black-Right-Pointing-Pointer Tunnel construction is essential to quantify the waste generated during the works. Black-Right-Pointing-Pointer There is a relationship between C and D waste generated and railway functional units. Black-Right-Pointing-Pointer The methodology proposed can be used to obtain new constants for other areas. - Abstract: In the last years, the European Union (EU) has been focused on the reduction of construction and demolition (C and D) waste. Specifically, in 2006, Spain generated roughly 47 million tons of C and D waste, of which only 13.6% was recycled. This situation has lead to the drawing up of many regulations on C and D waste during the past years forcing EU countries to include new measures for waste prevention and recycling. Among these measures, the mandatory obligation to quantify the C and D waste expected to be originated during a construction project is mandated. However, limited data is available on civil engineering projects. Therefore, the aim of this research study is to improve C and D waste management in railway projects, by developing a model for C and D waste quantification. For this purpose, we develop two equations which estimate in advance the amount, both in weight and volume, of the C and D waste likely to be generated in railway construction projects, including the category of C and D waste generated for the entire project.

  14. Liquid return from gas pressurization of grouted waste

    SciTech Connect

    Powell, W.J.; Benny, H.L.

    1994-05-01

    The ability to force pore liquids out of a simulated waste grout matrix using air pressure was measured. Specimens cured under various conditions were placed in a permeameter and subjected to increasing air pressure. The pressure was held constant for 24 hours and then stepped up until either liquid was released or 150 psi was reached. One specimen was taken to 190 psi with no liquid release. Permeability to simulated tank waste was then measured. Compressive strength was measured following these tests. This data is to assess the amount of fluid that might be released from grouted waste resulting from the buildup of radiolytically generated hydrogen and other gasses within the waste form matrix. A plot of the unconfined compressive strength versus breakthrough pressures identifies a region of ``good`` grout, which will resist liquid release.

  15. OBSERVATIONS ON WASTE DESTRUCTION IN LIQUID INJECTION INCINERATORS

    EPA Science Inventory

    Various factors affecting the performance of a subscale liquid injection incinerator simulator are discussed. The mechanisms by which waste escapes incineration within the spray flame are investigated for variations in atomization quality, flame stoichiometry. and the initial was...

  16. Evaluation of mercury in the liquid waste processing facilities

    SciTech Connect

    Jain, Vijay; Shah, Hasmukh; Occhipinti, John E.; Wilmarth, William R.; Edwards, Richard E.

    2015-08-13

    This report provides a summary of Phase I activities conducted to support an Integrated Evaluation of Mercury in Liquid Waste System (LWS) Processing Facilities. Phase I activities included a review and assessment of the liquid waste inventory and chemical processing behavior of mercury using a system by system review methodology approach. Gaps in understanding mercury behavior as well as action items from the structured reviews are being tracked. 64% of the gaps and actions have been resolved.

  17. Decommissioning and Dismantling of Liquid Waste Storage and Liquid Waste Treatment Facility from Paldiski Nuclear Site, Estonia

    SciTech Connect

    Varvas, M.; Putnik, H.; Johnsson, B.

    2006-07-01

    The Paldiski Nuclear Facility in Estonia, with two nuclear reactors was owned by the Soviet Navy and was used for training the navy personnel to operate submarine nuclear reactors. After collapse of Soviet Union the Facility was shut down and handed over to the Estonian government in 1995. In co-operation with the Paldiski International Expert Reference Group (PIERG) decommission strategy was worked out and started to implement. Conditioning of solid and liquid operational waste and dismantling of contaminated installations and buildings were among the key issues of the Strategy. Most of the liquid waste volume, remained at the Facility, was processed in the frames of an Estonian-Finnish co-operation project using a mobile wastewater purification unit NURES (IVO International OY) and water was discharged prior to the site take-over. In 1999-2002 ca 120 m{sup 3} of semi-liquid tank sediments (a mixture of ion exchange resins, sand filters, evaporator and flocculation slurry), remained after treatment of liquid waste were solidified in steel containers and stored into interim storage. The project was carried out under the Swedish - Estonian co-operation program on radiation protection and nuclear safety. Contaminated installations in buildings, used for treatment and storage of liquid waste (Liquid Waste Treatment Facility and Liquid Waste Storage) were then dismantled and the buildings demolished in 2001-2004. (authors)

  18. Radioactive Liquid Waste Treatment Facility: Environmental Information Document

    SciTech Connect

    Haagenstad, H.T.; Gonzales, G.; Suazo, I.L.

    1993-11-01

    At Los Alamos National Laboratory (LANL), the treatment of radioactive liquid waste is an integral function of the LANL mission: to assure U.S. military deterrence capability through nuclear weapons technology. As part of this mission, LANL conducts nuclear materials research and development (R&D) activities. These activities generate radioactive liquid waste that must be handled in a manner to ensure protection of workers, the public, and the environment. Radioactive liquid waste currently generated at LANL is treated at the Radioactive Liquid Waste Treatment Facility (RLWTF), located at Technical Area (TA)-50. The RLWTF is 30 years old and nearing the end of its useful design life. The facility was designed at a time when environmental requirements, as well as more effective treatment technologies, were not inherent in engineering design criteria. The evolution of engineering design criteria has resulted in the older technology becoming less effective in treating radioactive liquid wastestreams in accordance with current National Pollutant Discharge Elimination System (NPDES) and Department of Energy (DOE) regulatory requirements. Therefore, to support ongoing R&D programs pertinent to its mission, LANL is in need of capabilities to efficiently treat radioactive liquid waste onsite or to transport the waste off site for treatment and/or disposal. The purpose of the EID is to provide the technical baseline information for subsequent preparation of an Environmental Impact Statement (EIS) for the RLWTF. This EID addresses the proposed action and alternatives for meeting the purpose and need for agency action.

  19. Direct quantification of dimethylsulfoniopropionate (DMSP) with hydrophilic interaction liquid chromatography/mass spectrometry.

    PubMed

    Spielmeyer, Astrid; Pohnert, Georg

    2010-12-01

    A simple, derivatization free method for the direct determination of dimethylsulfoniopropionate (DMSP) using hydrophilic interaction liquid chromatography (HILIC)/mass spectrometry is introduced. DMSP is a zwitterionic osmolyte which is produced from marine plankton, macro algae and higher plants. Due to its central role in climate relevant geochemical processes as well as in plant physiology and chemical ecology there is a great interest in methods for its quantification. Since DMSP is labile and difficult to extract currently most protocols for quantification are based on indirect methods. Here we show that ultra performance liquid chromatography/mass spectrometry using a HILIC stationary phase is suitable for the direct quantification of DMSP from aqueous samples and microalgal extracts. The protocol requires minimal sample preparation and phytoplankton samples can be investigated after filtration of small volumes. The limit of detection is 20nM and the calibration curve is linear in the range of 60nM to 50μM. The use of [(2)H(6)]-DMSP as internal standard allows prolonged sample storage since it is transformed with the same kinetics as natural DMSP. This makes the method suitable for both laboratory and field studies. PMID:21030323

  20. Quantification of astaxanthin in shrimp waste hydrolysate by HPLC.

    PubMed

    López-Cervantes, J; Sánchez-Machado, D I; Gutiérrez-Coronado, M A; Ríos-Vázquez, N J

    2006-10-01

    In the present study, a simple and rapid reversed-phase HPLC method for the determination of astaxanthin in shrimp waste hydrolysate has been developed and validated. The analytical procedure involves the direct extraction of astaxanthin from the lipid fraction with methanol. The analytical column, SS Exil ODS, was operated at 25C. The mobile phase consisted of a mixture of water:methanol:dichloromethane:acetonitrile (4.5:28:22:45.5 v/v/v/v) at a flow rate of 1.0 mL/min. Detection and identification were performed using a photodiode array detector (lambda(detection) = 476 nm). The proposed HPLC method showed adequate linearity, repeatability and accuracy. PMID:16802328

  1. Membrane Treatment of Liquid Salt Bearing Radioactive Wastes

    SciTech Connect

    Dmitriev, S. A.; Adamovich, D. V.; Demkin, V. I.; Timofeev, E. M.

    2003-02-25

    The main fields of introduction and application of membrane methods for preliminary treatment and processing salt liquid radioactive waste (SLRW) can be nuclear power stations (NPP) and enterprises on atomic submarines (AS) utilization. Unlike the earlier developed technology for the liquid salt bearing radioactive waste decontamination and concentrating this report presents the new enhanced membrane technology for the liquid salt bearing radioactive waste processing based on the state-of-the-art membrane unit design, namely, the filtering units equipped with the metal-ceramic membranes of ''TruMem'' brand, as well as the electrodialysis and electroosmosis concentrators. Application of the above mentioned units in conjunction with the pulse pole changer will allow the marked increase of the radioactive waste concentrating factor and the significant reduction of the waste volume intended for conversion into monolith and disposal. Besides, the application of the electrodialysis units loaded with an ion exchange material at the end polishing stage of the radioactive waste decontamination process will allow the reagent-free radioactive waste treatment that meets the standards set for the release of the decontaminated liquid radioactive waste effluents into the natural reservoirs of fish-farming value.

  2. In-Situ Chemical Precipitation of Radioactive Liquid Waste - 12492

    SciTech Connect

    Osmanlioglu, Ahmet Erdal

    2012-07-01

    This paper presented in-situ chemical precipitation for radioactive liquid waste by using chemical agents. Results are reported on large-scale implementation on the removal of {sup 137}Cs, {sup 134}Cs and {sup 60}Co from liquid radioactive waste generating from Nuclear Research and Training Centre. Total amount of liquid radioactive waste was 35 m{sup 3} and main radionuclides were Cs-137, Cs- 134 and Co-60. Initial radioactivity concentration of the liquid waste was 2264, 17 and 9 Bq/liter for Cs-137, Cs-134 and Co-60 respectively. Potassium ferro cyanide was selected as chemical agent at high pH levels 8-10 according to laboratory tests. After the process, radioactive sludge precipitated at the bottom of the tank and decontaminated clean liquid was evaluated depending on discharge limits. By this precipitation method decontamination factors were determined as 60, 9 and 17 for Cs-137, Cs-134 and Co-60 respectively. At the bottom of the tank radioactive sludge amount was 0.98 m{sup 3}. It was transferred by sludge pumps to cementation unit for solidification. By in situ chemical processing 97% of volume reduction was achieved. Using the optimal concentration of 0.75 M potassium ferro cyanide about 98% of the {sup 137}Cs can be removed at pH 8. The Potassium ferro cyanide precipitation method could be used successfully in large scale applications with nickel and ferrum agents for removal of Cs-137, Cs-134 and Co- 60. Although DF values of laboratory test were much higher than in-situ implementation, liquid radioactive waste was decontaminated successfully by using potassium ferro cyanide. Majority of liquid waste were discharged as clean liquid. %97.2 volumetric amount of liquid waste was cleaned and discharged at the original site. Reduced amount of sludge transportation in drums is more economical and safer method than liquid transportation. Although DF values could be different for each of applications related to main specifications of original liquid waste, this

  3. Process for treating liquid chlorinated hydrocarbon wastes containing iron

    SciTech Connect

    Doane, E.P.

    1986-09-30

    A process is described for reducing the ferric chloride content of liquid waste streams comprising higher boiling chlorinated hydrocarbons and containing amounts of ferric chloride. The process consists essentially of contacting the waste stream with an amount of water sufficient to convert ferric chloride contained in the stream to solid ferric chloride hexahydrate, and then removing the solid hexahydrate by filtration or centrifugation from the waste stream.

  4. APPLICATION OF PULSE COMBUSTION TO INCINERATION OF LIQUID HAZARDOUS WASTE

    EPA Science Inventory

    The report gives results of a study to determine the effect of acoustic pulsations on the steady-state operation of a pulse combustor burning liquid hazardous waste. A horizontal tunnel furnace was retrofitted with a liquid injection pulse combustor that burned No. 2 fuel oil. Th...

  5. Quantification of regional leachate variance from municipal solid waste landfills in China.

    PubMed

    Yang, Na; Damgaard, Anders; Kjeldsen, Peter; Shao, Li-Ming; He, Pin-Jing

    2015-12-01

    The quantity of leachate is crucial when assessing pollution emanating from municipal landfills. In most cases, existing leachate quantification measures only take into account one source - precipitation, which resulted in serious underestimation in China due to its waste properties: high moisture contents. To overcome this problem, a new estimation method was established considering two sources: (1) precipitation infiltrated throughout waste layers, which was simulated with the HELP model, (2) water squeezed out of the waste itself, which was theoretically calculated using actual data of Chinese waste. The two sources depended on climate conditions and waste characteristics, respectively, which both varied in different regions. In this study, 31 Chinese cities were investigated and classified into three geographic regions according to landfill leachate generation performance: northwestern China (China-NW) with semi-arid and temperate climate and waste moisture content of about 46.0%, northern China (China-N) with semi-humid and temperate climate and waste moisture content of about 58.2%, and southern China (China-S) with humid and sub-tropical/tropical climate and waste moisture content of about 58.2%. In China-NW, accumulated leachate amounts were very low and mainly the result of waste degradation, implying on-site spraying/irrigation or recirculation may be an economic approach to treatment. In China-N, water squeezed out of waste by compaction totaled 22-45% of overall leachate amounts in the first 40 years, so decreasing the initial moisture content of waste arriving at landfills could reduce leachate generation. In China-S, the leachate generated by infiltrated precipitation after HDPE geomembranes in top cover started failing, contributed more than 60% of the overall amounts over 100 years of landfilling. Therefore, the quality and placing of HDPE geomembranes in the top cover should be controlled strictly for the purpose of mitigation leachate generation

  6. Elimination of liquid discharge to the environment from the TA-50 Radioactive Liquid Waste Treatment Facility

    SciTech Connect

    Moss, D.; Williams, N.; Hall, D.; Hargis, K.; Saladen, M.; Sanders, M.; Voit, S.; Worland, P.; Yarbro, S.

    1998-06-01

    Alternatives were evaluated for management of treated radioactive liquid waste from the radioactive liquid waste treatment facility (RLWTF) at Los Alamos National Laboratory. The alternatives included continued discharge into Mortandad Canyon, diversion to the sanitary wastewater treatment facility and discharge of its effluent to Sandia Canyon or Canada del Buey, and zero liquid discharge. Implementation of a zero liquid discharge system is recommended in addition to two phases of upgrades currently under way. Three additional phases of upgrades to the present radioactive liquid waste system are proposed to accomplish zero liquid discharge. The first phase involves minimization of liquid waste generation, along with improved characterization and monitoring of the remaining liquid waste. The second phase removes dissolved salts from the reverse osmosis concentrate stream to yield a higher effluent quality. In the final phase, the high-quality effluent is reused for industrial purposes within the Laboratory or evaporated. Completion of these three phases will result in zero discharge of treated radioactive liquid wastewater from the RLWTF.

  7. Corrosion experience in calcination of liquid nuclear waste

    SciTech Connect

    Zimmerman, C A

    1980-01-01

    The Waste Calcining Facility (WCF) at the Idaho National Engineering Laboratory became operational in 1963. Since that time, approximately 13,337,137 litres (3,523,375 gallons) of liquid nuclear wastes, generated during the reprocessing of spent nuclear fuel materials, have been reduced to dry granular solids. The volume reduction is about seven or eight gallons of liquid waste to one gallon of dry granular solids. This paper covers some of the corrosion experiences encountered in over fifteen years of operating that calcination facility. 7 figures, 7 tables.

  8. Assessment and quantification of plastics waste generation in major 60 cities of India.

    PubMed

    Nalini, R; Srinivasulu, B; Shit, Subhas C; Nigam, Suneel Kumar; Akolkar, A B; Dwivedfi, R K

    2013-04-01

    Polymers or plastics materials registered rapid growth in 1970s, 1980s and 1990s at the rate of 2-2.5 times the GDP growth in India. The demand for plastic raw material got more than doubled from 3.3 Million Metric Ton to 6.8 Million Metric Tons in 2010 attributed mainly to rapid urbanization, spread of retail chains, plastics based packaging from grocery to food and vegetable products to cosmetics and consumer items. Plastics packages have its merits over many of conventional materials in the related sector but unless they are collected back effectively after their use to go into recycling process, they become an eyesore in the stream of Municipal Solid Waste (MSW) due to high visibility. As the synthetic and conventional plastics are non-biodegradable in nature, these remain in the dump yards/ landfills for several years, if not collected properly. Due to non- biodegradability, plastics waste remains in the environment for several years, if not collected and disposing plastics wastes at landfills are unsafe since toxic chemicals leach out into the soil and as they contaminate soil and underground water quality. The municipal solid waste also increasing day-by-day due to the inefficient source collection, segregation and transmission of plastics waste for recycling and reusing. In order to find out the realistic plastics waste generation, a study on assessment and quantification of plastics waste has been carried out by CPCB in collaboration with CIPET on selected 60 major cities of India. PMID:25464691

  9. Assessment and quantification of plastics waste generation in major 60 cities of India.

    PubMed

    Nalini, R; Srinivasulu, B; Shit, Subhas C; Nigam, Suneel Kumar; Akolkar, A B; Dwivedfi, R K

    2013-04-01

    Polymers or plastics materials registered rapid growth in 1970s, 1980s and 1990s at the rate of 2-2.5 times the GDP growth in India. The demand for plastic raw material got more than doubled from 3.3 Million Metric Ton to 6.8 Million Metric Tons in 2010 attributed mainly to rapid urbanization, spread of retail chains, plastics based packaging from grocery to food and vegetable products to cosmetics and consumer items. Plastics packages have its merits over many of conventional materials in the related sector but unless they are collected back effectively after their use to go into recycling process, they become an eyesore in the stream of Municipal Solid Waste (MSW) due to high visibility. As the synthetic and conventional plastics are non-biodegradable in nature, these remain in the dump yards/ landfills for several years, if not collected properly. Due to non- biodegradability, plastics waste remains in the environment for several years, if not collected and disposing plastics wastes at landfills are unsafe since toxic chemicals leach out into the soil and as they contaminate soil and underground water quality. The municipal solid waste also increasing day-by-day due to the inefficient source collection, segregation and transmission of plastics waste for recycling and reusing. In order to find out the realistic plastics waste generation, a study on assessment and quantification of plastics waste has been carried out by CPCB in collaboration with CIPET on selected 60 major cities of India. PMID:25508322

  10. ICPP radioactive liquid and calcine waste technologies evaluation. Interim report

    SciTech Connect

    Murphy, J.A.; Pincock, L.F.; Christiansen, I.N.

    1994-06-01

    The Department of Energy (DOE) has received spent nuclear fuel (SNF) at the Idaho Chemical Processing Plant (ICPP) for interim storage since 1951 and reprocessing since 1953. Until recently, the major activity of the ICPP has been the reprocessing of SNF to recover fissile uranium; however, changing world events have raised questions concerning the need to recover and recycle this material. In April 1992, DOE chose to discontinue reprocessing SNF for uranium recovery and shifted its focus toward the management and disposition of radioactive wastes accumulated through reprocessing activities. Currently, 1.8 million gallons of radioactive liquid wastes (1.5 million gallons of radioactive sodium-bearing liquid wastes and 0.3 million gallons of high-level liquid waste) and 3,800 cubic meters (m{sup 3}) of calcine waste are in inventory at the ICPP. Legal drivers and agreements exist obligating the INEL to develop, demonstrate, and implement technologies for safe and environmentally sound treatment and interim storage of radioactive liquid and calcine waste. Candidate treatment processes and waste forms are being evaluated using the Technology Evaluation and Analysis Methodology (TEAM) Model. This process allows decision makers to (1) identify optimum radioactive waste treatment and disposal form alternatives; (2) assess tradeoffs between various optimization criteria; (3) identify uncertainties in performance parameters; and (4) focus development efforts on options that best satisfy stakeholder concerns. The Systems Analysis technology evaluation presented in this document supports the DOE in selecting the most effective radioactive liquid and calcine waste management plan to implement in compliance with established regulations, court orders, and agreements.

  11. QUANTIFICATION OF CERAMIDE SPECIES IN BIOLOGICAL SAMPLES BY LIQUID CHROMATOGRAPHY-ELECTROSPRAY TANDEM MASS SPECTROMETRY

    PubMed Central

    Kasumov, Takhar; Huang, Hazel; Chung, Yoon-Mi; Zhang, Renliang; McCullough, Arthur J.; Kirwan, John P.

    2010-01-01

    We present an optimized and validated liquid chromatography-electrospray ionization tandem mass spectrometric (LC-ESI-MS/MS) method for the simultaneous measurement of concentrations of different ceramide species in biological samples. The method of analysis of tissue samples is based on Bligh and Dyer extraction, reverse-phase HPLC separation and multiple reaction monitoring of ceramides. Preparation of plasma samples also requires isolation of sphingolipids by silica gel column chromatography prior to LC-ESI-MS/MS analysis. The limits of detection and quantification are in a range of 5–50 pg/ml for distinct ceramides. The method was reliable for inter-assay and intra-assay precision, accuracy and linearity. Recovery of ceramide subspecies from human plasma, rat liver and muscle tissue were 78–91%, 70–99%, and 71–95%, respectively. The separation and quantification of several endogenous long-chain and very-long-chain ceramides using two non-physiological odd chain ceramide (C17 and C25) internal standards was achieved within a single 21 min chromatographic run. The technique was applied to quantify distinct ceramide species in different rat tissues (muscle, liver, and heart) and in human plasma. Using this analytical technique we demonstrated that a clinical exercise training intervention reduces the levels of ceramides in plasma of obese adults. This technique could be extended for quantification of other ceramides and sphyngolipids with no significant modification. PMID:20178771

  12. Municipal solid waste characterization and quantification as a measure towards effective waste management in Ghana.

    PubMed

    Miezah, Kodwo; Obiri-Danso, Kwasi; Kádár, Zsófia; Fei-Baffoe, Bernard; Mensah, Moses Y

    2015-12-01

    Reliable national data on waste generation and composition that will inform effective planning on waste management in Ghana is absent. To help obtain this data on a regional basis, selected households in each region were recruited to obtain data on rate of waste generation, physical composition of waste, sorting and separation efficiency and per capita of waste. Results show that rate of waste generation in Ghana was 0.47 kg/person/day, which translates into about 12,710 tons of waste per day per the current population of 27,043,093. Nationally, biodegradable waste (organics and papers) was 0.318 kg/person/day and non-biodegradable or recyclables (metals, glass, textiles, leather and rubbers) was 0.096 kg/person/day. Inert and miscellaneous waste was 0.055 kg/person/day. The average household waste generation rate among the metropolitan cities, except Tamale, was high, 0.72 kg/person/day. Metropolises generated higher waste (average 0.63 kg/person/day) than the municipalities (0.40 kg/person/day) and the least in the districts (0.28 kg/person/day) which are less developed. The waste generation rate also varied across geographical locations, the coastal and forest zones generated higher waste than the northern savanna zone. Waste composition was 61% organics, 14% plastics, 6% inert, 5% miscellaneous, 5% paper, 3% metals, 3% glass, 1% leather and rubber, and 1% textiles. However, organics and plastics, the two major fractions of the household waste varied considerably across the geographical areas. In the coastal zone, the organic waste fraction was highest but decreased through the forest zone towards the northern savanna. However, through the same zones towards the north, plastic waste rather increased in percentage fraction. Households did separate their waste effectively averaging 80%. However, in terms of separating into the bin marked biodegradables, 84% effectiveness was obtained whiles 76% effectiveness for sorting into the bin labeled other waste was

  13. Quantification and pharmacokinetics of crizotinib in rats by liquid chromatography-tandem mass spectrometry.

    PubMed

    Qiu, Feng; Gu, Yanan; Wang, Tingting; Gao, Yingying; Li, Xiao; Gao, Xiangyu; Cheng, Shan

    2016-06-01

    Crizotinib is a small molecule inhibitor of anaplastic lymphoma kinase (ALK) and can be used to treat ALK-positive nonsmall-cell lung cancer. A rapid and simple high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantification of crizotinib in rat plasma using a chemical synthetic compound buspirone as the internal standard (IS). The plasma samples were pretreated by a simple protein precipitation with methanol-acetonitrile (1:1, v/v). Chromatographic separation was successfully achieved on an Agilent Zorbax XDB C18 column (2.1 × 50 mm, 3.5 µm). The gradient elution system was composed of 0.1% formic acid aqueous solution and 0.1% formic acid in methanol solution. The flow rate was set at 0.50 mL/min. The multiple reaction monitoring was based on the transitions of m/z = 450.3 → 177.1 for crizotinib and 386.2 → 122.2 for buspirone (IS). The assay was successfully validated to demonstrate the selectivity, matrix effect, linearity, lower limit of quantification, accuracy, precision, recovery and stability according to the international guidelines. The lower limit of quantification was 1.00 ng/mL in 50 μL of rat plasma. This LC-MS/MS assay was successfully applied to the quantification and pharmacokinetic study of crizotinib in rats after intravenous and oral administration of crizotinib. The oral absolute bioavailability of crizotinib in rats was 68.6 ± 9.63%. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26467669

  14. Liquid radioactive waste discharges from B plant to cribs

    SciTech Connect

    Williams, J.C., Westinghouse Hanford

    1996-05-29

    This engineering report compiles information on types and quantities of liquid waste discharged from B-Plant directly to cribs, ditches, reverse wells, etc., that are associated with B-Plant. Waste discharges to these cribs via overflow form 241-B, 241-BX, and 241-BY tank farms, and waste discharged to these cribs from sources other than B-Plant are discussed.Discharges from B-Plant to other cribs, unplanned releases, or waste remaining in tanks are not included in the report. Waste stream composition information is used to predict quantities of individual chemicals sent to cribs. This provides an accurate mass balance of waste streams from B-Plant to these cribs. These predictions are compared with known crib inventories as a verification of the process.

  15. Quantification of breast density using dual-energy mammography with liquid phantom calibration

    NASA Astrophysics Data System (ADS)

    Lam, Alfonso R.; Ding, Huanjun; Molloi, Sabee

    2014-07-01

    Breast density is a widely recognized potential risk factor for breast cancer. However, accurate quantification of breast density is a challenging task in mammography. The current use of plastic breast-equivalent phantoms for calibration provides limited accuracy in dual-energy mammography due to the chemical composition of the phantom. We implemented a breast-equivalent liquid phantom for dual-energy calibration in order to improve the accuracy of breast density measurement. To design these phantoms, three liquid compounds were chosen: water, isopropyl alcohol, and glycerol. Chemical compositions of glandular and adipose tissues, obtained from NIST database, were used as reference materials. Dual-energy signal of the liquid phantom at different breast densities (0% to 100%) and thicknesses (1 to 8 cm) were simulated. Glandular and adipose tissue thicknesses were estimated from a higher order polynomial of the signals. Our results indicated that the linear attenuation coefficients of the breast-equivalent liquid phantoms match those of the target material. Comparison between measured and known breast density data shows a linear correlation with a slope close to 1 and a non-zero intercept of 7%, while plastic phantoms showed a slope of 0.6 and a non-zero intercept of 8%. Breast density results derived from the liquid calibration phantoms showed higher accuracy than those derived from the plastic phantoms for different breast thicknesses and various tube voltages. We performed experimental phantom studies using liquid phantoms and then compared the computed breast density with those obtained using a bovine tissue model. The experimental data and the known values were in good correlation with a slope close to 1 (˜1.1). In conclusion, our results indicate that liquid phantoms are a reliable alternative for calibration in dual-energy mammography and better reproduce the chemical properties of the target material.

  16. Real-time quantification of viable bacteria in liquid medium using infrared thermography

    NASA Astrophysics Data System (ADS)

    Salaimeh, Ahmad A.; Campion, Jeffrey J.; Gharaibeh, Belal Y.; Evans, Martin E.; Saito, Kozo

    2011-11-01

    Quantifying viable bacteria in liquids is important in environmental, food processing, manufacturing, and medical applications. Since vegetative bacteria generate heat as a result of biochemical reactions associated with cellular functions, thermal sensing techniques, including infrared thermography (IRT), have been used to detect viable cells in biologic samples. We developed a novel method that extends the dynamic range and improves the sensitivity of bacterial quantification by IRT. The approach uses IRT video, thermodynamics laws, and heat transfer mechanisms to directly measure, in real-time, the amount of energy lost as heat from the surface of a liquid sample containing bacteria when the specimen cools to a lower temperature over 2 min. We show that the Energy Content ( EC) of liquid media containing as few as 120 colony-forming units (CFU) of Escherichia coli per ml was significantly higher than that of sterile media ( P < 0.0001), and that EC and viable counts were strongly positively correlated ( r = 0.986) over a range of 120 to approximately 5 × 10 8 CFU/ml. Our IRT approach is a unique non-contact method that provides real-time bacterial enumeration over a wide dynamic range without the need for sample concentration, modification, or destruction. The approach could be adapted to quantify other living cells in a liquid milieu and has the potential for automation and high throughput.

  17. Methane Production Quantification and Energy Estimation for Bangalore Municipal Solid Waste

    NASA Astrophysics Data System (ADS)

    Kumar, A.; Dand, R.; Lakshmikanthan, P.; Babu, G. L. Sivakumar

    2014-01-01

    Landfills are considered as cornerstone of solid waste management. Landfill gas (LFG) and leachate are principal outputs from landfills. Methane, occupying significant volume of landfill gas, has considerable potential as a source of energy replacing enormous amounts of fossil fuels currently in use. Gas extraction and utilization systems need to be designed and implemented in order to exploit this resource. Assessment of economic viability of these systems necessitates estimation of gas released and its energy potential. Gas quantification and energy estimation for municipal solid waste (MSW) of Bangalore city was carried out using five independent methodologies. A small scale experiment was conducted to monitor the gas generation and the results were compared and analysed. Results show that significant energy can be harnessed from the MSW if requisite LFG management systems are installed. The use of methane as an energy source maximizes the extraction of useful resources from landfills, minimizes the global warming and offsets significant amount of fossil fuels.

  18. Removal of dissolved and suspended radionuclides from Hanford Waste Vitrification Plant liquid wastes

    SciTech Connect

    Sharp, S.D. ); Nankani, F.D. ); Bray, L.A.; Eakin, D.E.; Larson, D.E. )

    1990-12-01

    It was determined during Preliminary Design of the Hanford Waste Vitrification Plant that certain intermediate process liquid waste streams should be decontaminated in a way that would permit the purge of dissolved chemical species from the process recycle shop. This capability is needed to ensure proper control of product glass chemical composition and to avoid excessive corrosion of process equipment. This paper discusses the process design of a system that will remove both radioactive particulates and certain dissolved fission products from process liquid waste streams. Supporting data obtained from literature sources as well as from laboratory- and pilot-scale tests are presented. 3 refs., 1 fig., 3 tabs.

  19. Liquid and Gaseous Waste Operations Department Annual Operating Report, CY 1993

    SciTech Connect

    Maddox, J.J.; Scott, C.B.

    1994-02-01

    This report summarizes the activities of the waste management operations section of the liquid and gaseous waste operations department at ORNL for 1993. The process waste, liquid low-level waste, gaseous waste systems activities are reported, as well as the low-level waste solidification project. Upgrade activities is the various waste processing and treatment systems are summarized. A maintenance activity overview is provided, and program management, training, and other miscellaneous activities are covered.

  20. Waste Form Development for the Solidification of PDCF/MOX Liquid Waste Streams

    SciTech Connect

    COZZI, ALEX

    2004-02-18

    At the Savannah River Site, part of the Department of Energy's nuclear materials complex located in South Carolina, cementation has been selected as the solidification method for high-alpha and low-activity waste streams generated in the planned plutonium disposition facilities. A Waste Solidification Building (WSB) that will be used to treat and solidify three radioactive liquid waste streams generated by the Pit Disassembly and Conversion Facility) and the Mixed Oxide Fuel Fabrication Facility is in the preliminary design stage. The WSB is expected to treat a transuranic (TRU) waste stream composed primarily of americium and two low-level waste (LLW) streams. The acidic wastes will be concentrated in the WSB evaporator and neutralized in a cement head tank prior to solidification. A series of TRU mixes were prepared to produce waste forms exhibiting a range of processing and cured properties. The LLW mixes were prepared using the premix from the preferred TRU waste form. All of the waste forms tested passed the Toxicity Characteristic Leaching Procedure. After processing in the WSB, current plans are to dispose of the solidified TRU waste at the Waste Isolation Pilot Plant in New Mexico and the solidified LLW waste at an approved low-level waste disposal facility.

  1. A Canadian Solution for Management of Mixed Liquid Waste - 13384

    SciTech Connect

    Suryanarayan, Sriram; Husain, Aamir

    2013-07-01

    Mixed liquid wastes (MLW) from Canadian nuclear facilities consist of solvents, PCB (Poly Chlorinated Biphenyls) and non-PCB contaminated oils and aqueous wastes. Historically, MLW drums were shipped to a licensed US facility for destruction via incineration. This option is relatively expensive considering the significant logistics and destruction costs involved. In addition, commercial waste destruction facilities in US cannot accept PCB wastes from non-US jurisdictions. Because of this, Kinectrics has recently developed a novel and flexible process for disposing both PCB as well as non-PCB contaminated MLW within Canada. This avoids the need for cross-border shipments which significantly reduces the complexity and cost for waste disposal. This paper presents an overview of the various approaches and activities undertaken to date by Kinectrics for successfully processing and disposing the MLW drums. A summary of the results, challenges and how they were overcome are also presented. (authors)

  2. ISOLATION OF RADIOACTIVE METALS FROM LIQUID WASTES

    EPA Science Inventory

    Metals are present in many waste streams, and pose challenges with regard to their disposal. Release of metals into the environment presents both human health and ecological concerns. As a result, efforts are directed at reducing their toxicity, bioavailability, and environment...

  3. WEEE and portable batteries in residual household waste: Quantification and characterisation of misplaced waste

    SciTech Connect

    Bigum, Marianne; Petersen, Claus; Scheutz, Charlotte

    2013-11-15

    Highlights: • We analyse 26.1 Mg of residual waste from 3129 Danish households. • We quantify and characterise misplaced WEEE and portable batteries. • We compare misplaced WEEE and batteries to collection through dedicated schemes. • Characterisation showed that primarily small WEEE and light sources are misplaced. • Significant amounts of misplaced batteries were discarded as built-in WEEE. - Abstract: A total of 26.1 Mg of residual waste from 3129 households in 12 Danish municipalities was analysed and revealed that 89.6 kg of Waste Electrical and Electronic Equipment (WEEE), 11 kg of batteries, 2.2 kg of toners and 16 kg of cables had been wrongfully discarded. This corresponds to a Danish household discarding 29 g of WEEE (7 items per year), 4 g of batteries (9 batteries per year), 1 g of toners and 7 g of unidentifiable cables on average per week, constituting 0.34% (w/w), 0.04% (w/w), 0.01% (w/w) and 0.09% (w/w), respectively, of residual waste. The study also found that misplaced WEEE and batteries in the residual waste constituted 16% and 39%, respectively, of what is being collected properly through the dedicated special waste collection schemes. This shows that a large amount of batteries are being discarded with the residual waste, whereas WEEE seems to be collected relatively successfully through the dedicated special waste collection schemes. Characterisation of the misplaced batteries showed that 20% (w/w) of the discarded batteries were discarded as part of WEEE (built-in). Primarily alkaline batteries, carbon zinc batteries and alkaline button cell batteries were found to be discarded with the residual household waste. Characterisation of WEEE showed that primarily small WEEE (WEEE directive categories 2, 5a, 6, 7 and 9) and light sources (WEEE directive category 5b) were misplaced. Electric tooth brushes, watches, clocks, headphones, flashlights, bicycle lights, and cables were items most frequently found. It is recommended that these

  4. Process for immobilizing radioactive boric acid liquid wastes

    SciTech Connect

    Greenhalgh, Wilbur O.

    1986-01-01

    A method of immobilizing boric acid liquid wastes containing radionuclides by neutralizing the solution and evaporating the resulting precipitate to near dryness. The dry residue is then fused into a reduced volume, insoluble, inert, solid form containing substantially all the radionuclides.

  5. Confirmation and quantification of clenbuterol in horse urine using liquid chromatography tandem mass spectrometry triple quadrupole.

    PubMed

    Bishop, Jennifer; Heffron, Brendan; Taddei, Lisa; Benoit, Marc; Hurt, Laura; Costello, Sara; Gross, Melissa; Negrusz, Adam

    2015-03-01

    Clenbuterol (CLE) is used in horses as a bronchodilator and for its anabolic steroid-like effects. CLE is a Class 3 drug according to current Association of Racing Commissioners International (ARCI) Uniform Classification Guidelines. The Racing Medication and Testing Consortium recommended a urine CLE threshold of 140 pg/mL after careful scientific review of the results of studies describing the disposition of CLE in the horse and this threshold was adopted by the ARCI. Enzyme-linked immunosorbent assay was previously used to screen samples for CLE in Illinois, but could not detect such low concentrations in urine. Thus, a liquid-liquid extraction of CLE from urine followed by quantification by liquid chromatography-tandem mass spectrometry was developed and validated. Method validation included testing stability, ion suppression and enhancement, precision, accuracy and uncertainty. Intra-, interday and total precision and accuracy were calculated for each control and found to be within the ±15% acceptance range. The Guide to the Expression of Uncertainty in Measurement approach was used to calculate uncertainty, which was 11% at the 95% confidence level. In the past 5 years, only 15 samples were reported as positive for CLE in Illinois. This new method was used in a pilot program to screen and confirm samples received from thoroughbred and harness horses. PMID:25505053

  6. Simultaneous liquid chromatography-mass spectrometry quantification of cefixime and clavulanic acid in human plasma.

    PubMed

    Dubala, Anil; Nagarajan, Janaki Sankarachari Krishnan; Vimal, Chandran Sathish; George, Renjith

    2015-01-01

    A simple and specific liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry (LC-APCI-MS) assay method has been developed and fully validated for the simultaneous quantification of cefixime (CX) and clavulanic acid (CA) in human plasma. Analytes and internal standard were extracted from human plasma by a solid phase extraction technique using a Sam prep (3 mL, 100 mg) extraction cartridge. The extracted samples were chromatographed on a reverse phase C18 column using a mixture of methanol : acetonitrile : 2 mM ammonium acetate (pH 3.5) (25 : 25 : 50, v/v/v) as the mobile phase at a flow rate of 0.8 mL/min. Quantification of the analytes were carried out using single quadrupole LC-APCI-MS through selected ion monitoring at m/z 452 and 198, respectively, for CX and CA. The assay was linear over the concentration range of 0.05-10.0 and 0.1-10.0 μg/mL, respectively, for CX and CA. The mean plasma extraction recoveries of the CX and CA were found to be 95.20-96.27% and 94.67-95.58%, respectively. The method was successfully applied for the determination of pharmacokinetics of CX and CA after oral administration of single dosage CX/CA (200/125 mg) pill to the humans (n = 12). PMID:25209681

  7. Methane-oxygen electrochemical coupling in an ionic liquid: a robust sensor for simultaneous quantification.

    PubMed

    Wang, Zhe; Guo, Min; Baker, Gary A; Stetter, Joseph R; Lin, Lu; Mason, Andrew J; Zeng, Xiangqun

    2014-10-21

    Current sensor devices for the detection of methane or natural gas emission are either expensive and have high power requirements or fail to provide a rapid response. This report describes an electrochemical methane sensor utilizing a non-volatile and conductive pyrrolidinium-based ionic liquid (IL) electrolyte and an innovative internal standard method for methane and oxygen dual-gas detection with high sensitivity, selectivity, and stability. At a platinum electrode in bis(trifluoromethylsulfonyl)imide (NTf2)-based ILs, methane is electro-oxidized to produce CO2 and water when an oxygen reduction process is included. The in situ generated CO2 arising from methane oxidation was shown to provide an excellent internal standard for quantification of the electrochemical oxygen sensor signal. The simultaneous quantification of both methane and oxygen in real time strengthens the reliability of the measurements by cross-validation of two ambient gases occurring within a single sample matrix and allows for the elimination of several types of random and systematic errors in the detection. We have also validated this IL-based methane sensor employing both conventional solid macroelectrodes and flexible microfabricated electrodes using single- and double-potential step chronoamperometry. PMID:25093213

  8. Recent progress in polar metabolite quantification in plants using liquid chromatography–mass spectrometry.

    PubMed

    Liu, Zhiqian; Rochfort, Simone

    2014-09-01

    Metabolite analysis or metabolomics is an important component of systems biology in the post-genomic era. Although separate liquid chromatography (LC) methods for quantification of the major classes of polar metabolites of plants have been available for decades, a single method that enables simultaneous determination of hundreds of polar metabolites is possible only with gas chromatography–mass spectrometry (GC–MS) techniques. The rapid expansion of new LC stationary phases in the market and the ready access of mass spectrometry in many laboratories provides an excellent opportunity for developing LC–MS based methods for multi-target quantification of polar metabolites. Although various LC–MS methods have been developed over the last 10 years with the aim to quantify one or more classes of polar compounds in different matrices, currently there is no consensus LC–MS method that is widely used in plant metabolomics studies. The most promising methods applicable to plant metabolite analysis will be reviewed in this paper and the major problems encountered highlighted. The aim of this review is to provide plant scientists, with limited to moderate experience in analytical chemistry, with up-to-date and simplified information regarding the current status of polar metabolite analysis using LC–MS techniques. PMID:25340205

  9. WEEE and portable batteries in residual household waste: quantification and characterisation of misplaced waste.

    PubMed

    Bigum, Marianne; Petersen, Claus; Christensen, Thomas H; Scheutz, Charlotte

    2013-11-01

    A total of 26.1Mg of residual waste from 3129 households in 12 Danish municipalities was analysed and revealed that 89.6kg of Waste Electrical and Electronic Equipment (WEEE), 11kg of batteries, 2.2kg of toners and 16kg of cables had been wrongfully discarded. This corresponds to a Danish household discarding 29g of WEEE (7 items per year), 4g of batteries (9 batteries per year), 1g of toners and 7g of unidentifiable cables on average per week, constituting 0.34% (w/w), 0.04% (w/w), 0.01% (w/w) and 0.09% (w/w), respectively, of residual waste. The study also found that misplaced WEEE and batteries in the residual waste constituted 16% and 39%, respectively, of what is being collected properly through the dedicated special waste collection schemes. This shows that a large amount of batteries are being discarded with the residual waste, whereas WEEE seems to be collected relatively successfully through the dedicated special waste collection schemes. Characterisation of the misplaced batteries showed that 20% (w/w) of the discarded batteries were discarded as part of WEEE (built-in). Primarily alkaline batteries, carbon zinc batteries and alkaline button cell batteries were found to be discarded with the residual household waste. Characterisation of WEEE showed that primarily small WEEE (WEEE directive categories 2, 5a, 6, 7 and 9) and light sources (WEEE directive category 5b) were misplaced. Electric tooth brushes, watches, clocks, headphones, flashlights, bicycle lights, and cables were items most frequently found. It is recommended that these findings are taken into account when designing new or improving existing special waste collection schemes. Improving the collection of WEEE is also recommended as one way to also improve the collection of batteries due to the large fraction of batteries found as built-in. The findings in this study were comparable to other western European studies, suggesting that the recommendations made in this study could apply to other

  10. Low level liquid waste conditioning at the ENEA Trisaia Centre

    SciTech Connect

    Di Pace, L.; Risoluti, P.; Lippolis, G.

    1993-12-31

    At the ENEA Trisaia Centre (Southern Italy) 56 m{sup 3} of radioactive low-level liquid wastes, generated during past operations of the ITREC reprocessing pilot plant and presently stored in a 60,000 liter carbon steel tank, have to be solidified in order to fulfill the specific requirements established by the Safety Authority, taking into account a Technical Guide issued on the matter of Radioactive Waste Management. For this purpose, the design of a facility, for conditioning this liquid LLW by cementation, was completed and submitted to the Safety Authority. The facility, named SIRTE, is composed of a transfer system and a cementation section based on the MOWA technique. Furthermore a qualification program for the treatment and conditioning process has been completed, in order to define the best cement matrix formulation, at the ENEA Casaccia Research Centre. The main characteristics of the cement matrix, coming from tests on simulated conditioned waste, are given.

  11. Iraq liquid radioactive waste tanks maintenance and monitoring program plan.

    SciTech Connect

    Dennis, Matthew L.; Cochran, John Russell; Sol Shamsaldin, Emad

    2011-10-01

    The purpose of this report is to develop a project management plan for maintaining and monitoring liquid radioactive waste tanks at Iraq's Al-Tuwaitha Nuclear Research Center. Based on information from several sources, the Al-Tuwaitha site has approximately 30 waste tanks that contain varying amounts of liquid or sludge radioactive waste. All of the tanks have been non-operational for over 20 years and most have limited characterization. The program plan embodied in this document provides guidance on conducting radiological surveys, posting radiation control areas and controlling access, performing tank hazard assessments to remove debris and gain access, and conducting routine tank inspections. This program plan provides general advice on how to sample and characterize tank contents, and how to prioritize tanks for soil sampling and borehole monitoring.

  12. Quantification of homocysteine and cysteine by derivatization with pyridoxal 5'-phosphate and hydrophilic interaction liquid chromatography.

    PubMed

    Głowacki, Rafał; Stachniuk, Justyna; Borowczyk, Kamila; Jakubowski, Hieronim

    2016-03-01

    A simple and rapid assay using pyridoxal 5'-phosphate (PLP) as a derivatizing reagent was developed for the simultaneous determination of homocysteine (Hcy) and cysteine (Cys) in human plasma. Derivatization with PLP affords UV-absorbing tetrahydrothiazine and thiazolidine derivatives of Hcy and Cys, respectively. Separation of these derivatives was achieved in 5 min using a hydrophilic interaction liquid chromatography, followed by UV detection at 330 nm. Linearity in detector response was observed over the range of 0.25-20 μM for Hcy and 10-300 μM for Cys. The limit of quantification (LOQ) values for Hcy and Cys were 0.25 and 2.5 μM, respectively. The method was successfully applied to plasma samples donated by apparently healthy volunteers. Graphical Abstract A flow chart diagram of analytical procedure for total plasma Hcy and Cys determination. PMID:26794212

  13. Supported liquid inorganic membranes for nuclear waste separation

    SciTech Connect

    Bhave, Ramesh R; DeBusk, Melanie M; DelCul, Guillermo D; Delmau, Laetitia H; Narula, Chaitanya K

    2015-04-07

    A system and method for the extraction of americium from radioactive waste solutions. The method includes the transfer of highly oxidized americium from an acidic aqueous feed solution through an immobilized liquid membrane to an organic receiving solvent, for example tributyl phosphate. The immobilized liquid membrane includes porous support and separating layers loaded with tributyl phosphate. The extracted solution is subsequently stripped of americium and recycled at the immobilized liquid membrane as neat tributyl phosphate for the continuous extraction of americium. The sequestered americium can be used as a nuclear fuel, a nuclear fuel component or a radiation source, and the remaining constituent elements in the aqueous feed solution can be stored in glassified waste forms substantially free of americium.

  14. Quantification of Bile Acids in Traditional Animal Medicines and Their Preparations Using Ultra High-Performance Liquid Chromatography-Mass Spectrometry in the Multiple Reaction Monitoring Mode.

    PubMed

    Yerigui; Wu, Xiu-Hong; Wang, Xi-Jun; Ma, Chao-Mei

    2016-01-01

    An ultra-high-performance liquid chromatograph-triple quadrupole mass spectrometry has been established and validated for the simultaneous quantification of 15 bile acids in four traditional animal medicines and their preparations. The separations of bile acids were performed on an Agilent ZORBAX Eclipse XDB-C18 column (50 × 2.1 mm; 1.8 μm) with methanol-0.1% formic acid as the mobile phase. Glycyrrhetinic acid was added as internal standard owing to its similar physiochemical properties with the bile acids. Using this condition, detected in the multiple reaction monitoring mode, the 15 bile acids, including three groups of isomers, were well quantified individually. Method validation showed that the linear regression relationship (r(2), 0.9993 - 0.9999), precisions (intra-day RSD, 0.96 - 4.31%; inter-day, 1.73 - 4.43%), and recovery (95.3 - 120.9%) were all satisfactory. The analysis results showed that bear bile and bezoar (Niu Huang) as well as their formulations contained large amounts of most of the 15 bile acids. In addition, this research revealed for the first time the presences of bile acids in animal waste medication used in traditional medicine from two clinics, Hei-Bing-Pian (discharges of wild boar) and Trogopterus Dung. The established method could be used for the quantification of other bile- or animal waste-based crude drugs and their formulated products. PMID:27169647

  15. Pilot studies to achieve waste minimization and enhance radioactive liquid waste treatment at the Los Alamos National Laboratory Radioactive Liquid Waste Treatment Facility

    SciTech Connect

    Freer, J.; Freer, E.; Bond, A.

    1996-07-01

    The Radioactive and Industrial Wastewater Science Group manages and operates the Radioactive Liquid Waste Treatment Facility (RLWTF) at the Los Alamos National Laboratory (LANL). The RLWTF treats low-level radioactive liquid waste generated by research and analytical facilities at approximately 35 technical areas throughout the 43-square-mile site. The RLWTF treats an average of 5.8 million gallons (21.8-million liters) of liquid waste annually. Clarifloculation and filtration is the primary treatment technology used by the RLWTF. This technology has been used since the RLWTF became operable in 1963. Last year the RLWTF achieved an average of 99.7% removal of gross alpha activity in the waste stream. The treatment process requires the addition of chemicals for the flocculation and subsequent precipitation of radionuclides. The resultant sludge generated during this process is solidified in drums and stored or disposed of at LANL.

  16. Sensitive quantification of omeprazole and its metabolites in human plasma by liquid chromatography-mass spectrometry.

    PubMed

    Hofmann, Ute; Schwab, Matthias; Treiber, Gerd; Klotz, Ulrich

    2006-02-01

    A sensitive method was developed for the simultaneous determination of omeprazole and its major metabolites 5-hydroxyomeprazole and omeprazole sulfone in human plasma by HPLC-electrospray mass spectrometry. Following liquid-liquid extraction HPLC separation was achieved on a ProntoSil AQ, C18 column using a gradient with 10 mM ammonium acetate in water (pH 7.25) and acetonitrile. The mass spectrometer was operated in the selected ion monitoring mode using the respective MH(+) ions, m/z 346 for omeprazole, m/z 362 for 5-hydroxy-omeprazole and omeprazol-sulfone and m/z 300 for the internal standard (2-{[(3,5-dimethylpyridine-2-yl)methyl]thio}-1H-benzimidazole-5-yl)methanol. The limit of quantification (LOQ) achieved with this method was 5 ng/ml for 5-hydroxyomeprazole and 10 ng/ml for omeprazole and omeprazole-sulfone using 0.25 ml of plasma. Intra- and inter-assay variability was below 11% over the whole concentration range from 5 to 250 ng/ml for 5-hydroxyomeprazol and from 10 to 750 ng/ml for omeprazole and omeprazole-sulfone. The method was successfully applied to the determination of pharmacokinetic parameters of esomeprazole and the two major metabolites after a single dose and under steady state conditions. PMID:16338182

  17. Determination of ethylenediaminetetraacetic acid in nuclear waste by high-performance liquid chromatography coupled with electrospray mass spectrometry.

    PubMed

    du Bois de Maquillé, Laurence; Renaudin, Laetitia; Goutelard, Florence; Jardy, Alain; Vial, Jérôme; Thiébaut, Didier

    2013-02-01

    EDTA is a chelating agent that has been used in decontamination processes. Its quantification is required for nuclear waste management because it affects the mobility of radionuclides and metals in environment and, thus, can harm the safety of the storage. Ion-pair chromatography coupled with electrospray mass spectrometry detection is a convenient method for quantitative analysis of EDTA but EDTA should be present as a single anionic chelate form. However, radioactive liquid wastes contain high concentrations of heavy metals and salts and consequently, EDTA is present as several chelates. Speciation studies were carried out to choose a metal cation to be added in excess to the solution to obtain a major chelate form. Fe is the predominant cation and Fe(III)-EDTA is thermodynamically favored but these speciation studies showed that ferric hydroxide precipitated above pH 2. Consequently, it was not possible to quantify EDTA as Fe(III)-EDTA complex. Therefore, Ni(2+) was chosen but its use implied pretreatment with a base of the solution to eliminate Fe. Deuterated EDTA was used as tracer in order to validate the whole procedure, from the treatment with a base to the final analysis by HPLC-ESI-MS. This analytical method was successfully applied for EDTA quantification in two real effluents resulting from a nuclear liquid waste process. A recovery rate between 60 and 80% was obtained. The limit of detection of this method was determined at 34×10(-9)mol L(-1). PMID:23312862

  18. RECOVERY OF MERCURY FROM CONTAMINATED LIQUID WASTES

    SciTech Connect

    Robin M. Stewart

    1999-09-29

    Mercury was widely used in U.S. Department of Energy (DOE) weapons facilities, resulting in a broad range of mercury-contaminated wastes and wastewaters. Some of the mercury contamination has escaped to the local environment, particularly at the Y-12 Plant in Oak Ridge, Tennessee, where approximately 330 metric tons of mercury were discharged to the environment between 1953 and 1963 (TN & Associates, 1998). Effective removal of mercury contamination from water is a complex and difficult problem. In particular, mercury treatment of natural waters is difficult because of the low regulatory standards. For example, the Environmental Protection Agency has established a national ambient water quality standard of 12 parts-per-trillion (ppt), whereas the standard is 1.8 ppt in the Great Lakes Region. In addition, mercury in the environment is typically present in several different forms, but sorption processes are rarely effective with more than one or two of these forms. To meet the low regulatory discharge limits, an effective sorption process must be able to address all forms of mercury present in the water. One approach is to apply different sorbents in series depending on the mercury speciation and the regulatory discharge limits. ADA Technologies, Inc. has developed four new sorbents to address the variety of mercury species present in industrial discharges and natural waters. Three of these sorbents have been field tested on contaminated creek water at the Y-12 Plant. Two of these sorbents have been successfully demonstrated very high removal efficiencies for soluble mercury species, reducing mercury concentrations at the outlet of a pilot-scale system to less than 12 ppt for as long as six months. The other sorbent tested at the Y-12 Plant targeted colloidal mercury not removed by standard sorption or filtration processes. At the Y-12 Plant, colloidal mercury appears to be associated with iron, so a sorbent that removes mercury-iron complexes in the presence of a

  19. Identification and Quantification of Dimethylamylamine in Geranium by Liquid Chromatography Tandem Mass Spectrometry

    PubMed Central

    Li, J.S.; Chen, M.; Li, Z.C.

    2012-01-01

    A sensitive and reliable method of liquid chromatography–electrospray ionization/tandem mass spectrometry (LC-ESI/MS/ MS) was developed and validated for determining 1,3-dimethylamylamine (1,3-DMAA) and 1,4-dimethylamylamine (1,4-DMAA) in geranium plants (Pelargonium graveolens). The sample was extracted with 0.5 M HCl and purified by liquid-liquid partition with hexane. The parameters for reverse-phase (C18) LC and positive ESI/MS/MS were optimized. The matrix effect, specificity, linearity, precision, accuracy and reproducibility of the method were determined and evaluated. The method was linear over a range of 0.10–10.00 ng/mL examined, with R2 of 0.99 for both 1,3-DMAA and 1,4-DMAA. The recoveries from spiked concentrations between 5.00–40.00 ng/g were 85.1%–104.9% for 1,3-DMAA, with relative standard deviation (RSD) of 2.9%–11.0%, and 82.9%–101.8% for 1,4-DMAA, with RSD of 3.2%–11.7%. The instrument detection limit was 1–2 pg for both DMAAs. The quantification limit was estimated to be 1–2 ng/g for the plant sample. This method was successfully applied to the quantitative determination of 1,3- and 1,4-DMAA in both geranium plant and geranium oil. PMID:22915838

  20. Quantification of six cannabinoids and metabolites in oral fluid by liquid chromatography-tandem mass spectrometry.

    PubMed

    Desrosiers, Nathalie A; Scheidweiler, Karl B; Huestis, Marilyn A

    2015-08-01

    Δ(9) -Tetrahydrocannabinol (THC) is the most commonly analyzed cannabinoid in oral fluid (OF); however, its metabolite 11-nor-9-carboxy-THC (THCCOOH) offers the advantage of documenting active consumption, as it is not detected in cannabis smoke. Analytical challenges such as low (ng/L) THCCOOH OF concentrations hampered routine OF THCCOOH monitoring. Presence of minor cannabinoids like cannabidiol and cannabinol offer the advantage of identifying recent cannabis intake. Published OF cannabinoids methods have limitations, including few analytes and lengthy derivatization. We developed and validated a sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for THC, its metabolites, 11-hydroxy-THC and THCCOOH quantification, and other natural cannabinoids including tetrahydrocannabivarin (THCV), cannabidiol (CBD), and cannabigerol (CBG) in 1 mL OF collected with the Quantisal device. After solid-phase extraction, chromatography was performed on a Selectra PFPP column with a 0.15% formic acid in water and acetonitrile gradient with a 0.5 mL/min flow rate. All analytes were monitored in positive mode atmospheric pressure chemical ionization (APCI) with multiple reaction monitoring. Limits of quantification were 15 ng/L THCCOOH and 0.2 µg/L for all other analytes. Linear ranges extended to 3750 ng/L THCCOOH, 100 µg/L THC, and 50 µg/L for all other analytes. Inter-day analytical recoveries (bias) and imprecision at low, mid, and high quality control (QC) concentrations were 88.7-107.3% and 2.3-6.7%, respectively (n = 20). Mean extraction efficiencies and matrix effects evaluated at low and high QC were 75.9-86.1% and 8.4-99.4%, respectively. This method will be highly useful for workplace, criminal justice, drug treatment and driving under the influence of cannabis OF testing. PMID:25428610

  1. Simultaneous quantification of Pacific ciguatoxins in fish blood using liquid chromatography-tandem mass spectrometry.

    PubMed

    Mak, Yim Ling; Wu, Jia Jun; Chan, Wing Hei; Murphy, Margaret B; Lam, James C W; Chan, Leo L; Lam, Paul K S

    2013-04-01

    Ciguatera fish poisoning (CFP) is a food intoxication caused by exposure to ciguatoxins (CTXs) in coral reef fish. Rapid analytical methods have been developed recently to quantify Pacific-CTX-1 (P-CTX-1) in fish muscle, but it is destructive and can cause harm to valuable live coral reef fish. Also fish muscle extract was complex making CTX quantification challenging. Not only P-CTX-1, but also P-CTX-2 and P-CTX-3 could be present in fish, contributing to ciguatoxicity. Therefore, an analytical method for simultaneous quantification of P-CTX-1, P-CTX-2, and P-CTX-3 in whole blood of marketed coral reef fish using sonication, solid-phase extraction (SPE), and liquid chromatography tandem mass spectrometry (LC-MS/MS) was developed. The optimized method gave acceptable recoveries of P-CTXs (74-103 %) in fish blood. Matrix effects (6-26 %) in blood extracts were found to be significantly reduced compared with those in muscle extracts (suppressed by 34-75 % as reported in other studies), thereby minimizing potential for false negative results. The target P-CTXs were detectable in whole blood from four coral reef fish species collected in a CFP-endemic region. Similar trends in total P-CTX levels and patterns of P-CTX composition profiles in blood and muscle of these fish were observed, suggesting a relationship between blood and muscle levels of P-CTXs. This optimized method provides an essential tool for studies of P-CTX pharmacokinetics and pharmacodynamics in fish, which are needed for establishing the use of fish blood as a reliable sample for the assessment and control of CFP. PMID:23392409

  2. Automated Label-free Quantification of Metabolites from Liquid Chromatography–Mass Spectrometry Data*

    PubMed Central

    Kenar, Erhan; Franken, Holger; Forcisi, Sara; Wörmann, Kilian; Häring, Hans-Ulrich; Lehmann, Rainer; Schmitt-Kopplin, Philippe; Zell, Andreas; Kohlbacher, Oliver

    2014-01-01

    Liquid chromatography coupled to mass spectrometry (LC-MS) has become a standard technology in metabolomics. In particular, label-free quantification based on LC-MS is easily amenable to large-scale studies and thus well suited to clinical metabolomics. Large-scale studies, however, require automated processing of the large and complex LC-MS datasets. We present a novel algorithm for the detection of mass traces and their aggregation into features (i.e. all signals caused by the same analyte species) that is computationally efficient and sensitive and that leads to reproducible quantification results. The algorithm is based on a sensitive detection of mass traces, which are then assembled into features based on mass-to-charge spacing, co-elution information, and a support vector machine–based classifier able to identify potential metabolite isotope patterns. The algorithm is not limited to metabolites but is applicable to a wide range of small molecules (e.g. lipidomics, peptidomics), as well as to other separation technologies. We assessed the algorithm's robustness with regard to varying noise levels on synthetic data and then validated the approach on experimental data investigating human plasma samples. We obtained excellent results in a fully automated data-processing pipeline with respect to both accuracy and reproducibility. Relative to state-of-the art algorithms, ours demonstrated increased precision and recall of the method. The algorithm is available as part of the open-source software package OpenMS and runs on all major operating systems. PMID:24176773

  3. Liquid and Gaseous Waste Operations Department annual operating report CY 1996

    SciTech Connect

    Maddox, J.J.; Scott, C.B.

    1997-03-01

    This annual report summarizes operating activities dealing with the process waste system, the liquid low-level waste system, and the gaseous waste system. It also describes upgrade activities dealing with the process and liquid low-level waste systems, the cathodic protection system, a stack ventilation system, and configuration control. Maintenance activities are described dealing with nonradiological wastewater treatment plant, process waste treatment plant and collection system, liquid low-level waste system, and gaseous waste system. Miscellaneous activities include training, audits/reviews/tours, and environmental restoration support.

  4. [A system for decontamination of liquid radioactive waste produced in in vitro tests in nuclear medicine].

    PubMed

    Tsuchiya, T; Norimura, T; Ueno, T

    1983-06-01

    It is well known that very large storage tanks for radioactive liquids are necessary for the disposal of liquid radioactive waste. In vitro tests in radioimmunoassay in nuclear medicine are rapidly increasing for clinical examination causing marked increase in the volume of liquid radioactive waste. Thus we have developed a system for decontaminating radioactivity from liquid waste. In the first step, the liquid waste is boiled by a sterilizer and, in the second step, this sterilised liquid is filtered by a cylindrical filter (Toyo filter No. 84). After filtration, the liquid waste is passed into a beaded charcoal column and an ion exchange resin (Amberlite IRA 402) column. After these treatments, the radioactivity level of liquid waste is lowered to less than 1% of the original radioactivity. We are now in the planning stages of building an apparatus for practical use. PMID:6622764

  5. Decontamination of a radioactive waste liquid by electrodialysis

    SciTech Connect

    Lundstrom, J.E.

    1987-02-24

    An apparatus is described for the removal and recovery of acidic and radioactive components of a liquid waste stream comprising in combination a series of at least two electrodialysis units or stacks. Each stack is comprised of a cathode chamber at one terminal end, and an anode chamber at the opposite terminal end. The chambers contain respectively a cathode and anode electrode. A deacidification stack is the first stack in the series having all of its chambers being separated one from the other by separate anion selective membranes defining between the electrode chambers at least one neutral liquid chamber positioned adjacent to the cathode chamber. A primary desalting stack is the second stack in the series comprising a multi-chamber unit having alternating salt diluting and salt concentrating chambers defined by alternating cation and anion selective membranes, means for introducing a liquid to be treated into the cathode chamber of the deacidification stack with exit means for withdrawal of the liquid, and means for passing the withdrawn liquid into and out of the salt diluting chambers of the primary desalting stack. A means is included for introducing a liquid into and out of the concentrating and electrode chambers of the primary desalting stack and for passing a direct electric current transversely across the membranes and chambers of each stack in the series.

  6. Quantification of maltol in Korean ginseng (Panax ginseng) products by high-performance liquid chromatography-diode array detector

    PubMed Central

    Jeong, Hyun Cheol; Hong, Hee-Do; Kim, Young-Chan; Rhee, Young Kyoung; Choi, Sang Yoon; Kim, Kyung-Tack; Kim, Sung Soo; Lee, Young-Chul; Cho, Chang-Won

    2015-01-01

    Background: Maltol, as a type of phenolic compounds, is produced by the browning reaction during the high-temperature treatment of ginseng. Thus, maltol can be used as a marker for the quality control of various ginseng products manufactured by high-temperature treatment including red ginseng. For the quantification of maltol in Korean ginseng products, an effective high-performance liquid chromatography-diode array detector (HPLC-DAD) method was developed. Materials and Methods: The HPLC-DAD method for maltol quantification coupled with a liquid-liquid extraction (LLE) method was developed and validated in terms of linearity, precision, and accuracy. An HPLC separation was performed on a C18 column. Results: The LLE methods and HPLC running conditions for maltol quantification were optimized. The calibration curve of the maltol exhibited good linearity (R2 = 1.00). The limit of detection value of maltol was 0.26 μg/mL, and the limit of quantification value was 0.79 μg/mL. The relative standard deviations (RSDs) of the data of the intra- and inter-day experiments were <1.27% and 0.61%, respectively. The results of the recovery test were 101.35–101.75% with an RSD value of 0.21–1.65%. The developed method was applied successfully to quantify the maltol in three ginseng products manufactured by different methods. Conclusion: The results of validation demonstrated that the proposed HPLC-DAD method was useful for the quantification of maltol in various ginseng products. PMID:26246746

  7. Idaho Nuclear Technology and Engineering Center Newly Generated Liquid Waste Demonstration Project Feasibility Study

    SciTech Connect

    Herbst, A.K.

    2000-02-01

    A research, development, and demonstration project for the grouting of newly generated liquid waste (NGLW) at the Idaho Nuclear Technology and Engineering Center is considered feasible. NGLW is expected from process equipment waste, decontamination waste, analytical laboratory waste, fuel storage basin waste water, and high-level liquid waste evaporator condensate. The potential grouted waste would be classed as mixed low-level waste, stabilized and immobilized to meet RCRA LDR disposal in a grouting process in the CPP-604 facility, and then transported to the state.

  8. Dielectric Properties of Low-Level Liquid Waste

    SciTech Connect

    L. E. Lagos; M. A. Ebadian

    1998-10-20

    The purpose of this study was to develop a data collection containing values for the dielectric properties of various low-level liquid waste (LLLW) simulants measured as a function of frequency, temperature, and composition. The investigation was motivated by current interest in the use of microwave processing for the treatment of radioactive waste. A large volume of transuranic liquid and sludge produced by the U.S. Department of Defense (DOD) during the production of nuclear fiel bars is stored at several U.S. Department of Energy (DOE) sites around the United States. Waste storage and disposal space is scarce, expensive, and must be minimized. Thus, several DOE sites are pursuing the use of microwave heating as a means of achieving volume reduction and solidification of low-level liquid wastes. It is important to know which microwave frequencies should be employed tc achieve the most efficient processing at a range of different temperatures. The dielectric properties of the LLLW simulants can be utilized to determine the optimum frequencies for use with a particular LLLW or with other LLLWS of similar composition. Furthermore, nonlinear thermal processes, such as thermal runaway, which occur in the material being treated cannot be modeled without a knowledge of the temperature dependence of the dielectric properties. Often, this data does not exist; however, when it does, only very limited data near room temperature are available. The data collection generated in this study can be used to predict the behavior of a variety of microwave thermal treatment technologies, which have the potential of substantially reducing the volume of the LLLWS that are currently stored at many DOE sites. This information should help the users of the microwave reduction and solidification technology to optimize microwave processes used in the treatment of LLLW. The microwave reduction and solidification technology has clear advantages over other methods of reducing LLLWS. These

  9. Using benchmarking to minimize common DOE waste streams. Volume 1, Methodology and liquid photographic waste

    SciTech Connect

    Levin, V.

    1994-04-01

    Finding innovative ways to reduce waste streams generated at Department of Energy (DOE) sites by 50% by the year 2000 is a challenge for DOE`s waste minimization efforts. This report examines the usefulness of benchmarking as a waste minimization tool, specifically regarding common waste streams at DOE sites. A team of process experts from a variety of sites, a project leader, and benchmarking consultants completed the project with management support provided by the Waste Minimization Division EM-352. Using a 12-step benchmarking process, the team examined current waste minimization processes for liquid photographic waste used at their sites and used telephone and written questionnaires to find ``best-in-class`` industrv partners willing to share information about their best waste minimization techniques and technologies through a site visit. Eastman Kodak Co., and Johnson Space Center/National Aeronautics and Space Administration (NASA) agreed to be partners. The site visits yielded strategies for source reduction, recycle/recovery of components, regeneration/reuse of solutions, and treatment of residuals, as well as best management practices. An additional benefit of the work was the opportunity for DOE process experts to network and exchange ideas with their peers at similar sites.

  10. Selective classification and quantification model of C&D waste from material resources consumed in residential building construction.

    PubMed

    Mercader-Moyano, Pilar; Ramírez-de-Arellano-Agudo, Antonio

    2013-05-01

    The unfortunate economic situation involving Spain and the European Union is, among other factors, the result of intensive construction activity over recent years. The excessive consumption of natural resources, together with the impact caused by the uncontrolled dumping of untreated C&D waste in illegal landfills have caused environmental pollution and a deterioration of the landscape. The objective of this research was to generate a selective classification and quantification model of C&D waste based on the material resources consumed in the construction of residential buildings, either new or renovated, namely the Conventional Constructive Model (CCM). A practical example carried out on ten residential buildings in Seville, Spain, enabled the identification and quantification of the C&D waste generated in their construction and the origin of the waste, in terms of the building material from which it originated and its impact for every m(2) constructed. This model enables other researchers to establish comparisons between the various improvements proposed for the minimization of the environmental impact produced by building a CCM, new corrective measures to be proposed in future policies that regulate the production and management of C&D waste generated in construction from the design stage to the completion of the construction process, and the establishment of sustainable management for C&D waste and for the selection of materials for the construction on projected or renovated buildings. PMID:23446631

  11. Liquid and Gaseous Waste Operations Department annual operating report CY 1994

    SciTech Connect

    Maddox, J.J.; Scott, C.B.

    1995-03-01

    This report presents details about the operation of the liquid and gaseous waste department of Oak Ridge National Laboratory for the calendar year 1994. Topics discussed include; process waste system, upgrade activities, low-level liquid radioactive waste solidification project, maintenance activities, and other activities such as training, audits, and tours.

  12. A study of waste liquid crystal display generation in mainland China.

    PubMed

    Liu, Zhifeng; Xu, Zeying; Huang, Haihong; Li, Bingbing

    2016-01-01

    The generation of liquid crystal display waste is becoming a serious social problem. Predicting liquid crystal display waste status is the foundation for establishing a recycling network; however, the difficulty in predicting liquid crystal display waste quantity lies in data mining. In order to determine the quantity and the distribution of liquid crystal display waste in China, the four top-selling liquid crystal display products (liquid crystal display TVs, desktop PCs, notebook PCs, and mobile phones) were selected as study objects. Then, the extended logistic model and market supply A method was used to predict the quantity of liquid crystal display waste products. Moreover, the distribution of liquid crystal display waste products in different regions was evaluated by examining the consumption levels of household equipment. The results revealed that the quantity of waste liquid crystal displays would increase rapidly in the next decade. In particular, the predicted quantity of waste liquid crystal displays would rise to approximately 4.262 × 10(9) pieces in 2020, and the total display area (i.e. the surface area of liquid crystal display panels) of waste liquid crystal displays would reach 5.539 × 10(7) m(2). The prediction on the display area of waste liquid crystal display TVs showed that it would account for 71.5% of the total display area by 2020. Meanwhile, the quantity of waste mobile phones would significantly grow, increasing 5.8 times from 2012 to 2020. In terms of distribution, Guangdong is the top waste liquid crystal display-generating province in China, followed by Jiangsu, Shandong, Henan, Zhejiang, and Sichuan. Considering its regional characteristics, Guangdong has been proposed to be the most important location of the recycling network. PMID:26542394

  13. Recovering low-turbidity cutting liquid from silicon slurry waste.

    PubMed

    Tsai, Tzu-Hsuan; Shih, Yu-Pei

    2014-04-30

    In order to recover a low-turbidity polyalkylene glycol (PAG) liquid from silicon slurry waste by sedimentation, temperatures were adjusted, and acetone, ethanol or water was used as a diluent. The experimental results show that the particles in the waste would aggregate and settle readily by using water as a diluent. This is because particle surfaces had lower surface potential value and weaker steric stabilization in PAG-water than in PAG-ethanol or PAG-acetone solutions. Therefore, water is the suggested diluent for recovering a low-turbidity PAG (<100 NTU) by sedimentation. After 50 wt.% water-assisted sedimentation for 21 days, the solid content of the upper liquid reduced to 0.122 g/L, and the turbidity decreased to 44 NTU. The obtained upper liquid was then vacuum-distillated to remove water. The final recovered PAG with 0.37 NTU had similar viscosity and density to the unused PAG and could be reused in the cutting process. PMID:24637449

  14. High performance liquid chromatography-charged aerosol detection applying an inverse gradient for quantification of rhamnolipid biosurfactants.

    PubMed

    Behrens, Beate; Baune, Matthias; Jungkeit, Janek; Tiso, Till; Blank, Lars M; Hayen, Heiko

    2016-07-15

    A method using high performance liquid chromatography coupled to charged-aerosol detection (HPLC-CAD) was developed for the quantification of rhamnolipid biosurfactants. Qualitative sample composition was determined by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS). The relative quantification of different derivatives of rhamnolipids including di-rhamnolipids, mono-rhamnolipids, and their precursors 3-(3-hydroxyalkanoyloxy)alkanoic acids (HAAs) differed for two compared LC-MS instruments and revealed instrument dependent responses. Our here reported HPLC-CAD method provides uniform response. An inverse gradient was applied for the absolute quantification of rhamnolipid congeners to account for the detector's dependency on the solvent composition. The CAD produces a uniform response not only for the analytes but also for structurally different (nonvolatile) compounds. It was demonstrated that n-dodecyl-β-d-maltoside or deoxycholic acid can be used as alternative standards. The method of HPLC-ultra violet (UV) detection after a derivatization of rhamnolipids and HAAs to their corresponding phenacyl esters confirmed the obtained results but required additional, laborious sample preparation steps. Sensitivity determined as limit of detection and limit of quantification for four mono-rhamnolipids was in the range of 0.3-1.0 and 1.2-2.0μg/mL, respectively, for HPLC-CAD and 0.4 and 1.5μg/mL, respectively, for HPLC-UV. Linearity for HPLC-CAD was at least 0.996 (R(2)) in the calibrated range of about 1-200μg/mL. Hence, the here presented HPLC-CAD method allows absolute quantification of rhamnolipids and derivatives. PMID:27283098

  15. Speciation and quantification of vapor phases in soy biodiesel and waste cooking oil biodiesel.

    PubMed

    Peng, Chiung-Yu; Lan, Cheng-Hang; Dai, Yu-Tung

    2006-12-01

    This study characterizes the compositions of two biodiesel vapors, soy biodiesel and waste cooking oil biodiesel, to provide a comprehensive understanding of biodiesels. Vapor phases were sampled by purging oil vapors through thermal desorption tubes which were then analyzed by the thermal desorption/GC/MS system. The results show that the compounds of biodiesel vapors can be divided into four groups. They include methyl esters (the main biodiesel components), oxygenated chemicals, alkanes and alkenes, and aromatics. The first two chemical groups are only found in biodiesel vapors, not in the diesel vapor emissions. The percentages of mean concentrations for methyl esters, oxygenated chemicals, alkanes and alkenes, and aromatics are 66.1%, 22.8%, 4.8% and 6.4%, respectively for soy biodiesel, and 35.8%, 35.9%, 27.9% and 0.3%, respectively for waste cooking oil biodiesel at a temperature of 25+/-2 degrees C. These results show that biodiesels have fewer chemicals and lower concentrations in vapor phase than petroleum diesel, and the total emission rates are between one-sixteenth and one-sixth of that of diesel emission, corresponding to fuel evaporative emissions of loading losses of between 106 microg l(-1) and 283 microg l(-1). Although diesels generate more vapor phase emissions, biodiesels still generate considerable amount of vapor emissions, particularly the emissions from methyl esters and oxygenated chemicals. These two chemical groups are more reactive than alkanes and aromatics. Therefore, speciation and quantification of biodiesel vapor phases are important. PMID:16904162

  16. Disposal of liquid radioactive wastes through wells or shafts

    SciTech Connect

    Perkins, B.L.

    1982-01-01

    This report describes disposal of liquids and, in some cases, suitable solids and/or entrapped gases, through: (1) well injection into deep permeable strata, bounded by impermeable layers; (2) grout injection into an impermeable host rock, forming fractures in which the waste solidifies; and (3) slurrying into excavated subsurface cavities. Radioactive materials are presently being disposed of worldwide using all three techniques. However, it would appear that if the techniques were verified as posing minimum hazards to the environment and suitable site-specific host rock were identified, these disposal techniques could be more widely used.

  17. Disposal of liquid radioactive wastes through wells or shafts

    NASA Astrophysics Data System (ADS)

    Perkins, B. L.

    1982-01-01

    Liquids and, in some cases, suitable solids and/or entrapped gases can be disposed of by: (1) well injection into deep permeable strata, bounded by impermeable layers; (2) grout injection into an impermeable host rock, forming fractures in which the waste solidifies; and (3) slurrying into excavated subsurface cavities. Radioactive materials are presently being disposed of worldwide using all three techniques; however, it would appear that if the techniques were verified as posing minimum hazards to the environment and suitable site-specific host rock were identified, these disposal techniques could be more widely used.

  18. Optimization of a packed bed reactor for liquid waste treatment

    SciTech Connect

    Schmidt, C.A.; Brower, M.J.; Coogan, J.J.; Tennant, R.A.

    1993-11-01

    The authors describe an optimization study of a packed bed reactor (PBR), developed for the treatment of hazardous liquid wastes. The focus is on the destruction of trichloroethylene (TCE). The PBR technology offers many distinct advantages over other processes: simple design, high destruction rates (99.99%), low costs, ambient pressure operation, easy maintenance and scaleability. The cost effectiveness, optimal operating parameters and scaleability were determined. As a second stage of treatment, a silent discharge plasma (SDP) reactor was installed to further treat offgases from the PBR. A primary advantage of this system is closed loop operation, where exhaust gases are continuously recycled and not released into the atmosphere.

  19. Quantification of free formaldehyde in carrageenan and processed Eucheuma seaweed using high-performance liquid chromatography.

    PubMed

    Hornshøj, Bettina Høj; Kobbelgaard, Sara; Blakemore, William R; Stapelfeldt, Henrik; Bixler, Harris J; Klinger, Markus

    2015-01-01

    In 2010 the European Commission placed a limit on the amount of free formaldehyde in carrageenan and processed Eucheuma seaweed (PES) of 5 mg kg(-1). Formaldehyde is not used in carrageenan and PES processing and accordingly one would not expect free formaldehyde to be present in carrageenan and PES. However, surprisingly high levels up to 10 mg kg(-1) have been found using the generally accepted AOAC and Hach tests. These findings are, per proposed reaction pathways, likely due to the formation of formaldehyde when sulphated galactose, the backbone of carrageenan, is hydrolysed with the strong acid used in these conventional tests. In order to minimise the risk of false-positives, which may lead to regulatory non-compliance, a new high-performance liquid chromatography (HPLC) method has been developed. Initially, carrageenan or PES is extracted with 2-propanol and subsequently reacted with 2,4-dinitrophenylhydrazine (DNPH) to form the chromophore formaldehyde-DNPH, which is finally quantified by reversed-phase HPLC with ultraviolet light detection at 355 nm. This method has been found to have a limit of detection of 0.05 mg kg(-1) and a limit of quantification of 0.2 mg kg(-1). Recoveries from samples spiked with known quantities of formaldehyde were 95-107%. Using this more specific technique, 20 samples of carrageenan and PES were tested for formaldehyde. Only one sample had a detectable content of formaldehyde (0.40 mg kg(-1)), thus demonstrating that the formaldehyde content of commercial carrageenan and PES products are well below the European Commission maximum limit of 5 mg kg(-1). PMID:25531040

  20. Simultaneous quantification of 21 water soluble vitamin circulating forms in human plasma by liquid chromatography-mass spectrometry.

    PubMed

    Meisser Redeuil, Karine; Longet, Karin; Bénet, Sylvie; Munari, Caroline; Campos-Giménez, Esther

    2015-11-27

    This manuscript reports a validated analytical approach for the quantification of 21 water soluble vitamins and their main circulating forms in human plasma. Isotope dilution-based sample preparation consisted of protein precipitation using acidic methanol enriched with stable isotope labelled internal standards. Separation was achieved by reversed-phase liquid chromatography and detection performed by tandem mass spectrometry in positive electrospray ionization mode. Instrumental lower limits of detection and quantification reached <0.1-10nM and 0.2-25nM, respectively. Commercially available pooled human plasma was used to build matrix-matched calibration curves ranging 2-500, 5-1250, 20-5000 or 150-37500nM depending on the analyte. The overall performance of the method was considered adequate, with 2.8-20.9% and 5.2-20.0% intra and inter-day precision, respectively and averaged accuracy reaching 91-108%. Recovery experiments were also performed and reached in average 82%. This analytical approach was then applied for the quantification of circulating water soluble vitamins in human plasma single donor samples. The present report provides a sensitive and reliable approach for the quantification of water soluble vitamins and main circulating forms in human plasma. In the future, the application of this analytical approach will give more confidence to provide a comprehensive assessment of water soluble vitamins nutritional status and bioavailability studies in humans. PMID:26522745

  1. Highly sensitive quantification of pyrethroid insecticide etofenprox in vegetables with high-performance liquid chromatography and fluorescence detection.

    PubMed

    Watanabe, Eiki; Baba, Koji

    2015-03-13

    This paper describes a highly sensitive analytical method using high-performance liquid chromatography and fluorescence detection (HPLC-FLD) capable of quantifying trace amounts of synthetic pyrethroid insecticide etofenprox residue in six vegetable samples: bell pepper, cucumber, eggplant, Japanese mustard spinach, spinach, and tomato. After extraction with acetonitrile, the crude sample extract was cleaned up with a solid-phase extraction cartridge. The matrix interference derived from the tested vegetable samples was evaluated. Quantification was conducted using external calibrators prepared in pure acetonitrile. The limits of quantification for etofenprox in each sample were 1.87-3.87 ng/g. Recoveries obtained by application of the proposed analytical method of vegetable samples spiked at the considerably low levels (5-100 ng/g) were 85-111% with relative standard deviations of less than 12%. The proposed method using the HPLC-FLD was applied for trace analysis of the insecticide residue in vegetable samples. PMID:25662063

  2. Real-time alpha monitoring of a radioactive liquid waste stream at Los Alamos National Laboratory

    SciTech Connect

    Johnson, J.D.; Whitley, C.R.; Rawool-Sullivan, M.

    1995-12-31

    This poster display concerns the development, installation, and testing of a real-time radioactive liquid waste monitor at Los Alamos National Laboratory (LANL). The detector system was designed for the LANL Radioactive Liquid Waste Treatment Facility so that influent to the plant could be monitored in real time. By knowing the activity of the influent, plant operators can better monitor treatment, better segregate waste (potentially), and monitor the regulatory compliance of users of the LANL Radioactive Liquid Waste Collection System. The detector system uses long-range alpha detection technology, which is a nonintrusive method of characterization that determines alpha activity on the liquid surface by measuring the ionization of ambient air. Extensive testing has been performed to ensure long-term use with a minimal amount of maintenance. The final design was a simple cost-effective alpha monitor that could be modified for monitoring influent waste streams at various points in the LANL Radioactive Liquid Waste Collection System.

  3. Innovative Process for Comprehensive Treatment of Liquid Radioactive Waste - 12551

    SciTech Connect

    Penzin, R.A.; Sarychev, G.A.

    2012-07-01

    the necessity to take emergency measures and to use marine water for cooling of reactor zone in contravention of the technological regulations. In these cases significant amount of liquid radioactive wastes of complex physicochemical composition is being generated, the purification of which by traditional methods is close to impossible. According to the practice of elimination of the accident after-effects at NPP 'Fukushima' there are still no technical means for the efficient purification of liquid radioactive wastes of complex composition like marine water from radionuclides. Therefore development of state-of-the-art highly efficient facilities capable of fast and safe purification of big amounts of liquid radioactive wastes of complex physicochemical composition from radionuclides turns to be utterly topical problem. Cesium radionuclides, being extremely dangerous for the environment, present over 90% of total radioactivity contained in liquid radioactive wastes left as a result of accidents at nuclear power objects. For the purpose of radiation accidents aftereffects liquidation VNIIHT proposes to create a plant for LRW reprocessing, consisting of 4 major technological modules: Module of LRW pretreatment to remove mechanical and organic impurities including oil products; Module of sorption purification of LWR by means of selective inorganic sorbents; Module of reverse osmotic purification and desalination; Module of deep evaporation of LRW concentrates. The first free modules are based on completed technological and designing concepts implemented by VNIIHT in the framework of LLRW Project in the period of 2000-2001 in Russia for comprehensive treatment of LWR of atomic fleet. These industrial plants proved to be highly efficient and secure during their long operation life. Module of deep evaporation is a new technological development. It will ensure conduction of evaporation and purification of LRW of different physicochemical composition, including those

  4. Incineration of radioactive organic liquid wastes by underwater thermal plasma

    NASA Astrophysics Data System (ADS)

    Mabrouk, M.; Lemont, F.; Baronnet, J. M.

    2012-12-01

    This work deals with incineration of radioactive organic liquid wastes using an oxygen thermal plasma jet, submerged under water. The results presented here are focused on incineration of three different wastes: a mixture of tributylphosphate (TBP) and dodecane, a perfluoropolyether oil (PFPE) and trichloroethylene (TCE). To evaluate the plutonium behavior in used TBP/dodecane incineration, zirconium is used as a surrogate of plutonium; the method to enrich TBP/dodecane mixture in zirconium is detailed. Experimental set-up is described. During a trial run, CO2 and CO contents in the exhaust gas are continuously measured; samples, periodically taken from the solution, are analyzed by appropriate chemical methods: contents in total organic carbon (COT), phosphorus, fluoride and nitrates are measured. Condensed residues are characterized by RX diffraction and SEM with EDS. Process efficiency, during tests with a few L/h of separated or mixed wastes, is given by mineralization rate which is better than 99.9 % for feed rate up to 4 L/h. Trapping rate is also better than 99 % for phosphorous as for fluorine and chlorine. Those trials, with long duration, have shown that there is no corrosion problems, also the hydrogen chloride and fluoride have been neutralized by an aqueous solution of potassium carbonate.

  5. Hydrophilic interaction liquid chromatography for the separation, purification, and quantification of raffinose family oligosaccharides from Lycopus lucidus Turcz.

    PubMed

    Liang, Tu; Fu, Qing; Li, Fangbing; Zhou, Wei; Xin, Huaxia; Wang, Hui; Jin, Yu; Liang, Xinmiao

    2015-08-01

    A systematic strategy based on hydrophilic interaction liquid chromatography was developed for the separation, purification and quantification of raffinose family oligosaccharides from Lycopus lucidus Turcz. Methods with enough hydrophilicity and selectivity were utilized to resolve the problems encountered in the separation of oligosaccharides such as low retention, low resolution and poor solubility. The raffinose family oligosaccharides in L. lucidus Turcz. were isolated using solid-phase extraction followed by hydrophilic interaction liquid chromatography at semi-preparative scale to obtain standards of stachyose, verbascose and ajugose. Utilizing the obtained oligosaccharides as standards, a quantitative determination method was developed, validated and applied for the content determination of raffinose family oligosaccharides both in the aerial and root parts of L. lucidus Turcz. There were no oligosaccharides in the aerial parts, while in the root parts, the total content was 686.5 mg/g with the average distribution: raffinose 66.5 mg/g, stachyose 289.0 mg/g, verbascose 212.4 mg/g, and ajugose 118.6 mg/g. The result provided the potential of roots of L. lucidus Turcz. as new raffinose family oligosaccharides sources for functional food. Moreover, since the present systematic strategy is efficient, sensitive and robust, separation, purification and quantification of oligosaccharides by hydrophilic interaction liquid chromatography seems to be possible. PMID:26011699

  6. Properties required by extractants and diluents for the decontamination of liquid wastes using supported liquid membranes

    SciTech Connect

    Dozol, J.F.; Rouquette, H.; Eymard, S.; Tournois, B.

    1993-12-31

    Macrocyclic extractants are now being studied more and more often for the decontamination of radioactive liquid wastes: coronands (crown ethers, azacrown...) and cryptands. As these very sophisticated compounds are expensive, the best technique is supported liquid membranes which need a very low extractant inventory. This paper deals with the properties required by the extractant and the diluent in order to be used in an SLM device and to ensure a stable and efficient SLM: solubility of the extractant in organic compounds and in aqueous solutions; size of crown ether cavities; influence of the substituent groups on the selectivity of the crown ether; and influence of the properties of the diluent (polarity, transport of acidity) on the efficiency of the process and on the stability of the membrane (interfacial tension between the organic and aqueous phases, solubility in the aqueous phase). The influence of these parameters is illustrated by experiments performed in order to remove strontium and cesium from high sodium content liquid waste. The studies described in this paper are focused on the decategorization of evaporator concentrates arising from the reprocessing of spent fuel.

  7. Quantification of Galactose-1-Phosphate Uridyltransferase Enzyme Activity by Liquid Chromatography–Tandem Mass Spectrometry

    PubMed Central

    Li, Yijun; Ptolemy, Adam S.; Harmonay, Lauren; Kellogg, Mark; Berry, Gerard T.

    2013-01-01

    Background The diagnosis of galactosemia usually involves the measurement of galactose-1-phosphate uridyltransferase (GALT) activity. Traditional radioactive and fluorescent GALT assays are nonspecific, laborious, and/or lack sufficient analytical sensitivity. We developed a liquid chromatography–tandem mass spectrometry (LC-MS/MS)–based assay for GALT enzyme activity measurement. Method Our assay used stable isotope-labeled α-galactose-1-phosphate ([13C6]-Gal-1-P) as an enzyme substrate. Sample cleanup and separation were achieved by reversed-phase ion-pair chromatography, and the enzymatic product, isotope-labeled uridine diphosphate galactose ([13C6]-UDPGal), was detected by MS/MS at mass transition (571 > 323) and quantified by use of [13C6]-Glu-1-P (265 > 79) as an internal standard. Results The method yielded a mean (SD) GALT enzyme activity of 23.8 (3.8) µmol · (gHgb)−1 · h−1 in erythrocyte extracts from 71 controls. The limit of quantification was 0.04 µmol · (g Hgb)−1 · h−1 (0.2% of normal control value). Intraassay imprecision was determined at 4 different levels (100%, 25%, 5%, and 0.2% of the normal control values), and the CVs were calculated to be 2.1%, 2.5%, 4.6%, and 9.7%, respectively (n = 3). Interassay imprecision CVs were 4.5%, 6.7%, 8.2%, and 13.2% (n = 5), respectively. The assay recoveries at the 4 levels were higher than 90%. The apparent Km of the 2 substrates, Gal-1-P and UDPGlc, were determined to be 0.38 mmol/L and 0.071 mmol/L, respectively. The assay in erythrocytes of 33 patients with classical galactosemia revealed no detectable activity. Conclusions This LC-MS/MS–based assay for GALT enzyme activity will be useful for the diagnosis and study of biochemically heterogeneous patients with galactosemia, especially those with uncommon genotypes and detectable but low residual activities. PMID:20348403

  8. A&M. Hot liquid waste holding tanks. Camera faces southeast. Located ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    A&M. Hot liquid waste holding tanks. Camera faces southeast. Located in vicinity of TAN-616, hot liquid waste treatment plant. Date: November 13, 1953. INEEL negative no. 9159 - Idaho National Engineering Laboratory, Test Area North, Scoville, Butte County, ID

  9. FORMATION OF TRANSIENT PUFFS FROM CONTAINED LIQUID WASTES IN A ROTARY KILN SIMULATOR

    EPA Science Inventory

    The paper gives results of a study of the generation of transient puffs resulting from the batch incineration of liquid waste into a 73 kW rotary kiln incinerator simulator. Liquid wastes investigated included toluene, methylene chloride, carbon tetrachloride, and No. 5 fuel oil....

  10. Non radiological issues in the treatment of low-level liquid wastes

    SciTech Connect

    Welbergen, Jeroen; Verhoef, Ewoud; Eijke, Anton; Best, Alex de; Hengst, Jan; Codee, Hans

    2007-07-01

    Available in abstract form only. Full text of publication follows: In the Netherlands there are some 200 producers of radioactive waste. Most of them generate only small volumes of low and medium level waste. These small volumes however cover a wide range of waste forms: solids, liquids of all nature, slurries, etc. Because of the resulting wide spectrum of radiological and chemical contaminations, a certain amount of flexibility is required in both solid and liquid waste treatment. In addition, the Nuclear Energy Act license requires a five yearly evaluation of the waste processing installation with respect to the Best Practicable Technologies. The bulk of the solid waste are compacted, conditioned as cemented packages and stored for at least hundred years. The low-level liquid waste is treated batch-wise as the volumes of liquid waste are too small to operate a continuous system. Moreover, batch-wise processing enables more flexibility. Discharge of treated water is bounded by concentration limits of chemicals and total activity per nuclide. Evaluation of the installation showed that the radiological constraints provide a larger degree of freedom to discharge, and the waste water treatment can effectively meet the required limits. The limits of concentration of chemicals are more restrictive. The liquid waste often has more chemical contamination than radiological. This paper describes the evaluation of the waste water treatment. (authors)

  11. Remediation of Hanford's N-Reactor Liquid Waste Disposal Sites.

    PubMed

    Sitsler, Robert B.; DeMers, Steven K.

    2003-02-01

    Hanford's N-Reactor operated from 1963 to 1987 generating approximately 9 x 10 m of radioactive and hazardous liquid effluent as a result of reactor operations. Two liquid waste disposal sites, essentially large trenches designed to filter contaminants from the water as it percolates through the soil column, were established to dispose of the effluent. The discharges to the sites included cooling water from the reactor primary, spent fuel storage, and periphery systems, along with miscellaneous drainage from reactor support facilities. Today, both sites are classified as Treatment Storage and Disposal Facilities under the Resource Conservation and Recovery Act of 1976, which makes them priority sites for remediation. The two sites cover approximately 4,100 m and 9,300 m, respectively. Remediation of the sites requires removing a combined total of approximately 2.6 x 10 kg of contaminated soil and debris. Principal radionuclides contained in the soil/debris are Co, Cs, Pu, and Sr. Remediation of these waste sites requires demolishing concrete structures and excavating, hauling, and disposing of contaminated soils in work areas containing high levels of contamination and whole body dose rates in excess of 1 mSv h. The work presents unique radiological control challenges, such as minimizing external dose to workers in a constantly changing outdoor work environment, maintaining contamination control during removal of a water distribution trough filled with highly contaminated sludge, and minimizing outdoor airborne contamination during size reduction of highly contaminated pipelines. Through innovative approaches to dose reduction and contamination control, Hanford's Environmental Restoration Contractor has met the challenge, completing the first phase on schedule and with a total project exposure below the goal of 0.1 person-Sv. PMID:12555036

  12. 324 Building liquid waste handling and removal system project plan

    SciTech Connect

    Ham, J.E.

    1998-07-29

    This report evaluates the modification options for handling radiological liquid waste generated during decontamination and cleanout of the 324 Building. Recent discussions indicate that the Hanford site railroad system will be closed by the end of FY 1998 necessitating the need for an alternate transfer method. The issue of handling of Radioactive Liquid Waste (RLW) from the 324 Building (assuming the 340 Facility is not available to accept the RLW) has been examined in at least two earlier engineering studies (Parsons 1997a and Hobart 1997). Each study identified a similar preferred alternative that included modifying the 324 Building RLWS to allow load-out of wastewater to a truck tanker, while making maximum use of existing piping, tanks, instrumentation, controls and other features to minimize costs and physical changes to the building. This alternative is accepted as the basis for further discussion presented in this study. The goal of this engineering study is to verify the path forward presented in the previous studies and assure that the selected alternative satisfies the 324 Building deactivation goals and objectives as currently described in the project management plan. This study will also evaluate options available to implement the preferred alternative and select the preferred option for implementation of the entire system. Items requiring further examination will also be identified. Finally, the study will provide a conceptual design, schedule and cost estimate for the required modifications to the 324 Building to allow removal of RLW. Attachment 5 is an excerpt from the project baseline schedule found in the Project Management Plan.

  13. Remediation of Hanford's N-reactor liquid waste disposal sites.

    PubMed

    Sitsler, Robert B; DeMers, Steven K

    2003-02-01

    Hanford's N-Reactor operated from 1963 to 1987 generating approximately 9 x 10(7) m3 of radioactive and hazardous liquid effluent as a result of reactor operations. Two liquid waste disposal sites, essentially large trenches designed to filter contaminants from the water as it percolates through the soil column, were established to dispose of the effluent. The discharges to the sites included cooling water from the reactor primary, spent fuel storage, and periphery systems, along with miscellaneous drainage from reactor support facilities. Today, both sites are classified as Treatment Storage and Disposal Facilities under the Resource Conservation and Recovery Act of 1976, which makes them priority sites for remediation. The two sites cover approximately 4,100 m2 and 9,300 m2, respectively. Remediation of the sites requires removing a combined total of approximately 2.6 x 10(8) kg of contaminated soil and debris. Principal radionuclides contained in the soil/debris are 60Co, 137Cs, 239Pu, and 90Sr. Remediation of these waste sites requires demolishing concrete structures and excavating, hauling, and disposing of contaminated soils in work areas containing high levels of contamination and whole body dose rates in excess of 1 mSv h-1. The work presents unique radiological control challenges, such as minimizing external dose to workers in a constantly changing outdoor work environment, maintaining contamination control during removal of a water distribution trough filled with highly contaminated sludge, and minimizing outdoor airborne contamination during size reduction of highly contaminated pipelines. Through innovative approaches to dose reduction and contamination control, Hanford's Environmental Restoration Contractor has met the challenge, completing the first phase on schedule and with a total project exposure below the goal of 0.1 person-Sv. PMID:12564346

  14. MECHANISMS GOVERNING TRANSIENTS FROM THE BATCH INCINERATION OF LIQUID WASTES IN ROTARY KILNS

    EPA Science Inventory

    When "containerized" liquid wastes, bound on sorbents. are introduced into a rotary kiln in a batch mode, transient phenomena in-volving heat transfer into, and waste mass transfer out of, the sorbent can oromote the raoid release of waste vaoor into the kiln environment. This ra...

  15. ISOLATION OF METALS FROM LIQUID WASTES: REACTIVE SCAVENGING IN TURBULENT THERMAL REACTORS

    EPA Science Inventory

    Metal-bearing liquids constitute a major part of the DOE waste inventory. This waste is extremely varied with respect to metals (radionuclides, heavy metals, transuranics) and other species (e.g., organics). For much of this waste, concentration of metals to reduce the volume req...

  16. Quantification of voriconazole in human bronchoalveolar lavage fluid using high-performance liquid chromatography with fluorescence detection.

    PubMed

    Heng, S C; Nation, R L; Levvey, B; Snell, G I; Slavin, M A; Kong, D C M

    2013-01-15

    The quantification of voriconazole concentration in lung epithelial lining fluid to facilitate the management of pulmonary fungal colonisation or aspergillosis is of increasing interest. An accurate and reproducible high-performance liquid chromatography method to quantify voriconazole in human bronchoalveolar lavage (BAL) fluid was developed and validated. BAL samples were concentrated by freeze-drying and reconstituted with water prior to deproteinisation. Separation was achieved with a C18 column employing fluorescence detection (excitation: 260nm, emission: 370nm). The calibration curves were linear from 2.5 to 500ng/mL. The intra- and inter-day precisions were within 7%. Accuracies ranged from 102% to 107%. The clinical applicability was established by successful measurement of voriconazole concentrations in lung transplant recipients. The assay provides an alternative approach for those with negligible access to liquid chromatography-tandem mass spectrometry instrumentation. PMID:23314356

  17. Packed bed reactor treatment of liquid hazardous and mixed wastes

    SciTech Connect

    Tennant, R.A.; Wantuck, P.J.; Vargas, R.

    1992-01-01

    We are developing thermal-based packed bed reactor (PBR) technology as an alternative to incineration for treatment of hazardous organic liquid wastes. The waste streams targeted by this technology are machining fluids contaminated with chlorocarbons and/or chlorofluorocarbons and low levels of plutonium or tritium The PBR offers several distinct advantages including simplistic design, rugged construction, ambient pressure processing, economical operations, as well as ease of scalability and maintainability. In this paper, we provide a description of the apparatus as well as test results using prepared mixtures of machining oils/emulsions with trichloroethylene (TCE), carbon tetrachloride (CCl{sub 4}), trichloroethane (TCA), and Freon TF. The current treatment system is configured as a two stage device with the PBR (1st stage) coupled to a silent discharge plasma (SDP) cell. The SDP serves as a second stage for further treatment of the gaseous effluent from the PBR. One of the primary advantages of this two stage system is that its suitability for closed loop operation where radioactive components are well contained and even CO{sub 2} is not released to the environment.

  18. Packed bed reactor treatment of liquid hazardous and mixed wastes

    SciTech Connect

    Tennant, R.A.; Wantuck, P.J.; Vargas, R.

    1992-05-01

    We are developing thermal-based packed bed reactor (PBR) technology as an alternative to incineration for treatment of hazardous organic liquid wastes. The waste streams targeted by this technology are machining fluids contaminated with chlorocarbons and/or chlorofluorocarbons and low levels of plutonium or tritium The PBR offers several distinct advantages including simplistic design, rugged construction, ambient pressure processing, economical operations, as well as ease of scalability and maintainability. In this paper, we provide a description of the apparatus as well as test results using prepared mixtures of machining oils/emulsions with trichloroethylene (TCE), carbon tetrachloride (CCl{sub 4}), trichloroethane (TCA), and Freon TF. The current treatment system is configured as a two stage device with the PBR (1st stage) coupled to a silent discharge plasma (SDP) cell. The SDP serves as a second stage for further treatment of the gaseous effluent from the PBR. One of the primary advantages of this two stage system is that its suitability for closed loop operation where radioactive components are well contained and even CO{sub 2} is not released to the environment.

  19. Low-level liquid waste decontamination by ion exchange

    SciTech Connect

    Campbell, D.O.; Lee, D.D.; Dillow, T.A.

    1991-12-01

    Improved processes are being developed to treat contaminated liquid wastes that have been and continue to be generated at Oak Ridge National Laboratory. Both inorganic and organic ion-exchange methods have given promising results. Nickel and cobalt hexacyanoferrate(2) compounds are extremely selective for cesium removal, with distribution coefficients in excess of 10{sup 6} and remarkable insensitivity to competition from sodium and potassium. They tend to lose effectiveness at pH > {approximately}11, but some formulations are useful for limited periods of time up to pH {approximately}13. Sodium titanate is selective for strontium removal at high pH. The separations are so efficient that simple batch processes can yield large decontamination factors while generating small volumes of solid waste. A resorcinol-based resin developed at the Savannah River Site gave superior cesium removal, compared with other organic ion exchangers; the distribution coefficient was limited primarily by competition from potassium and was nearly independent of sodium. The optimum pH was {approximately}12.5. It was much less effective for strontium removal, which was limited by competition from sodium. 8 refs., 6 figs., 9 tabs.

  20. CONTINUOUS MICRO-SORTING OF COMPLEX WASTE PLASTICS PARTICLEMIXTURES VIA LIQUID-FLUIDIZED BED CLASSIFICATION (LFBC) FOR WASTE MINIMIZATIONAND RECYCLING

    EPA Science Inventory

    A fundamental investigation is proposed to provide a technical basis for the development of a novel, liquid-fluidized bed classification (LFBC) technology for the continuous separation of complex waste plastic mixtures for in-process recycling and waste minimization. Although ...

  1. Baseline-Corrected Second-Order Derivative Electroanalysis Combined With Ultrasound-Assisted Liquid-Liquid Microextraction: Simultaneous Quantification of Fluoroquinolones at Low Levels.

    PubMed

    de Oliveira, Luiz Henrique; Trindade, Magno Aparecido Gonçalves

    2016-06-21

    A baseline-corrected second-order derivative procedure and a miniaturized sample preparation based on low-density solvent and ultrasound-assisted liquid-liquid microextraction (LDS-UA-LLME) was combined to provide the simultaneous electroanalysis of three fluoroquinolones (FQ) as emerging contaminants (ECs). The enhanced mathematical processing provided the best separation with an accurate measurement of the overlapping peaks during the simultaneous electro-oxidation of target FQs that were directly dropped on the surface of carbon nanofiber-modified screen-printed electrodes. The adapted LDS-UA-LLME protocol was the key step involved in the sample preparation, which preconcentrate target analytes from diluted tap water samples with an enrichment factor of around 80×, allowing their quantification at trace levels. This combined feature demonstrated the unique application of an electroanalytical technique for the simultaneous electroanalysis of three FQs in spiked tap water samples, with recovery values remarkably close to 100%. PMID:27249314

  2. Value added liquid products from waste biomass pyrolysis using pretreatments.

    PubMed

    Das, Oisik; Sarmah, Ajit K

    2015-12-15

    Douglas fir wood, a forestry waste, was attempted to be converted into value added products by pretreatments followed by pyrolysis. Four different types of pretreatments were employed, namely, hot water treatment, torrefaction, sulphuric acid and ammonium phosphate doping. Subsequently, pyrolysis was done at 500°C and the resulting bio-oils were analysed for their chemical composition using Karl Fischer titration, thermogravimetry, ion exchange, and gas chromatography. Pretreatment with acid resulted in the highest yield of bio-oil (~60%). The acid and salt pretreatments were responsible for drastic reduction in the lignin oligomers and enhancement of water content in the pyrolytic liquid. The quantity of xylose/mannose reduced as a result of pretreatments. Although, the content of fermentable sugars remained similar across all the pretreatments, the yield of levoglucosan increased. Pretreatment of the biomass with acid yielded the highest amount of levoglucosan in the bio-oil (13.21%). The acid and salt pretreatments also elevated the amount of acetic acid in the bio-oils. Addition of acid and salt to the biomass altered the interaction of cellulose-lignin in the pyrolysis regime. Application of pretreatments should be based on the intended end use of the liquid product having a desired chemical composition. PMID:26298257

  3. Solid Waste Composition and Quantification at Taman Melewar, Parit Raja, Batu Pahat

    NASA Astrophysics Data System (ADS)

    Kadir, A. A.; Abidin, S. S. S. Z.

    2016-07-01

    The poor management of solid waste is noticeable through the increasing of the solid waste each year and the difficulties in disposing the waste in the current available landfill. This study was undertaken to analyze the quantity and composition of waste generation in Taman melewar. Taman Melewar is a student residential area and this study is focusing on student's daily waste composition. The objective of this study was to identify the amount of solid waste generation, analyze and classify the composition of solid waste in Taman Melewar. The waste collection was conducted for 50 houses on a daily basis for two weeks. The average household waste generation rate was 0.082 kg/person/day. Organic waste was the major constituent of waste production. The average of organic waste represents about 72.4% followed by paper (9%), plastics film (5.5%), plastics rigid (4.7%), napkins (3.8%), tetrapek (1.3%), glass (1.1%), household hazardous waste (0.85%), textiles (0.52%), metal (0.51%) and rubber (0.34%). The moisture content was ranging from 27.67% to 28.68%. An evaluation was made based on student's behavior towards waste production and recycling. In conclusion, the results revealed that organic waste is the highest waste generated and recycling habits is also poor in Taman Melewar.

  4. Recovery of valuable materials from waste liquid crystal display panel

    SciTech Connect

    Li Jinhui Gao Song; Duan Huabo; Liu Lili

    2009-07-15

    Associated with the rapid development of the information and electronic industry, liquid crystal displays (LCDs) have been increasingly sold as displays. However, during the discarding at their end-of-life stage, significant environmental hazards, impacts on health and a loss of resources may occur, if the scraps are not managed in an appropriate way. In order to improve the efficiency of the recovery of valuable materials from waste LCDs panel in an environmentally sound manner, this study presents a combined recycling technology process on the basis of manual dismantling and chemical treatment of LCDs. Three key processes of this technology have been studied, including the separation of LCD polarizing film by thermal shock method the removal of liquid crystals between the glass substrates by the ultrasonic cleaning, and the recovery of indium metal from glass by dissolution. The results show that valuable materials (e.g. indium) and harmful substances (e.g. liquid crystals) could be efficiently recovered or separated through above-mentioned combined technology. The optimal conditions are: (1) the peak temperature of thermal shock to separate polarizing film, ranges from 230 to 240 deg. C, where pyrolysis could be avoided; (2) the ultrasonic-assisted cleaning was most efficient at a frequency of 40 KHz (P = 40 W) and the exposure of the substrate to industrial detergents for 10 min; and (3) indium separation from glass in a mix of concentrated hydrochloric acid at 38% and nitric acid at 69% (HCl:HNO{sub 3}:H{sub 2}O = 45:5:50, volume ratio). The indium separation process was conducted with an exposure time of 30 min at a constant temperature of 60 deg. C.

  5. Identification and absolute quantification of enzymes in laundry detergents by liquid chromatography tandem mass spectrometry.

    PubMed

    Gaubert, Alexandra; Jeudy, Jérémy; Rougemont, Blandine; Bordes, Claire; Lemoine, Jérôme; Casabianca, Hervé; Salvador, Arnaud

    2016-07-01

    In a stricter legislative context, greener detergent formulations are developed. In this way, synthetic surfactants are frequently replaced by bio-sourced surfactants and/or used at lower concentrations in combination with enzymes. In this paper, a LC-MS/MS method was developed for the identification and quantification of enzymes in laundry detergents. Prior to the LC-MS/MS analyses, a specific sample preparation protocol was developed due to matrix complexity (high surfactant percentages). Then for each enzyme family mainly used in detergent formulations (protease, amylase, cellulase, and lipase), specific peptides were identified on a high resolution platform. A LC-MS/MS method was then developed in selected reaction monitoring (SRM) MS mode for the light and corresponding heavy peptides. The method was linear on the peptide concentration ranges 25-1000 ng/mL for protease, lipase, and cellulase; 50-1000 ng/mL for amylase; and 5-1000 ng/mL for cellulase in both water and laundry detergent matrices. The application of the developed analytical strategy to real commercial laundry detergents enabled enzyme identification and absolute quantification. For the first time, identification and absolute quantification of enzymes in laundry detergent was realized by LC-MS/MS in a single run. Graphical Abstract Identification and quantification of enzymes by LC-MS/MS. PMID:27098933

  6. Review of Potential Candidate Stabilization Technologies for Liquid and Solid Secondary Waste Streams

    SciTech Connect

    Pierce, Eric M.; Mattigod, Shas V.; Westsik, Joseph H.; Serne, R. Jeffrey; Icenhower, Jonathan P.; Scheele, Randall D.; Um, Wooyong; Qafoku, Nikolla

    2010-01-30

    Pacific Northwest National Laboratory has initiated a waste form testing program to support the long-term durability evaluation of a waste form for secondary wastes generated from the treatment and immobilization of Hanford radioactive tank wastes. The purpose of the work discussed in this report is to identify candidate stabilization technologies and getters that have the potential to successfully treat the secondary waste stream liquid effluent, mainly from off-gas scrubbers and spent solids, produced by the Hanford Tank Waste Treatment and Immobilization Plant (WTP). Down-selection to the most promising stabilization processes/waste forms is needed to support the design of a solidification treatment unit (STU) to be added to the Effluent Treatment Facility (ETF). To support key decision processes, an initial screening of the secondary liquid waste forms must be completed by February 2010.

  7. A sensitive high performance liquid chromatography assay for the quantification of doxorubicin associated with DNA in tumor and tissues.

    PubMed

    Lucas, Andrew T; O'Neal, Sara K; Santos, Charlene M; White, Taylor F; Zamboni, William C

    2016-02-01

    Doxorubicin, a widely used anticancer agent, exhibits antitumor activity against a wide variety of malignancies. The drug exerts its cytotoxic effects by binding to and intercalating within the DNA of tumor and tissue cells. However, current assays are unable to accurately determine the concentration of the intracellular active form of doxorubicin. Thus, the development of a sample processing method and a high-performance liquid chromatography (HPLC) methodology was performed in order to quantify doxorubicin that is associated with DNA in tumors and tissues, which provided an intracellular cytotoxic measure of doxorubicin exposure after administration of small molecule and nanoparticle formulations of doxorubicin. The assay uses daunorubicin as an internal standard; liquid-liquid phase extraction to isolate drug associated with DNA; a Shimadzu HPLC with fluorescence detection equipped with a Phenomenex Luna C18 (2μm, 2.0×100mm) analytical column and a gradient mobile phase of 0.1% formic acid in water or acetonitrile for separation and quantification. The assay has a lower limit of detection (LLOQ) of 10ng/mL and is shown to be linear up to 3000ng/mL. The intra- and inter-day precision of the assay expressed as a coefficient of variation (CV%) ranged from 4.01 to 8.81%. Furthermore, the suitability of this assay for measuring doxorubicin associated with DNA in vivo was demonstrated by using it to quantify the doxorubicin concentration within tumor samples from SKOV3 and HEC1A mice obtained 72h after administration of PEGylated liposomal doxorubicin (Doxil(®); PLD) at 6mg/kg IV x 1. This HPLC assay allows for sensitive intracellular quantification of doxorubicin and will be an important tool for future studies evaluating intracellular pharmacokinetics of doxorubicin and various nanoparticle formulations of doxorubicin. PMID:26678179

  8. ICPP radioactive liquid and calcine waste technologies evaluation final report and recommendation

    SciTech Connect

    1995-04-01

    Using a formalized Systems Engineering approach, the Latched Idaho Technologies Company developed and evaluated numerous alternatives for treating, immobilizing, and disposing of radioactive liquid and calcine wastes at the Idaho Chemical Processing Plant. Based on technical analysis data as of March, 1995, it is recommended that the Department of Energy consider a phased processing approach -- utilizing Radionuclide Partitioning for radioactive liquid and calcine waste treatment, FUETAP Grout for low-activity waste immobilization, and Glass (Vitrification) for high-activity waste immobilization -- as the preferred treatment and immobilization alternative.

  9. Reduction of Sodium Nitrate Liquid Waste in Nuclear Reprocessing Plants

    SciTech Connect

    Numata, M.; Mihara, S.; Kojima, S.; Ito, H.; Kato, T.

    2006-07-01

    Sodium nitrate solution has been generated from nuclear reprocessing plant as a result of neutralization of nitric acid. The sodium nitrate has been immobilized by bitumen, cement or other material in the site and waste packages have been produced. In order to reduce an environmental impact of the waste packages from the reprocessing plant, it is preferable to decompose nitrate ion to harmless gases such as nitrogen. A combination of formic acid and catalyst has been proposed for this purpose. But, the method is inadequate for a full decomposition of the nitrate ion. In addition, a mixture of NO and NO{sub 2} is produced during the reaction. Formaldehyde and hydrazine were selected as reductants and a combined use of Pd-Cu catalyst was tried to decompose the nitrate ion. As a result, the nitrate ion can almost entirely be decomposed without any generation of NO and NO{sub 2}. The test was conducted by 1 L flask. In case of formaldehyde, nitrate ion concentration can be reduced from 0.017 mol/l to 3.9x10{sup -4} mol/l. In case of hydrazine, nitrate concentration can be decreased from 2.8 mol/l to 9.5 x 10{sup -3} mol/l and ammonium ion is detected. The ammonium ion concentration in the final solution is 0.12 mol/l when 2.8 mol/l nitrate is reduced by hydrazine. Chemical reactions for formaldehyde on the Pd-Cu catalyst are estimated as combination of: NO{sub 3-} + HCHO = NO{sub 2-} + HCOOH; 2NO{sub 2-} + 3HCOOH = N{sub 2} + 3CO{sub 2} + 2H{sub 2}O + 2OH-; 4NO{sub 2-} + 3HCHO = 2N{sub 2} + 3CO{sub 2} + H{sub 2}O + 4OH-. the other hand, for hydrazine with the Pd-Cu catalyst: 3N{sub 2}H{sub 4} = 2NH{sub 3} + 2N{sub 2} + 3H{sub 2}; NO{sub 3-} + H{sub 2} = NO{sub 2-} + H{sub 2}O; NO{sub 2-} + NH{sub 3} = N{sub 2} + H{sub 2}O + OH-. The fundamental research shows that the combination usage of the Pd-Cu catalyst and formaldehyde or hydrazine is applicable for the reduction of nitrate liquid waste in the nuclear reprocessing plant. (authors)

  10. Quantification of Food Waste Disposal in the United States: A Meta-Analysis.

    PubMed

    Thyberg, Krista L; Tonjes, David J; Gurevitch, Jessica

    2015-12-15

    Food waste has major consequences for social, nutritional, economic, and environmental issues, and yet the amount of food waste disposed in the U.S. has not been accurately quantified. We introduce the transparent and repeatable methods of meta-analysis and systematic reviewing to determine how much food is discarded in the U.S., and to determine if specific factors drive increased disposal. The aggregate proportion of food waste in U.S. municipal solid waste from 1995 to 2013 was found to be 0.147 (95% CI 0.137-0.157) of total disposed waste, which is lower than that estimated by U.S. Environmental Protection Agency for the same period (0.176). The proportion of food waste increased significantly with time, with the western U.S. region having consistently and significantly higher proportions of food waste than other regions. There were no significant differences in food waste between rural and urban samples, or between commercial/institutional and residential samples. The aggregate disposal rate for food waste was 0.615 pounds (0.279 kg) (95% CI 0.565-0.664) of food waste disposed per person per day, which equates to over 35.5 million tons (32.2 million tonnes) of food waste disposed annually in the U.S. PMID:26551283

  11. Simultaneous Quantification of Dexpanthenol and Resorcinol from Hair Care Formulation Using Liquid Chromatography: Method Development and Validation

    PubMed Central

    De, Amit Kumar; Chowdhury, Partha Pratim; Chattapadhyay, Shyamaprasad

    2016-01-01

    The current study presents the simultaneous quantification of dexpanthenol and resorcinol from marketed hair care formulation. Dexpanthenol is often present as an active ingredient in personal care products for its beautifying and invigorating properties and restorative and smoothing properties. On the other hand resorcinol is mainly prescribed for the treatment of seborrheic dermatitis of scalp. The toxic side effects of resorcinol limit its use in dermatological preparations. Therefore an accurate quantification technique for the simultaneous estimation of these two components can be helpful for the formulation industries for the accurate analysis of their product quality. In the current study a high performance liquid chromatographic technique has been developed using a C18 column and a mobile phase consisting of phosphate buffer of pH = 2.8 following a gradient elution. The mobile phase flow rate was 0.6 mL per minute and the detection wavelength was 210 nm for dexpanthenol and 280 nm for resorcinol. The linearity study was carried out using five solutions having concentrations ranging between 10.34 μg·mL−1 and 82.69 μg·mL−1 (r2 = 0.999) for resorcinol and 10.44 μg·mL−1 and 83.50 μg·mL−1 (r2 = 0.998) for dexpanthenol. The method has been validated as per ICH Q2(R1) guidelines. The ease of single step sample preparation, accuracy, and precision (intraday and interday) study presents the method suitable for the simultaneous quantification of dexpanthenol and resorcinol from any personal care product and dermatological preparations containing these two ingredients. PMID:27042377

  12. Quantification of anthocyanins and flavonols in milk-based food products by ultra performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Nagy, Kornél; Redeuil, Karine; Bertholet, Raymond; Steiling, Heike; Kussmann, Martin

    2009-08-01

    The present article describes the development and validation of an ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for the comprehensive quantification of anthocyanin and flavonol constituents of milk-based food products. Protein precipitation by acidified methanol and ultrafiltration was utilized as sample preparation to preserve overall polyphenol composition but to eliminate milk proteins in order to comply with UPLC. Reversed-phase chromatography was optimized to achieve separation of 27 analytes in 10 min in order to reduce suppression effects, achieve a wide dynamic range, and most importantly, to resolve isomeric compounds. Positive-ion electrospray mass spectrometric detection and fragmentation of analytes was optimized, final transitions were selected for maximized selectivity, reliable quantification, and reduction of false positives. The quantitative performance of the method was validated, the main features include (1) range of lower limits of detection 0.3-30 ng/mL for glycosylated analytes, 10-300 ng/mL for aglycones, (2) lower limits of quantification 1-100 ng/mL for glycosylated analytes, 30-1,000 ng/mL for aglycones, (3) averaged intraday precision 9%, (4) calibrated range 2-180,000 ng/mL for glycosylated analytes, 60-600,000 ng/mL for aglycones, and (5) averaged accuracy 101%. Applications for yogurt and ice cream products are given. The presented data suggest that this method will help to better characterize the polyphenol composition of milk-based food products for quality control, for assessment of dietary intake, and for polyphenol bioavailability/bioefficacy studies. PMID:20337399

  13. Radwaste desk reference - Volume 3, Part 2: Liquid waste management. Final report

    SciTech Connect

    Deltete, D.; Fisher, S.; Kelly, J.J.; Mis, F.; Miller, C.; Soto, R.; Vance, J.

    1994-05-01

    EPRI began, in late in 1987, to produce a Radwaste Desk Reference that would allow each of the member utilities access to the available information and expertise on radwaste management. EPRI considers this important because radwaste management involves a wide variety of scientific and engineering disciplines. These include chemical and mechanical engineering, chemistry, and health physics. Radwaste management also plays a role in implementing a wide variety of regulatory requirements. These include plant-specific technical specifications, NRC standards for protection against radiation, DOT transportation regulations and major environmental legislation such as the Resource Conservation and Recovery Act. EPRI chose a question and answer format because it could be easily accessed by radwaste professionals with a variety of interests. The questions were generated at two meetings of utility radwaste professionals and EPRI contractors. Volume 1, which is already in publication, addresses dry active waste generation, processing and measurement. Volume 2 addresses low level waste storage, transportation and disposal. This volume, Volume 3, is being issued in two parts. Part 1 concentrates on the processing of liquid radioactive waste, whereas Part 2, included here, addresses liquid waste management. It includes extensive information and operating practices related to liquid waste generation and control, liquid waste processing systems at existing U.S. nuclear plants, processes for managing wet wastes (handling, dewatering, solidifying, processing, and packaging), and liquid waste measurement and analysis.

  14. Modified microspheres for cleaning liquid wastes from radioactive nuclides

    SciTech Connect

    Danilin, Lev; Drozhzhin, Valery

    2007-07-01

    An effective solution of nuclear industry problems related to deactivation of technological and natural waters polluted with toxic and radioactive elements is the development of inorganic sorbents capable of not only withdrawing radioactive nuclides, but also of providing their subsequent conservation under conditions of long-term storage. A successful technical approach to creation of sorbents can be the use of hollow aluminosilicate microspheres. Such microspheres are formed from mineral additives during coal burning in furnaces of boiler units of electric power stations. Despite some reduction in exchange capacity per a mass unit of sorbents the latter have high kinetic characteristics that makes it possible to carry out the sorption process both in static and dynamic modes. Taking into account large industrial resources of microspheres as by-products of electric power stations, a comparative simplicity of the modification process, as well as good kinetic and capacitor characteristics, this class of sorbents can be considered promising enough for solving the problems of cleaning liquid radioactive wastes of various pollution levels. (authors)

  15. Radioactive Liquid Waste Treatment Facility Discharges in 2011

    SciTech Connect

    Del Signore, John C.

    2012-05-16

    This report documents radioactive discharges from the TA50 Radioactive Liquid Waste Treatment Facilities (RLWTF) during calendar 2011. During 2011, three pathways were available for the discharge of treated water to the environment: discharge as water through NPDES Outfall 051 into Mortandad Canyon, evaporation via the TA50 cooling towers, and evaporation using the newly-installed natural-gas effluent evaporator at TA50. Only one of these pathways was used; all treated water (3,352,890 liters) was fed to the effluent evaporator. The quality of treated water was established by collecting a weekly grab sample of water being fed to the effluent evaporator. Forty weekly samples were collected; each was analyzed for gross alpha, gross beta, and tritium. Weekly samples were also composited at the end of each month. These flow-weighted composite samples were then analyzed for 37 radioisotopes: nine alpha-emitting isotopes, 27 beta emitters, and tritium. These monthly analyses were used to estimate the radioactive content of treated water fed to the effluent evaporator. Table 1 summarizes this information. The concentrations and quantities of radioactivity in Table 1 are for treated water fed to the evaporator. Amounts of radioactivity discharged to the environment through the evaporator stack were likely smaller since only entrained materials would exit via the evaporator stack.

  16. Identification, characterization, and high-performance liquid chromatography quantification of process-related impurities in vonoprazan fumarate.

    PubMed

    Liu, Lei; Cao, Na; Ma, Xingling; Xiong, Kaihe; Sun, Lili; Zou, Qiaogen

    2016-04-01

    High-performance liquid chromatography analysis of vonoprazan fumarate, a novel proton pump inhibitor drug revealed six impurities. These were identified by liquid chromatography with mass spectrometry. Further, the structures of the impurities were confirmed by synthesis followed by characterization by mass spectrometry, NMR spectroscopy, and infrared spectroscopy. On the basis of these data and knowledge of the synthetic scheme of vonoprazan fumarate, the previously unknown impurity was identified as 1-[5-(2-fluorophenyl)-1-(pyridin-3-ylsulfonyl)-1H-pyrrol-3-yl]-N-methyldimethylamine, which is a new compound. The possible mechanisms by which these impurities were formed were also discussed. A high-performance liquid chromatography method was optimized in order to separate, selectively detect, and quantify all process-related impurities of vonoprazan fumarate. The presented method has been validated in terms of linearity, limits of detection, and quantification, and response factors and, therefore, is highly suitable for routine analysis of vonoprazan fumarate related substances as well as stability studies. PMID:26843471

  17. Quantification of roxatidine in human plasma by liquid chromatography electrospray ionization tandem mass spectrometry: application to a bioequivalence study.

    PubMed

    Ryu, Ju-Hee; Choi, Sang-Jun; Lee, Heon-Woo; Choi, Seung-Ki; Lee, Kyung-Tae

    2008-12-01

    A sensitive and specific method using a one-step liquid-liquid extraction (LLE) with ethyl acetate followed by high-performance liquid chromatography (HPLC) coupled with positive ion electrospray ionization tandem mass spectrometry (ESI-MS/MS) detection was developed and validated for the determination of roxatidine in human plasma using famotidine as an internal standard (IS). Data acquisition was carried out in multiple reaction monitoring (MRM) mode, by monitoring the transitions m/z 307.3-->107.1 for roxatidine and m/z 338.4-->189.1 for famotidine. Chromatographic separation was performed on a reverse phase Hydrosphere C(18) column at 0.2 mL min(-1) using a mixture of methanol-ammonium formate buffer as mobile phase (20:80, v/v; adjusted to pH 3.9 with formic acid). The achieved lower limit of quantification (LLOQ) was 1.0 ng mL(-1) and the standard calibration curve for roxatidine was linear (r(2)=0.998) over the studied range (1-1000 ng mL(-1)) with acceptable accuracy and precision. Roxatidine was found to be stable in human plasma samples under short-, long-term storage and processing conditions. The developed method was validated and successfully applied to the bioequivalence study of roxatidine administrated as a single oral dose (75 mg as roxatidine acetate hydrochloride) to healthy female Korean volunteers. PMID:18977187

  18. Quantification of Modified Tyrosines in Healthy and Diabetic Human Urine using Liquid Chromatography/Tandem Mass Spectrometry.

    PubMed

    Kato, Yoji; Dozaki, Natsuko; Nakamura, Toshiyuki; Kitamoto, Noritoshi; Yoshida, Akihiro; Naito, Michitaka; Kitamura, Masayasu; Osawa, Toshihiko

    2009-01-01

    The quantification of urinary oxidized tyrosines, dityrosine (DiY), nitrotyrosine (NY), bromotyrosine (BrY), and dibromotyrosine (DiBrY), was accomplished by quadruple liquid chromatography-tandem mass spectrometry (LC/MS/MS). The sample was partially purified by solid phase extraction, and was then applied to the LC/MS/MS using multiple-reaction monitoring (MRM) methods. The analysis for the DiY quantification was done first. The residual samples were further butylated with n-butanol/HCl, and the other modified tyrosines were then quantified with isotopic dilution methods. MRM peaks of the modified tyrosines (DiY, NY, BrY, and DiBrY) from human urine were measured and the elution times coincided with the authentic and isotopic standards. The amounts of modified tyrosines in healthy human urine (n = 23) were 8.8 +/- 0.6 (DiY), 1.4 +/- 0.4 (NY), 3.8 +/- 0.3 (BrY), and 0.7 +/- 0.1 (DiBrY) micromol/mol of creatinine, respectively. A comparison of the modified tyrosines with urinary 8-oxo-deoxyguanosine, pentosidine, and N(epsilon)-(hexanoyl)lysine was also performed. Almost all products, except for NY, showed good correlations with each other. The amounts of the modified tyrosines (NY, BrY, and DiBrY) in the diabetic urine were higher than those in the urine from healthy people. PMID:19177191

  19. Quantification of multiple DNA adducts formed through oxidative stress using liquid chromatography and electrospray tandem mass spectrometry.

    PubMed

    Churchwell, Mona I; Beland, Frederick A; Doerge, Daniel R

    2002-10-01

    Damage to DNA can arise through covalent modification of bases by reaction with oxidants and products of lipid peroxidation derived through normal aerobic metabolism. Such premutagenic lesions, including 8-oxo-7,8-dihydro-2'-deoxyguanosine (8-oxo-dG), pyrimido[1,2alpha]purine-10(3H)one-2'-deoxyribose (M1-dG), etheno-2'-deoxyadenosine (epsilon-dA), and etheno-2'-deoxycytidine (epsilon-dC), are believed to be important in the development of human cancers related to diet, disease states, and lifestyle. We report the development of a method for concurrent quantification of these four adducts in DNA hydrolysates of 100 microg or less using on-line sample preparation coupled with liquid chromatography and tandem mass spectrometry. The sensitive detection permitted adduct quantification at levels below one adduct in 10(8) normal nucleotides and measurement of these adducts in DNA from untreated rodent liver and normal human liver samples. This methodology should prove useful in hypothesis-driven studies of cancer etiology in laboratory animals and humans. PMID:12387628

  20. Identification and quantification of active alkaloids in Catharanthus roseus by liquid chromatography-ion trap mass spectrometry.

    PubMed

    Chen, Qinhua; Zhang, Wenpeng; Zhang, Yulin; Chen, Jing; Chen, Zilin

    2013-08-15

    Catharanthus roseus is an important dicotyledonous medicinal plant that produces anticancer compounds. The active alkaloids vinblastine, vindoline, ajmalicine, catharanthine, and vinleurosine were identified by direct-injection ion trap-mass spectrometry (IT-MS) for collecting MS(1-2) spectra. The determinations of five alkaloids were accomplished by liquid chromatography (LC) with UV and MS detections. The analytes provided good signals corresponding to the protonated molecular ions [M+H](+) and product ions. The precursor ions and product ions for quantification of vinblastine, vindoline, ajmalicine, catharanthine, and vinleurosine were m/z 825→807, 457→397, 353→144, 337→144 and 809→748 by LC-IT-MS, respectively. Two methods were used to evaluate a number of validation characteristics (repeatability, LOD, calibration range, and recovery). MS provided a high selectivity and sensitivity for determination of five alkaloids in positive mode. After optimisation of the methods, separation, identification and quantification of the five components in C. roseus were comprehensively accomplished by HPLC with UV and MS detection. PMID:23561180

  1. Liquid-phase microextraction and desorption electrospray ionization mass spectrometry for identification and quantification of basic drugs in human urine.

    PubMed

    Thunig, Janina; Flø, Linda; Pedersen-Bjergaard, Stig; Hansen, Steen Honoré; Janfelt, Christian

    2012-01-30

    Hollow fibre liquid-phase microextraction (LPME) and desorption electrospray ionization mass spectrometry (DESI-MS) were evaluated for the identification and quantification of basic drugs in human urine samples. The selective extraction capabilities of three-phase LPME provided a significant reduction in the matrix effects otherwise observed in direct DESI-MS analysis of urine samples. Aqueous LPME extracts (in 10 mM HCl) were deposited on porous Teflon, dried at room temperature, and the dried spots were then analyzed directly with DESI-MS in full scan mode. Pethidine, diphenhydramine, nortriptyline, and methadone were used as model compounds for identification, and their limits of identification were determined to be 100, 25, 100, and 30 ng/mL, respectively. In a reliability test with 19 spiked urine samples, 100% of the positive samples containing the model drugs in concentrations at or above the limit of identification were identified. Diphenhydramine was used as a model compound for quantitative analysis with diphenhydramine-d(5) as an internal standard. The calibration curve was linear in the range 50-2000 ng/mL (R(2) = 0.992) with a limit of quantification at approximately 140 ng/mL. The intra- and inter-day relative standard deviations were <9.5%. In a reliability test with six spiked urine samples, deviations between the measured and the true values for diphenhydramine were in the range 0.2-22.9%. PMID:22173801

  2. Pantothenic acid quantification by a stable isotope dilution assay based on liquid chromatography-tandem mass spectrometry.

    PubMed

    Rychlik, Michael

    2003-07-01

    A stable isotope dilution assay for the quantification of free and total pantothenic acid has been developed by using [13C3,15N]-pantothenic acid as the internal standard. The three-dimensional specificity of liquid chromatography-tandem mass spectrometry enabled unequivocal determination of the vitamin. Due to the very simple extraction and clean-up procedure, free pantothenic acid could be analysed within 2 h, which is much faster than by microbiological or gas chromatographic assays. For quantification of total pantothenic acid, the vitamin was liberated from its conjugates by an overnight incubation with pigeon liver pantetheinase and alkaline phosphatase. In analyses of corn flour, the intra-assay coefficient of variation was 8.5% (n = 5) and 15.3% (n = 4) for free and total pantothenic acid, respectively. When pantothenic acid was added to corn starch at a level of 6 mg kg(-1), a recovery of 97.5% was found. Application of the stable isotope dilution assay to whole egg powder, hazel nuts and corn revealed similar data compared to those listed in nutrition data bases, whereas the content in mushrooms and porcine liver determined by the newly developed assay appeared to be lower and that of cocoa higher than reported in the literature. PMID:12894818

  3. Quantification of phylloquinone and menaquinones in feces, serum, and food by high-performance liquid chromatography-mass spectrometry.

    PubMed

    Karl, J Philip; Fu, Xueyan; Dolnikowski, Gregory G; Saltzman, Edward; Booth, Sarah L

    2014-07-15

    Vitamin K, comprising phylloquinone (PK) and menaquinones (MKn), is a family of vitamers found in multiple biological and environmental matrices. Advancing emerging evidence for novel and distinct physiologic roles of these vitamers in human health and disease necessitates sensitive and selective methods for quantifying PK and MKn in these matrices. We developed a novel method employing high-performance liquid chromatography-mass spectrometry with atmospheric pressure chemical ionization (LC-APCI-MS) for simultaneous quantification of 11 vitamin K vitamers that can be applied in feces, serum and food. Minimal detectable concentrations of vitamin K vitamers ranged from 1 pmol/g to 30 pmol/g. Limits of quantification ranged from 5 pmol/g to 90 pmol/g. Inter-assay and intra-assay variations were <17% and <8%, respectively, in food, and <12% and <8%, respectively, in feces. Recovery exceeded 80% for all vitamers in both food and feces. The method successfully quantified PK and MKn concentrations in rat chow, feces and serum. In summary, this LC-APCI-MS method provides a sensitive and selective tool for quantifying vitamin K vitamers in feces, serum and food. This method can be applied in human and animal studies examining the role of vitamin K vitamers derived from the diet and gut bacteria synthesis in health and disease. PMID:24956079

  4. Quantification of isocyanates and amines in polyurethane foams and coated products by liquid chromatography–tandem mass spectrometry

    PubMed Central

    Mutsuga, Motoh; Yamaguchi, Miku; Kawamura, Yoko

    2014-01-01

    An analytical method for the identification and quantification of 10 different isocyanates and 11 different amines in polyurethane (PUR) foam and PUR-coated products was developed and optimized. Isocyanates were extracted and derivatized with di-n-butylamine, while amines were extracted with methanol. Quantification was subsequently performed by liquid chromatography–tandem mass spectrometry. Using this methodology, residual levels of isocyanates and amines in commercial PUR products were quantified. Although the recoveries of certain isocyanates and amines were low, the main compounds used as monomers in the production of PUR products, and their decomposition species, were clearly identified at quantifiable levels. 2,4-and 2,6-toluenediisocyanate were detected in most PUR foam samples and a pastry bag in the range of 0.02–0.92 mg/kg, with their decomposition compounds, 2,4-and 2,6-toluenediamine, detected in all PUR foam samples in the range of 9.5–59 mg/kg. PUR-coated gloves are manufactured using 4,4′-methylenebisphenyl diisocyanate as the main raw material, and a large amount of this compound, in addition to 4,4′-methylenedianiline and dicyclohexylmethane-4,4′-diamine were found in these samples. PMID:24804074

  5. Environmental data package for ORNL Solid Waste Storage Area Four, the adjacent intermediate-level liquid waste transfer line, and the liquid waste pilot pit area

    SciTech Connect

    Davis, E.C.; Shoun, R.R.

    1986-09-01

    The Oak Ridge National Laboratory Remedial Action Program has determined through its review of past environmental studies that Solid Waste Storage Area Four (SWSA-4) continually releases radioactivity to White Oak Creek and therefore requires application of the site stabilization and remedial actions outlined under the 3004u provisions of the Resource Conservation and Recovery Act. Under these provisions, a Remedial Investigation/Feasibility Study (RI/FS) forms the basis for determining the extent of actions. This report assembles available historical and environmental data relative to the SWSA-4 waste area grouping (WAG), which includes the 9.3-ha SWSA-4 site, the adjacent abandoned intermediate-level liquid waste transfer line, and the experimental pilot pit area. The rationale for grouping these three waste management units into the SWSA-4 WAG is the fact that they each lie in the same hydrologic unit and share a common tributary to White Oak Creek. The results of this compilation demonstrate that although a considerable number of studies have been carried out in SWSA-4, needs such as installation of water quality wells and continued monitoring and reporting of hydrologic data still exist. These needs will become even more critical as the RI/FS process proceeds and remedial measures for the site are considered. Fewer studies have been carried out to characterize the extent of contamination at the waste transfer line and the pilot pit area. Alternatives for characterizing and stabilizing these two minor components of the SWSA-4 WAG are presented; however, extensive remedial actions do not appear to be warranted.

  6. Solid waste characterization, quantification and management practices in developing countries. a case study: Nablus district - Palestine.

    PubMed

    Al-Khatib, Issam A; Monou, Maria; Abu Zahra, Abdul Salam F; Shaheen, Hafez Q; Kassinos, Despo

    2010-05-01

    Solid waste management (SWM) is one of the most challenging issues faced by developing countries that suffer from serious pollution problems caused by the generation of large waste quantities. This paper presents the case study of SWM in the Nablus district - Palestine. Surveys for household residents' and SWM program operators, field investigations, on-site waste measurements and characterizations were conducted. Per capita waste generation rates varied between different localities although trends were similar. Overall, the majority of waste was organic (65.1% by weight), suggesting a strong resource recovery potential in terms of animal feed or compost. Recyclable waste (plastic, paper and card) made up 16.7% by weight the waste composition suggesting an incentive to introduce source separation. Household attitudes complemented the waste characterization study, revealing the main problems faced. SWM operators quoted on the current status, highlighting problems with disposing in unsanitary landfills, ineffective solid waste fees system, increasing solid waste quantities and lacking equipment and experienced personnel. To enhance sustainable SWM, public awareness, funding, expertise, equipment and facilities and other provisions currently lacking or inappropriate must be provided. PMID:20116162

  7. Detection and Quantification of Pu(III, IV, V, and VI) Using a1.0-meter Liquid Core Waveguide

    SciTech Connect

    Wilson, Richard E.; Hu, Yung-Jin; Nitsche, Heino

    2005-02-15

    Detection and quantification of the aquo ions of Pu in 1 MHClO4 was carried out using a 1-meter liquid core waveguide (LCW) coupledto a fiber optic UV-Vis spectrometer. Detection limits of 7 x 10-7 M forPu(VI), 1.6 x 10-5 M for Pu(V), 5 x 10-6 M for Pu(IV) and 8 x 10-6 M forPu(III) were achieved. The limits of detection represent increases of 18to 33 times those achievable using a conventional 1-cm path length.Because of the much lower detection limits of the LCW, routineidentification of the oxidation states in dilute Pu solutions can bemade.

  8. A&M. Hot liquid waste building (TAN616) under construction. Camera facing ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    A&M. Hot liquid waste building (TAN-616) under construction. Camera facing northeast. Date: November 25, 1953. INEEL negative no. 9232 - Idaho National Engineering Laboratory, Test Area North, Scoville, Butte County, ID

  9. A&M. Hot liquid waste building (TAN616). Interior of evaporator control ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    A&M. Hot liquid waste building (TAN-616). Interior of evaporator control room. Date: 1962. INEEL negative no. 62-6824 - Idaho National Engineering Laboratory, Test Area North, Scoville, Butte County, ID

  10. Liquid and Gaseous Waste Operations Department annual operating report, CY 1995

    SciTech Connect

    Maddox, J.J.; Scott, C.B.

    1996-03-01

    This report describes the operating activities, upgrade activities, maintenance, and other activities regarding liquid and gaseous low level radioactive waste management at the Oak Ridge National Laboratory. Miscellaneous activities include training, audits, tours, and environmental restoration support.

  11. Disposal of Liquid Wastes from Parlors and Milkhouses. Special Circular 154.

    ERIC Educational Resources Information Center

    Wooding, N. Henry

    This circular provides information to assist in assessing the pollution potential of liquid wastes from parlors and milkhouses. Approaches to resolving problems through stabilization lagoons, irrigation, and tank collection as mandated in statutory authority are discussed. (CS)

  12. Electrophoresis Gel Quantification with a Flatbed Scanner and Versatile Lighting from a Screen Scavenged from a Liquid Crystal Display (LCD) Monitor

    ERIC Educational Resources Information Center

    Yeung, Brendan; Ng, Tuck Wah; Tan, Han Yen; Liew, Oi Wah

    2012-01-01

    The use of different types of stains in the quantification of proteins separated on gels using electrophoresis offers the capability of deriving good outcomes in terms of linear dynamic range, sensitivity, and compatibility with specific proteins. An inexpensive, simple, and versatile lighting system based on liquid crystal display backlighting is…

  13. Functions and requirements document, WESF decoupling project, low-level liquid waste system

    SciTech Connect

    Rasmussen, J.H., Fluor Daniel Hanford

    1997-02-27

    The Waste Encapsulation and Storage Facility (WESF) was constructed in 1974 to encapsulate and store cesium and strontium which were isolated at B Plant from underground storage tank waste. The WESF, Building 225-B, is attached physically to the west end of B Plant, Building 221-B, 200 East area. The WESF currently utilizes B Plant facilities for disposing liquid and solid waste streams. With the deactivation of B Plant, the WESF Decoupling Project will provide replacement systems allowing WESF to continue operations independently from B Plant. Four major systems have been identified to be replaced by the WESF Decoupling Project, including the following: Low Level Liquid Waste System, Solid Waste Handling System, Liquid Effluent Control System, and Deionized Water System.

  14. A Regulatory Analysis and Reassessment of U.S. Environmental Protection Agency Listed Hazardous Waste Numbers for Applicability to the INTEC Liquid Waste System

    SciTech Connect

    Gilbert, K.L.; Venneman, T.E.

    1998-12-01

    This report concludes that there are four listed hazardous waste numbers (F001, F002, F005, and U134) applicable to the waste in the Process Equipment Waste Evaporator (PEWE) liquid waste system at the Idaho National Engineering and Environmental Laboratory. The chemical constituents associated with these listed hazardous waste numbers, including those listed only for ignitability are identified. The RCRA Part A permit application hazardous waste numbers identify chemical constituents that may be treated or stored by the PEWE liquid waste system either as a result of a particular characteristic (40 CFR, Subpart C) or as a result of a specific process (40 CFR 261, Subpart D). The RCRA Part A permit application for the PEWE liquid waste system identifies the universe of Environmental Protection Agency (EPA) hazardous waste numbers [23 characteristic (hazardous waste codes) numbers and 105 listed numbers (four F-listed hazardous waste numbers, 20 P-listed hazardous waste numbers, and 81 U-listed hazardous waste numbers)] deemed acceptable for storage and treatment. This evaluation, however, identifies only listed wastes (and their chemical constituents) that have actually entered the PEWE liquid waste system and would, therefore, be assigned to the PEWE liquids and treatment residuals.

  15. Disposal of Liquid Combustible Wastes using Flameless Burners with Porous Carbon Matrix

    NASA Astrophysics Data System (ADS)

    Dolgov, Sergei; Savchenko, Evgenii; Khaustov, Sergei; Tabakaev, Roman; Zavorin, Alexander

    2016-02-01

    Two modifications of flameless burners with a carbon porous media in the combustion area were investigated. Kerosene TS-1 and mixtures of highly flammable liquids wastes (HIL) were used as fuel. Experimental data are presented in a graphical form as plot of the burner thermal capacity. Results show capacity for of the developed devices and prove the prospects of disposal of liquid combustible wastes using flameless burners with porous carbon matrix.

  16. Evaluation of Mercury in Liquid Waste Processing Facilities - Phase I Report

    SciTech Connect

    Jain, V.; Occhipinti, J.; Shah, H.; Wilmarth, B.; Edwards, R.

    2015-07-01

    This report provides a summary of Phase I activities conducted to support an Integrated Evaluation of Mercury in Liquid Waste System (LWS) Processing Facilities. Phase I activities included a review and assessment of the liquid waste inventory and chemical processing behavior of mercury using a system by system review methodology approach. Gaps in understanding mercury behavior as well as action items from the structured reviews are being tracked. 64% of the gaps and actions have been resolved.

  17. Evaluation of mercury in liquid waste processing facilities - Phase I report

    SciTech Connect

    Jain, V.; Occhipinti, J. E.; Shah, H.; Wilmarth, W. R.; Edwards, R. E.

    2015-07-01

    This report provides a summary of Phase I activities conducted to support an Integrated Evaluation of Mercury in Liquid Waste System (LWS) Processing Facilities. Phase I activities included a review and assessment of the liquid waste inventory and chemical processing behavior of mercury using a system by system review methodology approach. Gaps in understanding mercury behavior as well as action items from the structured reviews are being tracked. 64% of the gaps and actions have been resolved.

  18. A&M. Hot liquid waste treatment building (TAN616). Camera facing southwest. ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    A&M. Hot liquid waste treatment building (TAN-616). Camera facing southwest. Oblique view of east and north walls. Note three corrugated pipes at lower left indicating location of underground hot waste storage tanks. Photographer: Ron Paarmann. Date: September 22, 1997. INEEL negative no. HD-20-1-4 - Idaho National Engineering Laboratory, Test Area North, Scoville, Butte County, ID

  19. ASSESSMENT OF LIQUID EMULSION MEMBRANE FOR CLEAN UP OF AQUEOUS WASTE EFFLUENTS FROM HAZARDOUS ELEMENTS

    SciTech Connect

    El-Reefy, Sohair A.; Selim, Y.T.; Hassan, M.A.; Aly, H.F.

    2003-02-27

    Four liquid emulsion membrane (LEM) systems are given to remove different hazardous elements such as uranium, thorium, cobalt, copper, lead, and cadmium from different aqueous waste effluents. The optimum conditions for use of these systems are deduced. The potentiality of LEM for removal of hazardous pollutants from aqueous waste solutions is given.

  20. FACTORS IN ASSESSING THE COMPATIBILITY OF FMLS (FLEXIBLE MEMBRANE LINERS) AND WASTE LIQUIDS

    EPA Science Inventory

    The experimental research project studied various factors in the compatibility of flexible membrane liners (FMLs) with waste liquids and other hazardous substances that may be encountered in waste storage and disposal facilities. This work included: (1) Swelling of FMLs and other...

  1. Quantification of construction waste prevented by BIM-based design validation: Case studies in South Korea.

    PubMed

    Won, Jongsung; Cheng, Jack C P; Lee, Ghang

    2016-03-01

    Waste generated in construction and demolition processes comprised around 50% of the solid waste in South Korea in 2013. Many cases show that design validation based on building information modeling (BIM) is an effective means to reduce the amount of construction waste since construction waste is mainly generated due to improper design and unexpected changes in the design and construction phases. However, the amount of construction waste that could be avoided by adopting BIM-based design validation has been unknown. This paper aims to estimate the amount of construction waste prevented by a BIM-based design validation process based on the amount of construction waste that might be generated due to design errors. Two project cases in South Korea were studied in this paper, with 381 and 136 design errors detected, respectively during the BIM-based design validation. Each design error was categorized according to its cause and the likelihood of detection before construction. The case studies show that BIM-based design validation could prevent 4.3-15.2% of construction waste that might have been generated without using BIM. PMID:26754615

  2. Liquid low-level waste generation projections for ORNL in 1993

    SciTech Connect

    DePaoli, S.M.

    1994-04-01

    Liquid low-level waste (LLLW) is generated by various programs and projects throughout Oak Ridge National Laboratory (ORNL). These wastes are collected in underground collection tanks, bottles, and trucks; they are then neutralized with sodium hydroxide and treated for volume reduction at the ORNL evaporator facility. This report presents historical and projected data concerning the volume and characterization of LLLW, prior to and after evaporation. Storage space for projected waste generation is also discussed.

  3. Current and projected liquid low-level waste generation at ORNL

    SciTech Connect

    DePaoli, S.M.; West, G.D.

    1996-04-01

    Liquid low-level waste (LLLW) is generated by various programs and projects throughout Oak Ridge National Laboratory (ORNL). This waste is collected in bottles, by trucks, or in underground collection tanks; it is then neutralized with sodium hydroxide and reduced in volume at the ORNL LLLW evaporator. This report presents historical and projected data concerning the volume and the characterization of LLLW, both prior to and after evaporation. Storage space for projected waste generation is also discussed.

  4. Biological Information Document, Radioactive Liquid Waste Treatment Facility

    SciTech Connect

    Biggs, J.

    1995-12-31

    This document is intended to act as a baseline source material for risk assessments which can be used in Environmental Assessments and Environmental Impact Statements. The current Radioactive Liquid Waste Treatment Facility (RLWTF) does not meet current General Design Criteria for Non-reactor Nuclear Facilities and could be shut down affecting several DOE programs. This Biological Information Document summarizes various biological studies that have been conducted in the vicinity of new Proposed RLWTF site and an Alternative site. The Proposed site is located on Mesita del Buey, a mess top, and the Alternative site is located in Mortandad Canyon. The Proposed Site is devoid of overstory species due to previous disturbance and is dominated by a mixture of grasses, forbs, and scattered low-growing shrubs. Vegetation immediately adjacent to the site is a pinyon-juniper woodland. The Mortandad canyon bottom overstory is dominated by ponderosa pine, willow, and rush. The south-facing slope was dominated by ponderosa pine, mountain mahogany, oak, and muhly. The north-facing slope is dominated by Douglas fir, ponderosa pine, and oak. Studies on wildlife species are limited in the vicinity of the proposed project and further studies will be necessary to accurately identify wildlife populations and to what extent they utilize the project area. Some information is provided on invertebrates, amphibians and reptiles, and small mammals. Additional species information from other nearby locations is discussed in detail. Habitat requirements exist in the project area for one federally threatened wildlife species, the peregrine falcon, and one federal candidate species, the spotted bat. However, based on surveys outside of the project area but in similar habitats, these species are not expected to occur in either the Proposed or Alternative RLWTF sites. Habitat Evaluation Procedures were used to evaluate ecological functioning in the project area.

  5. 327 Building liquid waste handling options modification project plan

    SciTech Connect

    Ham, J.E.

    1998-03-28

    This report evaluates the modification options for handling radiological liquid waste (RLW) generated during decontamination and cleanout of the 327 Building. The overall objective of the 327 Facility Stabilization Project is to establish a passively safe and environmentally secure configuration of the 327 Facility. The issue of handling of RLW from the 327 Facility (assuming the 34O Facility is not available to accept the RLW) has been conceptually examined in at least two earlier engineering studies (Parsons 1997a and Hobart l997). Each study identified a similar preferred alternative that included modifying the 327 Facility RLWS handling systems to provide a truck load-out station, either within the confines of the facility or exterior to the facility. The alternatives also maximized the use of existing piping, tanks, instrumentation, controls and other features to minimize costs and physical changes. An issue discussed in each study involved the anticipated volume of the RLW stream. Estimates ranged between 113,550 and 387,500 liters in the earlier studies. During the development of the 324/327 Building Stabilization/Deactivation Project Management Plan, the lower estimate of approximately 113,550 liters was confirmed and has been adopted as the baseline for the 327 Facility RLW stream. The goal of this engineering study is to reevaluate the existing preferred alternative and select a new preferred alternative, if appropriate. Based on the new or confirmed preferred alternative, this study will also provide a conceptual design and cost estimate for required modifications to the 327 Facility to allow removal of RLWS and treatment of the RLW generated during deactivation.

  6. OCCURRENCE OF TRANSIENT PUFFS IN A ROTARY KILN INCINERATOR SIMULATOR. 2. CONTAINED LIQUID WASTES ON SORBENT

    EPA Science Inventory

    The paper gives results of a study of the generation of transient puffs resulting from the batch incineration of liquid waste into a 73 kW rotary kiln incinerator simulator. The liquid was added onto a sorbent, enclosed in cardboard cylinders that are introduced into the combusti...

  7. Quantification of photoinduced order increase in liquid crystals with naphthopyran guests

    NASA Astrophysics Data System (ADS)

    Rumi, Mariacristina; Cazzell, Seth A.; Kosa, Tamas; Sukhomlinova, Ludmila; Taheri, Bahman; White, Timothy J.; Bunning, Timothy J.

    2016-03-01

    Photoinduced order-increasing phase transitions can occur in dye-liquid crystal mixtures when the photoproduct of the excitation of the dye molecules is more compatible with the liquid crystalline medium than the initial dye species. A detailed investigation of the photoinduced changes of the phase behavior and optical properties of mixtures of liquid crystals with naphthopyran guests upon exposure to light at 365 nm is presented here. In these guest-host systems, the nematic-to-isotropic phase transition temperature is increased upon irradiation. We show that the nematic range can be extended up to 2.9 °C by illumination in 5CB (4 -n -pentyl-4'-cyanobiphenyl) liquid crystal mixtures. The order parameter is significantly increased by illumination at all temperatures within the nematic range and the changes are larger at higher concentrations of the guests. In particular, the illuminated guest-host mixtures exhibit order parameters close to those of the neat liquid crystal host at the same temperature relative to the clearing point. An improved understanding of the photophysical processes taking place at the molecular level in these material systems can inform the design of photoresponsive materials and enhance their potential utility in optical or photonic devices.

  8. System for removing liquid waste from a tank

    DOEpatents

    Meneely, T.K.; Sherbine, C.A.

    1994-04-26

    A tank especially suited for nuclear applications is disclosed. The tank comprises a tank shell for protectively surrounding the liquid contained therein; an inlet positioned on the tank for passing a liquid into the tank; a sump positioned in an interior portion of the tank for forming a reservoir of the liquid; a sloped incline for resting the tank thereon and for creating a natural flow of the liquid toward the sump; a pump disposed adjacent the tank for pumping the liquid; and a pipe attached to the pump and extending into the sump for passing the liquid there through. The pump pumps the liquid in the sump through the pipe and into the pump for discharging the liquid out of the tank. 2 figures.

  9. System for removing liquid waste from a tank

    DOEpatents

    Meneely, Timothy K.; Sherbine, Catherine A.

    1994-01-01

    A tank especially suited for nuclear applications is disclosed. The tank comprises a tank shell for protectively surrounding the liquid contained therein; an inlet positioned on the tank for passing a liquid into the tank; a sump positioned in an interior portion of the tank for forming a reservoir of the liquid; a sloped incline for resting the tank thereon and for creating a natural flow of the liquid toward the sump; a pump disposed adjacent the tank for pumping the liquid; and a pipe attached to the pump and extending into the sump for passing the liquid therethrough. The pump pumps the liquid in the sump through the pipe and into the pump for discharging the liquid out of the tank.

  10. Simultaneous quantification of cardiovascular disease related metabolic risk factors using liquid chromatography tandem mass spectrometry in human serum.

    PubMed

    Wang, Mo; Yang, Ruiyue; Dong, Jun; Zhang, Tianjiao; Wang, Siming; Zhou, Weiyan; Li, Hongxia; Zhao, Haijian; Zhang, Lijiao; Wang, Shu; Zhang, Chuanbao; Chen, Wenxiang

    2016-01-15

    Recent observations from metabonomic studies have consistently found that branched-chain amino acids (BCAAs), aromatic amino acids (AAAs), glutamine (Gln), glutamic acid (Glu), Gln/Glu ratio, carnitine, and several species of acylcarnitines and lysophosphatidylcholines (LPCs) are possible risk factors for metabolic diseases such as diabetes mellitus (DM) and cardiovascular diseases (CVD). We described here a simple and reliable method for simultaneous quantification of these metabolic risk factors by liquid chromatography tandem mass spectrometry (LC-MS/MS). Serum samples were extracted with isopropanol, and the extracted metabolites were separated by hydrophilic interaction liquid chromatography (HILIC) and detected with electrospary ionization (ESI) inpositive ion mode with multiple reaction monitor (MRM) mode. All the metabolites were effectively separated within 5.5min. Analytical recoveries were in the range of 92.8-106.9%, with an average of 100.6%. The intra- run and total imprecisions for the measurement of these metabolites were 1.2-3.8% and 1.5-7.4%, respectively. Serum concentrations of the metabolites were analyzed in 123 apparently healthy volunteers. Significant associations between the metabolites and traditional CVD risk factors were observed. The newly developed LC-MS/MS method was simple, precise, and accurate and can be used as an efficient tool in CVD research and studies. PMID:26735710

  11. Remotely operated organic liquid waste incinerator for the fuels and materials examination facility

    SciTech Connect

    Sales, W.L.; Barker, R.E.; Hershey, R.B.

    1980-01-01

    The search for a practical method for the disposal of small quantities of oraganic liquid waste, a waste product of metallographic sample preparation at the Fuels and Materials Examination Facility has led to the design of an incinerator/off-gas system to burn organic liquid wastes and selected organic solids. The incinerator is to be installed in a shielded inert-atmosphere cell, and will be remotely operated and maintained. The off-gas system is a wet-scrubber and filter system designed to release particulate-free off-gas to the FMEF Building Exhaust System.

  12. Low-level detection and quantification of Plutonium(III, IV, V,and VI) using a liquid core waveguide

    SciTech Connect

    Wilson, Richard E.; Hu, Yung-Jin; Nitsche, Heino

    2003-06-28

    Understanding the aqueous chemistry of plutonium, in particular in environmental conditions, is often complicated by plutonium's complex redox chemistry. Because plutonium possesses four oxidation states, all of which can coexist in solution, a reliable method for the identification of these oxidation states is needed. The identification of plutonium oxidation states at low levels in aqueous solution is often accomplished through an indirect determination using series of liquid-liquid extraction procedures using oxidation state specific reagents such as HDEHP and TTA. While these methods, coupled with radioactive counting techniques provide superior limits of detection they may influence the plutonium redox equilibrium, are time consuming, waste intensive and costly. Other analytical methods such as mass spectrometry and radioactive counting as stand alone methods provide excellent detection limits but lack the ability to discriminate between the oxidation states of the plutonium ions in solution.

  13. Rapid quantification of imidazolium-based ionic liquids by hydrophilic interaction liquid chromatography: Methodology and an investigation of the retention mechanisms.

    PubMed

    Hawkins, Cory A; Rud, Anna; Guthrie, Margaret L; Dietz, Mark L

    2015-06-26

    The separation of nine N,N'-dialkylimidazolium-based ionic liquids (ILs) by an isocratic hydrophilic interaction high-performance liquid chromatographic method using an unmodified silica column was investigated. The chosen analytical conditions using a 90:10 acetonitrile-ammonium formate buffer mobile phase on a high-purity, unmodified silica column were found to be efficient, robust, and sensitive for the determination of ILs in a variety of solutions. The retention window (k' = 2-11) was narrower than that of previous methods, resulting in a 7-min runtime for the nine IL homologues. The lower limit of quantification of the method, 2-3 μmol L(-1), was significantly lower than those reported previously for HPLC-UV methods. The effects of systematically modifying the IL cation alkyl chain length, column temperature, and mobile-phase water and buffer content on solute retention were examined. Cation exchange was identified as the dominant retention mechanism for most of the solutes, with a distinct (single methylene group) transition to a dominant partitioning mode at the highest solute polarity. PMID:25979537

  14. Simultaneous Quantification of 20 Synthetic Cannabinoids and 21 Metabolites, and Semi-quantification of 12 Alkyl Hydroxy Metabolites in Human Urine by Liquid Chromatography-Tandem Mass Spectrometry

    PubMed Central

    Scheidweiler, Karl B.; Huestis, Marilyn A.

    2014-01-01

    Clandestine laboratories constantly produce new synthetic cannabinoids to circumvent legislative efforts, complicating toxicological analysis. No extensive synthetic cannabinoid quantitative urinary methods are reported in the literature. We developed and validated a liquid chromatography tandem mass spectrometric (LC-MS/MS) method for simultaneously quantifying JWH-018, JWH-019, JWH-073, JWH-081, JWH-122, JWH-200, JWH-210, JWH-250, JWH-398, RCS-4, AM-2201, MAM-2201, UR-144, CP 47,497-C7, CP 47,497-C8 and their metabolites, and JWH-203, AM-694, RCS-8, XLR-11 and HU-210 parent compounds in urine. Non-chromatographically resolved alkyl hydroxy metabolite isomers were considered semi-quantitative. β-glucuronidase hydrolyzed urine was extracted with 1 ml Biotage SLE+ columns. Specimens were reconstituted in 150 µL mobile phase consisting of 50% A (0.01% formic acid in water) and 50% B (0.01% formic acid in 50:50 methanol:acetonitrile). 4 and 25 µL injections were performed to acquire data in positive and negative ionization modes, respectively. The LC-MS/MS instrument consisted of a Shimadzu UFLCxr system and an ABSciex 5500 Qtrap mass spectrometer with an electrospray source. Gradient chromatographic separation was achieved utilizing a Restek Ultra Biphenyl column with a 0.5 ml/min flow rate and an overall run time of 19.5 and 11.4 min for positive and negative mode methods, respectively. Quantification was by multiple reaction monitoring with CP 47,497 compounds and HU-210 ionized via negative polarity; all other analytes were acquired in positive mode. Lower and upper limits of linearity were 0.1–1.0 and 50–100 µg/l (r2 > 0.994). Validation parameters were evaluated at three concentrations spanning linear dynamic ranges. Inter-day analytical recovery (bias) and imprecision (N=20) were 88.3–112.2% and 4.3–13.5% coefficient of variation, respectively. Extraction efficiencies and matrix effect (N=10) were 44–110 and −73 to 52%, respectively. We present

  15. Treatment of radioactive liquid waste by sorption on natural zeolite in Turkey.

    PubMed

    Osmanlioglu, Ahmet Erdal

    2006-09-01

    Liquid radioactive waste has been generated from the use of radioactive materials in industrial applications, research and medicine in Turkey. Natural zeolites (clinoptilolite) have been studied for the removal of several key radionuclides ((137)Cs, (60)Co, (90)Sr and (110m)Ag) from liquid radioactive waste. The aim of the present study is to investigate effectiveness of zeolite treatment on decontamination factor (DF) in a combined process (chemical precipitation and adsorption) at the laboratory tests and scale up to the waste treatment plant. In this study, sorption and precipitation techniques were adapted to decontamination of liquid low level waste (LLW). Effective decontamination was achieved when sorbents are used during the chemical precipitation. Natural zeolite samples were taken from different zeolite formations in Turkey. Comparison of the ion-exchange properties of zeolite minerals from different formations shows that Gordes clinoptilolite was the most suitable natural sorbent for radionuclides under dynamic treatment conditions and as an additive for chemical precipitation process. Clinoptilolite were shown to have a high selectivity for (137)Cs and (110m)Ag as sorbent. In the absence of potassium ions, native clinoptilolite removed (60)Co and (90)Sr very effectively from the liquid waste. In the end of this liquid waste treatment, decontamination factor was provided as 430 by using 0.5 mm clinoptilolite at 30 degrees C. PMID:16563616

  16. A New Technique for Quantification of Elemental Hg in Mine Wastes and Its Implications for Mercury Evasion Into the Atmosphere

    PubMed Central

    JEW, ADAM D.; KIM, CHRISTOPHER S.; RYTUBA, JAMES J.; GUSTIN, MAE S.; BROWN, GORDON E.

    2010-01-01

    Mercury in the environment is of prime concern to both ecosystem and human health. Determination of the molecular-level speciation of Hg in soils and mine wastes is important for understanding its sequestration, mobility, and availability for methylation. Extended x-ray absorption fine structure (EXAFS) spectroscopy carried out under ambient P-T conditions has been used in a number of past studies to determine Hg speciation in complex mine wastes and associated soils. However, this approach cannot detect elemental (liquid) mercury in Hg-polluted soils and sediments due to the significant structural disorder of liquid Hg at ambient-temperature. A new sample preparation protocol involving slow cooling through the crystallization temperature of Hg(0) (234K) results in its transformation to crystalline α-Hg(0). The presence and proportion of Hg(0), relative to other crystalline Hg-bearing phases, in samples prepared in this way can be quantified by low-temperature (77K) EXAFS spectroscopy. Using this approach, we have determined the relative concentrations of liquid Hg(0) in Hg mine wastes from several sites in the California Coast Range and have found that they correlate well with measured fluxes of gaseous Hg released during light and dark exposure of the same samples, with higher evasion ratios from samples containing higher concentrations of liquid Hg(0). Two different linear relationships are observed in plots of the ratio of Hg emission under light and dark conditions vs. % Hg(0), corresponding to silica-carbonate- and hot springs-type Hg deposits, with the hot springs-type samples exhibiting higher evasion fluxes than silica-carbonate type samples at similar Hg(0) concentrations. Our findings help explain significant differences in Hg evasion data for different mine sites in the California Coast Range. PMID:21121657

  17. New technique for quantification of elemental hg in mine wastes and its implications for mercury evasion into the atmosphere

    USGS Publications Warehouse

    Jew, A.D.; Kim, C.S.; Rytuba, J.J.; Gustin, M.S.; Brown, Gordon E., Jr.

    2011-01-01

    Mercury in the environment is of prime concern to both ecosystem and human health. Determination of the molecular-level speciation of Hg in soils and mine wastes is important for understanding its sequestration, mobility, and availability for methylation. Extended X-ray absorption fine structure (EXAFS) spectroscopy carried out under ambient P-T conditions has been used in a number of past studies to determine Hg speciation in complex mine wastes and associated soils. However, this approach cannot detect elemental (liquid) mercury in Hg-polluted soils and sediments due to the significant structural disorder of liquid Hg at ambient-temperature. A new sample preparation protocol involving slow cooling through the crystallization temperature of Hg(0) (234 K) results in its transformation to crystalline ??-Hg(0). The presence and proportion of Hg(0), relative to other crystalline Hg-bearing phases, in samples prepared in this way can be quantified by low-temperature (77 K) EXAFS spectroscopy. Using this approach, we have determined the relative concentrations of liquid Hg(0) in Hg mine wastes from several sites in the California Coast Range and have found that they correlate well with measured fluxes of gaseous Hg released during light and dark exposure of the same samples, with higher evasion ratios from samples containing higher concentrations of liquid Hg(0). Two different linear relationships are observed in plots of the ratio of Hg emission under light and dark conditions vs % Hg(0), corresponding to silica-carbonate- and hot springs-type Hg deposits, with the hot springs-type samples exhibiting higher evasion fluxes than silica-carbonate type samples at similar Hg(0) concentrations. Our findings help explain significant differences in Hg evasion data for different mine sites in the California Coast Range. ?? 2011 American Chemical Society.

  18. PARTITIONING TRACERS FOR IN SITU DETECTION AND QUANTIFICATION OF DENSE NONAQUEOUS PHASE LIQUIDS IN GROUNDWATER SYSTEMS

    EPA Science Inventory

    The overall goal of the proposed project is to explore the use of partitioning tracers to characterize dense nonaqueous phase liquids (DNAPLs) in aquifer systems. Bulk-phase partitioning tracers will be investigated to detect and determine DNAPL saturation, while interface partit...

  19. Pressurized liquid extraction and quantification of anthocyanins in purple-fleshed sweetpotato genotypes

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Analysis of anthocyanins responsible for the purple flesh color is important for breeding programs and development of value-added products. This study aimed to optimize the conditions for anthocyanin extraction from purple-fleshed sweet potatoes (PFSP) using pressurized-liquid extraction (PLE) metho...

  20. Oak Ridge National Lebroatory Liquid&Gaseous Waste Treatment System Strategic Plan

    SciTech Connect

    Van Hoesen, S.D.

    2003-09-09

    Excellence in Laboratory operations is one of the three key goals of the Oak Ridge National Laboratory (ORNL) Agenda. That goal will be met through comprehensive upgrades of facilities and operational approaches over the next few years. Many of ORNL's physical facilities, including the liquid and gaseous waste collection and treatment systems, are quite old, and are reaching the end of their safe operating life. The condition of research facilities and supporting infrastructure, including the waste handling facilities, is a key environmental, safety and health (ES&H) concern. The existing infrastructure will add considerably to the overhead costs of research due to increased maintenance and operating costs as these facilities continue to age. The Liquid Gaseous Waste Treatment System (LGWTS) Reengineering Project is a UT-Battelle, LLC (UT-B) Operations Improvement Program (OIP) project that was undertaken to develop a plan for upgrading the ORNL liquid and gaseous waste systems to support ORNL's research mission.

  1. Heat transfer enhanced microwave process for stabilization of liquid radioactive waste slurry. Final report

    SciTech Connect

    White, T.L.

    1995-03-31

    The objectve of this CRADA is to combine a polymer process for encapsulation of liquid radioactive waste slurry developed by Monolith Technology, Inc. (MTI), with an in-drum microwave process for drying radioactive wastes developed by Oak Ridge National Laboratory (ORNL), for the purpose of achieving a fast, cost-effectve commercial process for solidification of liquid radioactive waste slurry. Tests performed so far show a four-fold increase in process throughput due to the direct microwave heating of the polymer/slurry mixture, compared to conventional edge-heating of the mixer. We measured a steady-state throughput of 33 ml/min for 1.4 kW of absorbed microwave power. The final waste form is a solid monolith with no free liquids and no free particulates.

  2. Distribution of aquifers, liquid-waste impoundments, and municipal water-supply sources, Massachusetts

    USGS Publications Warehouse

    Delaney, David F.; Maevsky, Anthony

    1980-01-01

    Impoundments of liquid waste are potential sources of ground-water contamination in Massachusetts. The map report, at a scale of 1 inch equals 4 miles, shows the idstribution of aquifers and the locations of municipal water-supply sources and known liquid-waste impoundments. Ground water, an important source of municipal water supply, is produced from shallow sand and gravel aquifers that are generally unconfined, less than 200 feet thick, and yield less than 2,000 gallons per minute to individual wells. These aquifers commonly occupy lowlands and stream valleys and are most extensive in eastern Massachusetts. Surface impoundments of liquid waste are commonly located over these aquifers. These impoundments may leak and allow waste to infiltrate underlying aquifers and alter their water quality. (USGS)

  3. Food waste within food supply chains: quantification and potential for change to 2050

    PubMed Central

    Parfitt, Julian; Barthel, Mark; Macnaughton, Sarah

    2010-01-01

    Food waste in the global food supply chain is reviewed in relation to the prospects for feeding a population of nine billion by 2050. Different definitions of food waste with respect to the complexities of food supply chains (FSCs)are discussed. An international literature review found a dearth of data on food waste and estimates varied widely; those for post-harvest losses of grain in developing countries might be overestimated. As much of the post-harvest loss data for developing countries was collected over 30 years ago, current global losses cannot be quantified. A significant gap exists in the understanding of the food waste implications of the rapid development of ‘BRIC’ economies. The limited data suggest that losses are much higher at the immediate post-harvest stages in developing countries and higher for perishable foods across industrialized and developing economies alike. For affluent economies, post-consumer food waste accounts for the greatest overall losses. To supplement the fragmentary picture and to gain a forward view, interviews were conducted with international FSC experts. The analyses highlighted the scale of the problem, the scope for improved system efficiencies and the challenges of affecting behavioural change to reduce post-consumer waste in affluent populations. PMID:20713403

  4. [Qualification and quantification of 10 sulfonamides in animal feedstuff by high performance liquid chromatography-electrospray tandem mass spectrometry].

    PubMed

    Qin, Yan; Zhang, Meijin; Lin, Haidan

    2005-07-01

    The presence of sulfonamide (SA) residues in foods is largely due to the raising of animals with sulfonamide antibiotics added or polluted feedstuff. Because of interference from the matrices, the commonly used immunoassay or chromatographic method is not suitable for the analysis of multi-SAs in feedstuff. A high performance liquid chromatographic-electrospray tandem mass spectrometric (HPLC/ESI-MS-MS) method has been established for the simultaneous determination of multi-SAs including sulfadiazine (SD), sulfapyridine (SPD), sulfamerazine (SM1), sulfameter (SM), sulfamethazine (SM2), sulfamethoxypyridazine (SMP), sulfamethoxazole (SMZ), sulfamonomethoxine (SMM), sulfadimethoxine (SDM) and sulfaquinoxaline (SQX). After solvent extraction, solid phase extraction, dilution and reversed-phase HPLC separation, SAs were detected by ESI-MS-MS under multi-reaction monitoring mode. The qualification analysis was done by using retention time and distribution of diagnostic ion pairs, and the quantification was based on the peak intensity of common fragment ion m/z 156. The limits of quantification for 10 SAs were 0.5 - 2.0 microg/kg (S/N = 10). The correlation coefficient of linear calibration curve was over 0.9995 within the SAs concentration range 2.0 - 200 microg/L except for SDM and SQX. At the spiked level of 1.0 mg/kg, the average recoveries for the 10 SAs were between 70% and 92%, the relative standard deviations were under 10% for intra-day and under 15% for inter-day. Routine tests showed the method was fast, sensitive, specific, and practical for the SAs determination in feedstuff. PMID:16250451

  5. Quantification of rifapentine, a potent antituberculosis drug, from dried blood spot samples using liquid chromatographic-tandem mass spectrometric analysis.

    PubMed

    Parsons, Teresa L; Marzinke, Mark A; Hoang, Thuy; Bliven-Sizemore, Erin; Weiner, Marc; Mac Kenzie, William R; Dorman, Susan E; Dooley, Kelly E

    2014-11-01

    The quantification of antituberculosis drug concentrations in multinational trials currently requires the collection of modest blood volumes, centrifugation, aliquoting of plasma, freezing, and keeping samples frozen during shipping. We prospectively enrolled healthy individuals into the Tuberculosis Trials Consortium Study 29B, a phase I dose escalation study of rifapentine, a rifamycin under evaluation in tuberculosis treatment trials. We developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for quantifying rifapentine in whole blood on dried blood spots (DBS) to facilitate pharmacokinetic/pharmacodynamic analyses in clinical trials. Paired plasma and whole-blood samples were collected by venipuncture, and whole blood was spotted on Whatman protein saver 903 cards. The methods were optimized for plasma and then validated for DBS. The analytical measuring range for quantification of rifapentine and its metabolite was 50 to 80,000 ng/ml in whole-blood DBS. The analyte was stable on the cards for 11 weeks with a desiccant at room temperature and protected from light. The method concordance for paired plasma and whole-blood DBS samples was determined after correcting for participant hematocrit or population-based estimates of bias from Bland-Altman plots. The application of either correction factor resulted in acceptable correlation between plasma and whole-blood DBS (Passing-Bablok regression corrected for hematocrit; y = 0.98x + 356). Concentrations of rifapentine may be determined from whole-blood DBS collected via venipuncture after normalization in order to account for the dilutional effects of red blood cells. Additional studies are focused on the application of this methodology to capillary blood collected by finger stick. The simplicity of processing, storage, shipping, and low blood volume makes whole-blood DBS attractive for rifapentine pharmacokinetic evaluations, especially in international and pediatric trials. PMID:25182637

  6. Localisation and quantification of benzalkonium chloride in eye tissue by TOF-SIMS imaging and liquid chromatography mass spectrometry.

    PubMed

    Desbenoit, Nicolas; Schmitz-Afonso, Isabelle; Baudouin, Christophe; Laprévote, Olivier; Touboul, David; Brignole-Baudouin, Françoise; Brunelle, Alain

    2013-05-01

    Benzalkonium (BAK) chloride is the most commonly used preservative in eye drops. It is generally composed of benzyldimethyldodecylammonium C12 and benzyldimethyltetradecylammonium C14 and is supposed to increase penetration of active compounds. However, numerous studies have reported its toxic effect to ocular surface especially in long-term treatments like against glaucoma, a sight-threatening disease. Albino rabbits were treated with a hyperosmolar solution and a high concentration of BAK solution for 1 month. Enucleated eyes were cryo-sectioned and analysed by mass spectrometry. Mass spectrometry imaging using time-of-flight secondary ion mass spectrometry (TOF-SIMS) has been used to characterize the spatial distribution and to determine the relative quantity of BAK at the surface of rabbit eye sections. Liquid chromatography coupled with mass spectrometry (LC-MS) using a hybrid linear ion trap-Orbitrap® mass spectrometer was used to obtain relative quantification of BAK at the sample surface. TOF-SIMS images of BAK ions indicated a distribution at the ocular surface and in deeper structures. Didecyldimethylammonium (DDMAC), which is used in hospitals as a substitute for BAK, was also detected and showed an accumulation around the eyes. After extraction with acetonitrile and chromatographic separation using a Gemini C18 column and an original elution gradient, the relative quantities of BAK and DDMAC present in the whole eye section surface were determined. This LC-MS method was validated in terms of limits of quantification, linearity, repeatability and reproducibility and its feasibility was evaluated in surgically obtained human samples. Specimens of iris, lens capsule or trabecular meshwork were found with significant levels of BAK and DDMAC, thus confirming the penetration of BAK in deep ocular structures, with potential deleterious effects induced by this cytotoxic compound. The analytical method developed here could therefore be of primary interest in

  7. Quantification of vincristine and its major metabolite in human plasma by high-performance liquid chromatography/tandem mass spectrometry.

    PubMed

    Dennison, Jennifer B; Renbarger, Jamie L; Walterhouse, David O; Jones, David R; Hall, Stephen D

    2008-06-01

    An analytical method using electrospray ionization and high-performance liquid chromatography/tandem mass spectrometry (LC/ESI-MS/MS) was developed to quantify vincristine and M1, the CYP3A-mediated metabolite of vincristine, in human plasma. Vinblastine (internal standard), vincristine, and M1 in plasma were extracted in methylene chloride after acidification with TCAA. The analytes were separated on an Inertsil ODS-3 C18 column (2.1 x 150 mm) with a 5-mum particle size using a gradient elution with a run time of 20 min. The initial mobile phase composition was 0.2% formic acid/water (80:20, v/v) with a final composition of 0.2% formic acid/water (20:80, v/v). Detection was accomplished with multiple reaction monitoring for vinblastine (m/z 406.3--> 271.7), vincristine (m/z 413.2--> 362.2), and M1 (m/z 397.3 --> 376.2). At three concentrations of vincristine and M1, the inter-day and intra-day accuracy and precision were within the acceptable limits for validation (106.8 +/- 9.6% for intra-day, n = 5 each concentration; 90.9 +/- 10.9% for inter-day, n = 4 each concentration). For both vincristine and M1, the concentration limits of quantification and detection were 12 pg/mL and 6 pg/mL, respectively. Stability studies indicated that 80% of M1 degraded in plasma after 15 hours at room temperature (n = 3, high and low QC concentrations). Therefore, short plasma processing times (<30 min) are recommended. The assay was used successfully to quantify vincristine and M1 in pediatric plasma samples up to 24 hours after vincristine administration. Vincristine and M1 concentrations were within the limits of quantification for all patient plasma samples. PMID:18520608

  8. Fast liquid chromatography-diode array detection assisted by chemometrics for quantification of seven ultraviolet filters in effluent wastewater.

    PubMed

    Vosough, Maryam; Mojdehi, Nahal Rahimdoost

    2011-09-30

    A fast chromatographic method is presented for simultaneous quantification of seven organic ultraviolet (UV) filters (benzophenone-3,4-methylbenzilidene camphor, octocrylene, 1-(4-tert-butylphenyl)-3-(4-methyoxyphenyl)1,3-propanedione), ethylhexyl methoxy cinnamate, ethylhexyl salicylate and homosalate) in effluent wastewater samples. The UV filters were pre-concentrated by Bond Elut-ENV cartridges and separated on an ODS column (15 cm × 0.46 cm, 5 μm) in less than 2.5 min using a non-aqueous mobile phase of methanol-acetonitrile (50:50, v/v) with flow-rate of 1.5 mL min(-1). Appropriate baseline correction through asymmetric least squares was applied to reduce the matrix of background signals in three way data. Then, second-order calibration based on multivariate curve resolution-alternating least squares (MCR-ALS) was implemented on the unfolded three-way data obtained from liquid chromatography with diode array detection (LC-DAD) through standard addition calibration method for handling co-eluted peaks, systematic and proportional errors. Recoveries ranging from 76% to 130% and %RSD values less than 11.2 for all UV filter shows the accuracy and precision of the proposed method in wastewater samples. In addition, statistical t-test as well as computed elliptical joint confidence region (EJCR) confirms the accuracy of the proposed method and indicates the absence of both constant and proportional errors in the predicted concentrations. This study demonstrates that coupling of the fast HPLC-DAD method with powerful algorithm of MCR-ALS can be considered as an efficient method for quantification of UV filters in highly contaminated samples of wastewaters where both time and cost per each analysis can be reduced significantly. PMID:21872075

  9. Quantification of Rifapentine, a Potent Antituberculosis Drug, from Dried Blood Spot Samples Using Liquid Chromatographic-Tandem Mass Spectrometric Analysis

    PubMed Central

    Parsons, Teresa L.; Marzinke, Mark A.; Hoang, Thuy; Bliven-Sizemore, Erin; Weiner, Marc; Mac Kenzie, William R.; Dorman, Susan E.

    2014-01-01

    The quantification of antituberculosis drug concentrations in multinational trials currently requires the collection of modest blood volumes, centrifugation, aliquoting of plasma, freezing, and keeping samples frozen during shipping. We prospectively enrolled healthy individuals into the Tuberculosis Trials Consortium Study 29B, a phase I dose escalation study of rifapentine, a rifamycin under evaluation in tuberculosis treatment trials. We developed a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for quantifying rifapentine in whole blood on dried blood spots (DBS) to facilitate pharmacokinetic/pharmacodynamic analyses in clinical trials. Paired plasma and whole-blood samples were collected by venipuncture, and whole blood was spotted on Whatman protein saver 903 cards. The methods were optimized for plasma and then validated for DBS. The analytical measuring range for quantification of rifapentine and its metabolite was 50 to 80,000 ng/ml in whole-blood DBS. The analyte was stable on the cards for 11 weeks with a desiccant at room temperature and protected from light. The method concordance for paired plasma and whole-blood DBS samples was determined after correcting for participant hematocrit or population-based estimates of bias from Bland-Altman plots. The application of either correction factor resulted in acceptable correlation between plasma and whole-blood DBS (Passing-Bablok regression corrected for hematocrit; y = 0.98x + 356). Concentrations of rifapentine may be determined from whole-blood DBS collected via venipuncture after normalization in order to account for the dilutional effects of red blood cells. Additional studies are focused on the application of this methodology to capillary blood collected by finger stick. The simplicity of processing, storage, shipping, and low blood volume makes whole-blood DBS attractive for rifapentine pharmacokinetic evaluations, especially in international and pediatric trials. PMID:25182637

  10. Quantification of L-ergothioneine in human plasma and erythrocytes by liquid chromatography-tandem mass spectrometry.

    PubMed

    Wang, Ling-Zhi; Thuya, Win-Lwin; Toh, Dorothy Su-Lin; Lie, Michael George-Limenta; Lau, Jie-Ying Amelia; Kong, Li-Ren; Wan, Seow-Ching; Chua, Kian-Ngiap; Lee, Edmund Jon-Deoon; Goh, Boon-Cher

    2013-03-01

    A sensitive analytical method has been developed and validated for the quantification of L-ergothioneine in human plasma and erythrocytes by liquid chromatography-tandem mass spectrometry. A commercially available isotope-labeled L-ergothioneine-d9 is used as the internal standard. A simple protein precipitation with acetonitrile is utilized for bio-sample preparation prior to analysis. Chromatographic separation of L-ergothioneine is conducted using gradient elution on Alltime C18 (150 mm × 2.1 mm, 5 µ). The run time is 6 min at a constant flow rate of 0.45 ml/min. The mass spectrometer is operated under a positive electrospray ionization condition with multiple reaction monitoring mode. The mass transitions of L-ergothioneine and L-ergothioneine-d9 are m/z 230 > 127 and m/z 239 > 127, respectively. Excellent linearity [coefficient of determination (r(2)) ≥ 0.9998] can be achieved for L-ergothioneine quantification at the ranges of 10 to 10,000 ng/ml, with the intra-day and inter-day precisions at 0.9-3.9% and 1.3-5.7%, respectively, and the accuracies for all quality control samples between 94.5 and 101.0%. This validated analytical method is suitable for pharmacokinetic monitoring of L-ergothioneine in human and erythrocytes. Based on the determination of bio-samples from five healthy subjects, the mean concentrations of L-ergothioneine in plasma and erythrocytes are 107.4 ± 20.5 ng/ml and 1285.0 ± 1363.0 ng/ml, respectively. PMID:23494799

  11. Peptides quantification by liquid chromatography with matrix-assisted laser desorption/ionization and selected reaction monitoring detection.

    PubMed

    Lesur, Antoine; Varesio, Emmanuel; Domon, Bruno; Hopfgartner, Gérard

    2012-10-01

    We present a novel analytical platform for peptides quantitative assays in biological matrices based on microscale liquid chromatography fractionation and matrix-assisted laser desorption/ionization mass spectrometric detection using the selected reaction monitoring (SRM) mode. The MALDI source was equipped with a high frequency Nd:YAG laser (1000 Hz) and mounted on a triple quadrupole/linear ion trap mass spectrometer (MALDI-QqQ(LIT)). Compared to conventional LC-ESI-SRM/MS, the separated analytes are "time-frozen" onto the MALDI plate in fractions, and navigation through the LC chromatogram makes it possible to perform SRM experiments as well as enhanced product ion spectra acquisition for confirmatory analyses without time constraints. The LC spots were analyzed using different rastering speeds ranging from 0.25 to 4 mm/sec with the shortest analysis time of 425 ms/spot. Since the LC runs can be multiplexed and do not need a comprehensive investigation, the present platform offers a valuable alternative to LC-ESI-SRM/MS for high throughput proteomic analyses. In addition, the derivatization of the N-terminal α-amino group by sulfonation was found to be key for the fragmentation of singly charged peptides under low collision energy regime. Under such conditions, y-ion series were observed in the MS/MS spectra, and thus the design of SRM experiments was greatly simplified. The quantitative performance of the platform was compared to that of LC-ESI-SRM/MS by spiking yeast tryptic peptides in human plasma digests. Both platforms exhibited similar sensitivities, accuracy (within ±20%) and precision (under 20%) in the relative quantification mode. As a proof of principle, the relative and absolute quantification of proteins associated with glycolysis, glyoxylate and tricarboxylic acid (TCA) cycles over a growth time course of Saccharomyces cerevisiae on glucose media was successfully performed using isotopic dilution. PMID:22897511

  12. Identification and quantification of ricin in biomedical samples by magnetic immunocapture enrichment and liquid chromatography electrospray ionization tandem mass spectrometry.

    PubMed

    Ma, Xiaoxi; Tang, Jijun; Li, Chunzheng; Liu, Qin; Chen, Jia; Li, Hua; Guo, Lei; Xie, Jianwei

    2014-08-01

    Ricin is a toxic protein derived from castor beans and composed of a cytotoxic A chain and a galactose-binding B chain linked by a disulfide bond, which can inhibit protein synthesis and cause cell death. Owing to its high toxicity, ease of preparation, and lack of medical countermeasures, ricin has been listed as both chemical and biological warfare agents. For homeland security or public safety, the unambiguous, sensitive, and rapid methods for identification and quantification of ricin in complicated matrices are of urgent need. Mass spectrometric analysis, which provides specific and sensitive characterization of protein, can be applied to confirm and quantify ricin. Here, we report a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) method in which ricin was extracted and enriched from serum by immunocapture using anti-ricin monoclonal antibody 3D74 linked to magnetic beads, then digested by trypsin, and analyzed by LC-ESI-MS/MS. Among 19 distinct peptides observed in LC-quadrupole/time of flight-MS (LC-QTOF-MS), two specific and sensitive peptides, T7A ((49)VGLPINQR(56)) and T14B ((188)DNCLTSDSNIR(198)), were chosen, and a highly sensitive determination of ricin was established in LC-triple quadrupole-MS (LC-QqQ-MS) operating in multiple reaction monitoring mode. These specific peptides can definitely distinguish ricin from the homologous protein Ricinus communis agglutinin (RCA120), even though the amino acid sequence homology of the A-chain of ricin and RCA120 is up to ca. 93% and that of B-chain is ca. 85%. Furthermore, peptide T7A was preferred in the quantification of ricin because its sensitivity was at least one order of magnitude higher than that of the peptide T14B. Combined with immunocapture enrichment, this method provided a limit of detection of ca. 2.5 ng/mL and the limit of quantification was ca. 5 ng/mL of ricin in serum, respectively. Both precision and accuracy of this method were determined and the RSD

  13. PROBABILITY BASED CORROSION CONTROL FOR LIQUID WASTE TANKS - PART III

    SciTech Connect

    Hoffman, E.; Edwards, T.

    2010-12-09

    The liquid waste chemistry control program is designed to reduce the pitting corrosion occurrence on tank walls. The chemistry control program has been implemented, in part, by applying engineering judgment safety factors to experimental data. However, the simple application of a general safety factor can result in use of excessive corrosion inhibiting agents. The required use of excess corrosion inhibitors can be costly for tank maintenance, waste processing, and in future tank closure. It is proposed that a probability-based approach can be used to quantify the risk associated with the chemistry control program. This approach can lead to the application of tank-specific chemistry control programs reducing overall costs associated with overly conservative use of inhibitor. Furthermore, when using nitrite as an inhibitor, the current chemistry control program is based on a linear model of increased aggressive species requiring increased protective species. This linear model was primarily supported by experimental data obtained from dilute solutions with nitrate concentrations less than 0.6 M, but is used to produce the current chemistry control program up to 1.0 M nitrate. Therefore, in the nitrate space between 0.6 and 1.0 M, the current control limit is based on assumptions that the linear model developed from data in the <0.6 M region is applicable in the 0.6-1.0 M region. Due to this assumption, further investigation of the nitrate region of 0.6 M to 1.0 M has potential for significant inhibitor reduction, while maintaining the same level of corrosion risk associated with the current chemistry control program. Ongoing studies have been conducted in FY07, FY08, FY09 and FY10 to evaluate the corrosion controls at the SRS tank farm and to assess the minimum nitrite concentrations to inhibit pitting in ASTM A537 carbon steel below 1.0 molar nitrate. The experimentation from FY08 suggested a non-linear model known as the mixture/amount model could be used to predict

  14. Quantification of ordering at a solid-liquid interface using plasmon electron energy loss spectroscopy

    SciTech Connect

    Gandman, Maria; Kauffmann, Yaron; Kaplan, Wayne D.

    2015-02-02

    We present an in situ electron energy loss spectroscopy (EELS) study of ordering of liquid Al at various Al-Al{sub 2}O{sub 3} interfaces. This technique utilizes precise measurements of the shifts in bulk plasmon resonance and their sensitivity to the valence electron density. Plasmon EELS combined with high resolution transmission electron microscopy provides information regarding the chemical composition in liquid Al at Al-Al{sub 2}O{sub 3} interfaces. Preferential oxygen segregation to the (0006) Al{sub 2}O{sub 3} plane was verified, and the (101{sup ¯}2) Al{sub 2}O{sub 3} plane was found to contain the lowest amount of segregated species.

  15. Data on subsurface storage of liquid waste near Pensacola, Florida, 1963-1980

    USGS Publications Warehouse

    Hull, R.W.; Martin, J.B.

    1982-01-01

    Since 1963, when industrial waste was first injected into the subsurface in northwest Florida, considerable data have been collected relating to the geochemistry of subsurface waste storage. This report presents hydrogeologic data on two subsurface waste storage. This report presents hydrogeologic data on two subsurface storage systems near Pensacola, Fla., which inject liquid industrial waste through deep wells into a saline aquifer. Injection sites are described giving a history of well construction, injection, and testing; geologic data from cores and grab samples; hydrographs of injection rates, volume, pressure, and water levels; and chemical and physical data from water-quality samples collected from injection and monitor wells. (USGS)

  16. Protein Quantification by Derivatization-Free High-Performance Liquid Chromatography of Aromatic Amino Acids

    PubMed Central

    Hesse, Almut

    2016-01-01

    Amino acid analysis is considered to be the gold standard for quantitative peptide and protein analysis. Here, we would like to propose a simple HPLC/UV method based on a reversed-phase separation of the aromatic amino acids tyrosine (Tyr), phenylalanine (Phe), and optionally tryptophan (Trp) without any derivatization. The hydrolysis of the proteins and peptides was performed by an accelerated microwave technique, which needs only 30 minutes. Two internal standard compounds, homotyrosine (HTyr) and 4-fluorophenylalanine (FPhe) were used for calibration. The limit of detection (LOD) was estimated to be 0.05 µM (~10 µg/L) for tyrosine and phenylalanine at 215 nm. The LOD for a protein determination was calculated to be below 16 mg/L (~300 ng BSA absolute). Aromatic amino acid analysis (AAAA) offers excellent accuracy and a precision of about 5% relative standard deviation, including the hydrolysis step. The method was validated with certified reference materials (CRM) of amino acids and of a pure protein (bovine serum albumin, BSA). AAAA can be used for the quantification of aromatic amino acids, isolated peptides or proteins, complex peptide or protein samples, such as serum or milk powder, and peptides or proteins immobilized on solid supports. PMID:27559481

  17. Protein Quantification by Derivatization-Free High-Performance Liquid Chromatography of Aromatic Amino Acids.

    PubMed

    Hesse, Almut; Weller, Michael G

    2016-01-01

    Amino acid analysis is considered to be the gold standard for quantitative peptide and protein analysis. Here, we would like to propose a simple HPLC/UV method based on a reversed-phase separation of the aromatic amino acids tyrosine (Tyr), phenylalanine (Phe), and optionally tryptophan (Trp) without any derivatization. The hydrolysis of the proteins and peptides was performed by an accelerated microwave technique, which needs only 30 minutes. Two internal standard compounds, homotyrosine (HTyr) and 4-fluorophenylalanine (FPhe) were used for calibration. The limit of detection (LOD) was estimated to be 0.05 µM (~10 µg/L) for tyrosine and phenylalanine at 215 nm. The LOD for a protein determination was calculated to be below 16 mg/L (~300 ng BSA absolute). Aromatic amino acid analysis (AAAA) offers excellent accuracy and a precision of about 5% relative standard deviation, including the hydrolysis step. The method was validated with certified reference materials (CRM) of amino acids and of a pure protein (bovine serum albumin, BSA). AAAA can be used for the quantification of aromatic amino acids, isolated peptides or proteins, complex peptide or protein samples, such as serum or milk powder, and peptides or proteins immobilized on solid supports. PMID:27559481

  18. Simultaneous quantification of carbamate insecticides in human plasma by liquid chromatography/tandem mass spectrometry.

    PubMed

    Mostafa, Ahmed; Medley, Gregory; Roberts, Darren M; Mohamed, Mosaad Sayed; Elshanawani, Abdalla A; Roberts, Michael S; Liu, Xin

    2011-08-01

    Carbofuran (CFN), carbosulfan (CSN) and fenobucarb (FBC) are carbamate pesticides that are widely used in gardening and agriculture for the control of insects. Human poisoning due to occupational or self-poisoning exposures is also reported, so assays are required to quantify the plasma concentration of these insecticides. An LC-MS/MS method was developed and validated for the simultaneous quantification of these three carbamate insecticides in the plasma of patients with acute intentional self-poisoning. Plasma samples were pretreated by acetonitrile for protein precipitation. Chromatography was carried out on a Luna C18(2) analytical column with gradient elution using a mobile phase containing acetonitrile and water with 10mM ammonium acetate. Mass spectrometric analysis was performed by an Applied Biosystems MDS Sciex API 2000 triple quadrupole mass spectrometer coupled with electrospray ionization (ESI) source in the positive ion mode. The total run time was 7 min. The assay was validated over a concentration range from 10 to 1000 ng/ml for CSN and FBC and 20-2000 ng/ml for CFN. The precision and accuracy for both intra- and inter-day determination of all analytes were acceptable (<15%). No significant matrix effect was observed. Stability of compounds was established for short term bench and autosampler storage as well as freeze/thaw cycles. The method was effectively applied to 270 clinical samples from patients with a history of acute intentional carbamate self-poisoning. PMID:21723210

  19. Quantification of chemical contaminants in the paper and board fractions of municipal solid waste.

    PubMed

    Pivnenko, K; Olsson, M E; Götze, R; Eriksson, E; Astrup, T F

    2016-05-01

    Chemicals are used in materials as additives in order to improve the performance of the material or the production process itself. The presence of these chemicals in recyclable waste materials may potentially affect the recyclability of the materials. The addition of chemicals may vary depending on the production technology or the potential end-use of the material. Paper has been previously shown to potentially contain a large variety of chemicals. Quantitative data on the presence of chemicals in paper are necessary for appropriate waste paper management, including the recycling and re-processing of paper. However, a lack of quantitative data on the presence of chemicals in paper is evident in the literature. The aim of the present work is to quantify the presence of selected chemicals in waste paper derived from households. Samples of paper and board were collected from Danish households, including both residual and source-segregated materials, which were disposed of (e.g., through incineration) and recycled, respectively. The concentration of selected chemicals was quantified for all of the samples. The quantified chemicals included mineral oil hydrocarbons, phthalates, phenols, polychlorinated biphenyls, and selected toxic metals (Cd, Co, Cr, Cu, Ni, and Pb). The results suggest large variations in the concentration of chemicals depending on the waste paper fraction analysed. Research on the fate of chemicals in waste recycling and potential problem mitigation measures should be focused on in further studies. PMID:26969284

  20. Process for immobilizing radioactive boric acid liquid wastes

    SciTech Connect

    Greenhalgh, W.O.

    1986-06-17

    A method is described for immobilizing radioactive boric acid waste solutions comprising: neutralizing a boric acid waste solution containing radionuclides with calcium hydroxide and forming a precipitate, evaporating the precipitate to near dryness, and firing the dry precipitate to form a calcium borate glass product containing the radionuclides.

  1. Time-of-flight direct recoil spectrometry: Application to liquid surfaces and steps toward quantification

    NASA Astrophysics Data System (ADS)

    Tassotto, Michael

    2001-08-01

    Liquid surfaces are very abundant in nature. Despite the importance of the liquid interface in general, experimental molecular-level data was almost completely lacking prior to the last decade and a half. The intent of this work is to provide a means by which experimental data on the composition of liquid surfaces and the average orientation of their constituent molecules can be obtained in order to supplement data from molecular dynamics and related computational techniques. To this end, a unique time-of-flight (TOF) spectrometer, which constitutes the backbone of a new method to study liquid surfaces, was constructed and commissioned. The performance of the spectrometer is demonstrated in a number of exemplary TOF spectra obtained from liquid glycerol. Moving from mere qualitative to quantitative surface analysis necessitates the ability to relate physical quantities such as detection efficiencies, accurate signal intensities, and interaction cross-sections for all elements to one another. As a first step, the absolute detection efficiency of a channel electron multiplier, used as particle detector in the spectrometer, was measured for the noble gas ions He+, Ar+, and Xe +. The data obtained led to an empirically derived, general expression of the detection efficiency that is applicable to particles of any atomic number. The results also show that the threshold velocity, below which a multiplier does not respond to impinging ions, cannot be regarded as independent of the ion's atomic number as previously reported in the literature. The second step involved a comprehensive investigation of ion-atom interactions and spectral features that are crucial for the processing of experimental signal intensities for quantitative analysis. For this purpose, the binary collision code MARLOWE was used in extensive trajectory calculations simulating TOF spectra. The simulation results confirm the high surface sensitivity of the technique and reveal the strong dependence of the

  2. Experimental quantification of a granular crater induced by a liquid-to-granular impact using a 3D scanner

    NASA Astrophysics Data System (ADS)

    Wyser, Emmanuel; Abellan, Antonio; Carrea, Dario; Rudaz, Benjamin; Jaboyedoff, Michel

    2015-04-01

    Granular impacts have been extensively studied but much remains to be investigated regarding the complex topic of liquid-to-granular impact. Its applications to Geosciences are of interest regarding recent advances in the investigation of the raindrop erosion or the sediment flux. In our study, we focus on the quantification of both the excavated and deposited volumes resulting from a water-droplet impact onto a fine granular. The quantification of the existing relationships between the impact energy, the packing fraction and the excavated volume is also of interest. Indeed, the relationship between the packing fraction and the excavated volume has still to be investigated for constant impact energy (fixed height of fall and droplet size). Moreover, the volume distribution of the granular matter around the impact target has still to be achieved regarding the previous studies. Much of the previous work was focused on the ejected particles distribution but less is known about the volume distribution of the ejected mass. In this study, we have developed a specific methodology in order to investigate these two topics, as follows: a) First of all, we carried out experimental investigations in laboratory on a setup inspired by the previous works of Long et al. (2014) and Furbish et al. (2007). Granular samples were prepared using a compaction device in order to produce various packing fractions. Pre- and post-impact surface geometries were recorded using a high precision 3D scanner (KONICA MINOLTA VIVID 9i). This provided an accurate point cloud of the impact crater and ejecta deposits. b) Afterwards, we processed each point cloud pairs using different softwares (PolyWorks & MATLAB). We used an accurate change detection method by computing orthogonal distance from points (post-geometry) to reference meshed surface (pre-geometry) to extract the points belonging to deposits (positive distance) or crater (negative distance). Then, we used the computational geometry toolbox

  3. Quantification of Dental Health Care Waste Generated among Private Dental Practices in Bengaluru City

    PubMed Central

    Krishnappa, Pushpanjali; Sreekantaiah, Pruthvish; Hiremath, S S; Thapsey, Hemanth; Shivraj, N S; Murthy, Nandagudi Srinavasa

    2015-01-01

    Background: Bengaluru, in India has more than 1148 practicing dentists for a population of 8.42 million. The amount and type of dental health care waste (DHCW) generated by the dental practitioners has to be assessed prior to chalking out and implementation of an effective DCHW management plan. Currently, there is no evidence available regarding the quantity, type, and method of disposal adopted by these practitioners. Hence, this study was conducted with the objective of estimating the quantity of DHCW by the private dental practitioners in Bengaluru city. Materials and Methods: The sample size was estimated to be 110. The sampling frame was constituted from the registered dental practitioners in Bengaluru with the Department of Health and Family Welfare, Govt. of Karnataka. Sampling strategy employed included a probability proportional sampling strategy for the four zones in Bengaluru followed by a simple random sampling of clinics from each zone. Standardized weight method was followed to estimate the quantity of different category of waste. Three data collectors who were trained and calibrated collected the information regarding the type and quantity of waste generated, the nature of practice and years of establishment. Results: Total quantity of waste generated was 0.161 kg/clinic/day with 0.130 kg and 0.026 kg of infectious and recyclables, respectively. The projected data for the actual number of private practices in Bengaluru city showed alarming figures of 41,535 kg and 8307 kg of infectious and recyclable waste being generated every year. Data also showed poor management practices of lead foil and plaster of paris and alarming figures projected annual quantity. Conclusion: The data demonstrated large quantities of hazardous waste generation and poor segregation practices of the practitioners. This warrants the immediate need for collective, voluntary measures to be initiated for appropriate and effective management of DHCW. PMID:26124606

  4. Accurate and reliable quantification of 25-hydroxy-vitamin D species by liquid chromatography high-resolution tandem mass spectrometry[S

    PubMed Central

    Liebisch, Gerhard; Matysik, Silke

    2015-01-01

    In general, mass spectrometric quantification of small molecules in routine laboratory testing utilizes liquid chromatography coupled to low mass resolution triple-quadrupole mass spectrometers (QQQs). Here we introduce high-resolution tandem mass spectrometry (quadrupole-Orbitrap) for the quantification of 25-hydroxy-vitamin D [25(OH)D], a marker of the vitamin D status, because the specificity of 25(OH)D immunoassays is still questionable and mass spectrometric quantification is becoming increasingly important. Liquid chromatography coupled to high-resolution tandem mass spectrometry (LC-MS/HR-MS) was used to quantify 25-hydroxy-cholecalciferol [25(OH)D3], 25-hydroxy-ergocalciferol [25(OH)D2], and their C3-epimers 3-epi-25(OH)D3 and 3-epi-25(OH)D2. The method has a run time of 5 min and was validated according to the US Food and Drug Administration and the European Medicines Agency guidelines. High mass resolution was advantageously applied to separate a quasi-isobaric interference of the internal standard D6-25(OH)D2 with 3-epi-25(OH)D3. All analytes showed an imprecision of below 10% coefficient of variation (CV), trueness between 90% and 110%, and limits of quantification below 10 nM. Concentrations measured by LC-MS/HR-MS are in good agreement with those of the National Institute of Standards and Technology reference methods using LC-MS/MS (QQQ). In conclusion, quantification of 25(OH)D by LC-MS/HR-MS is applicable for routine testing and also holds promise for highly specific quantification of other small molecules. PMID:25833687

  5. LABORATORY INVESTIGATION OF RESIDUAL LIQUID ORGANICS FROM SPILLS, LEAKS, AND THE DISPOSAL OF HAZARDOUS WASTES IN GROUNDWATER

    EPA Science Inventory

    Organic liquids that are essentially immiscible with water migrate through the subsurface under the influence of capillary, viscous, and buoyancy forces. These liquids originate from the improper disposal of hazardous wastes, and the spills and leaks of petroleum hydrocarbons a...

  6. Liquid and Gaseous Waste Operations Project Annual Operating Report CY 1999

    SciTech Connect

    Maddox, J.J.; Scott, C.B.

    2000-03-01

    A total of 5.77 x 10 7 gallons (gal) of liquid waste was decontaminated by the Process Waste Treatment Complex (PWTC) - Building 3544 ion exchange system during calendar year (CY) 1999. This averaged to 110 gpm throughout the year. An additional 3.94 x 10 6 gal of liquid waste (average of 8 gpm throughout the year) was decontaminated using the zeolite treatment system due to periods of high Cesium levels in the influent wastewater. A total of 6.17 x 10 7 gal of liquid waste (average of 118 gpm throughout the year) was decontaminated at Building 3544 during the year. During the year, the regeneration of the ion exchange resins resulted in the generation of 8.00 x 10 3 gal of Liquid Low-Level Waste (LLLW) concentrate and 9.00 x 10 2 gal of LLLW supernate. See Table 1 for a monthly summary of activities at Building 3544. Figure 1 shows a diagram of the Process Waste Collection and Transfer System and Figure 2 shows a diagram of the Building 3544 treatment process. Figures 3, 4 5, and 6 s how a comparison of operations at Building 3544 in 1997 with previous years. Figure 7 shows a comparison of annual rainfall at Oak Ridge National Laboratory (ORNL) since 1995.

  7. Treatment of Bottled Liquid Waste During Remediation of the Hanford 618-10 Burial Ground - 13001

    SciTech Connect

    Faulk, Darrin E.; Pearson, Chris M.; Vedder, Barry L.; Martin, David W.

    2013-07-01

    A problematic waste form encountered during remediation of the Hanford Site 618-10 burial ground consists of bottled aqueous waste potentially contaminated with regulated metals. The liquid waste requires stabilization prior to landfill disposal. Prior remediation activities at other Hanford burial grounds resulted in a standard process for sampling and analyzing liquid waste using manual methods. Due to the highly dispersible characteristics of alpha contamination, and the potential for shock sensitive chemicals, a different method for bottle processing was needed for the 618-10 burial ground. Discussions with the United States Department of Energy (DOE) and United States Environmental Protection Agency (EPA) led to development of a modified approach. The modified approach involves treatment of liquid waste in bottles, up to one gallon per bottle, in a tray or box within the excavation of the remediation site. Bottles are placed in the box, covered with soil and fixative, crushed, and mixed with a Portland cement grout. The potential hazards of the liquid waste preclude sampling prior to treatment. Post treatment verification sampling is performed to demonstrate compliance with land disposal restrictions and disposal facility acceptance criteria. (authors)

  8. Quantification of cortisol in human eccrine sweat by liquid chromatography - tandem mass spectrometry.

    PubMed

    Jia, Min; Chew, Wade M; Feinstein, Yelena; Skeath, Perry; Sternberg, Esther M

    2016-03-21

    Cortisol has long been recognized as the "stress biomarker" in evaluating stress related disorders. Plasma, urine or saliva are the current source for cortisol analysis. The sampling of these biofluids is either invasive or has reliability problems that could lead to inaccurate results. Sweat has drawn increasing attention as a promising source for non-invasive stress analysis. A sensitive HPLC-MS/MS method was developed for the quantitation of cortisol ((11β)-11,17,21-trihydroxypregn-4-ene-3,20-dione) in human eccrine sweat. At least one unknown isomer that has previously not been reported and could potentially interfere with quantification was separated from cortisol with mixed mode RP HPLC. Detection of cortisol was carried out using atmospheric pressure chemical ionization (APCI) and selected reaction monitoring (SRM) in positive ion mode, using cortisol-9,11,12,12-D4 as internal standard. LOD and LOQ were estimated to be 0.04 ng ml(-1) and 0.1 ng ml(-1), respectively. Linear range of 0.10-25.00 ng ml(-1) was obtained. Intraday precision (2.5%-9.7%) and accuracy (0.5%-2.1%), interday precision (12.3%-18.7%) and accuracy (7.1%-15.1%) were achieved. This method has been successfully applied to the cortisol analysis of human eccrine sweat samples. This is the first demonstration that HPLC-MS/MS can be used for the sensitive and highly specific determination of cortisol in human eccrine sweat in the presence of at least one isomer that has similar hydrophobicity as cortisol. This study demonstrated that human eccrine sweat could be used as a promising source for non-invasive assessment of stress biomarkers such as cortisol and other steroid hormones. PMID:26858998

  9. Quantification of melamine in drinking water and wastewater by micellar liquid chromatography.

    PubMed

    Beltrán-Martinavarro, Beatriz; Peris-Vicente, Juan; Rambla-Alegre, Maria; Marco-Peiró, Sergio; Esteve-Romero, Josep; Carda-Broch, Samuel

    2013-01-01

    Because of the large potential health impact caused by deliberate contamination with the synthetic chemical melamine of different products for human and animal consumption, the World Health Organization and the Food and Agriculture Organization of the United Nations provided a range of recommendations in order to facilitate obtaining needed data, among which was the determination of the background levels of melamine in drinking water and wastewater (December 4, 2008). A chromatographic procedure using a C18 column, a micellar mobile phase consisting of sodium dodecyl sulfate (0.1 M), and 1-propanol (7.5%) buffered at pH 3, and detection by absorbance at 210 nm is reported in this paper for the quantification of melamine in drinking water and wastewater. Samples were filtered and directly injected into the chromatographic system, thus avoiding an extraction procedure. The optimal mobile phase composition was obtained by a chemometrics approach that considered the retention factor, efficiency, and peak shape. Melamine was eluted in about 6.2 min without interferences. Validation was performed following U.S. Food and Drug Administration guidelines. The analytical parameters studied were linearity (0.03-5 microg/mL, R2 = 0.998), LOD (13 nglmL), intraday and interday accuracy (between 4.1 and 12.2%), intraday and interday precision (less than 14.8%), and robustness (RSD < 5.1% for retention time and <9.0% for area). The proposed methodology was successfully applied for analysis of local wastewater and drinking water, in which no melamine was found. PMID:24000762

  10. Assessment of Tank 241-S-112 Liquid Waste Mixing in Tank 241-SY-101

    SciTech Connect

    Onishi, Yasuo; Trent, Donald S.; Wells, Beric E.; Mahoney, Lenna A.

    2003-10-01

    The objectives of this study were to evaluate mixing of liquid waste from Tank 241-S-112 with waste in Tank 241-SY-101 and to determine the properties of the resulting waste for the cross-site transfer to avoid potential double-shell tank corrosion and pipeline plugging. We applied the time-varying, three-dimensional computer code TEMPEST to Tank SY-101 as it received the S-112 liquid waste. The model predicts that temperature variations in Tank SY-101 generate a natural convection flow that is very slow, varying from about 7 x 10{sup -5} to 1 x 10{sup -3} ft/sec (0.3 to about 4 ft/hr) in most areas. Thus, natural convection would eventually mix the liquid waste in SY-101 but would be very slow to achieve nearly complete mixing. These simulations indicate that the mixing of S-112 and SY-101 wastes in Tank SY-101 is a very slow process, and the density difference between the two wastes would further limit mixing. It is expected to take days or weeks to achieve relatively complete mixing in Tank SY-101.

  11. On-line desalting and carbohydrate analysis for immobilized enzyme hydrolysis of waste cellulosic biomass by column-switching high-performance liquid chromatography.

    PubMed

    Cheng, Cheanyeh; Chen, Chi-Sung; Hsieh, Pei-Hsin

    2010-04-01

    An innovative green column-switching high-performance liquid chromatographic (HPLC) technique was developed by coupling traditional and Pb(2+) ion-exclusion columns to study enzyme hydrolysis components of waste cellulosic biomass. Pure water was used as the mobile phase to separate neutral polar analytes in high salt content solution. The column-switching HPLC-RI was connected on-line to the immobilized enzyme reactor for successive on-line desalting and simultaneous analysis of six carbohydrates (cellobiose, glucose, xylose, galactose, mannose, and arabinose) in the hydrolysate of waste paper and waste tree branch by incorporating the heart-cut and the elution-time-difference techniques. Six internal standard calibration curves in the linear concentration range of 0-2,000 microg mL(-1) were prepared. Xylitol was used as the internal standard to give excellent linear correlation coefficients (0.9984-0.9999). The limits of detection and quantification for cellobiose, glucose, xylose, galactose, mannose, and arabinose varied between 0.12-4.88 and 0.40-16.3 microg mL(-1), respectively, with an accuracy of 90-102% and a precision of 0.1-7.8%. Cellulose and hemicellulose contents were higher in waste paper than in waste tree branch. PMID:20181346

  12. Differentiated quantification of human bile acids in serum by high-performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Burkard, Ines; von Eckardstein, Arnold; Rentsch, Katharina M

    2005-11-01

    Determination of quantitative changes in the pattern of serum bile acids is important for the monitoring of diseases affecting bile acid metabolism. A sensitive and specific high-performance liquid chromatography (HPLC)-MS/MS method was developed for the differentiated quantification of unconjugated as well as glycine- and taurine-conjugated cholic, chenodeoxycholic (CDCA), deoxycholic (DCA), ursodeoxycholic (UDCA) and lithocholic acid (LCA) in serum samples. After solid-phase extraction and reversed-phase HPLC separation, detection of the conjugated bile acids was performed using electrospray ionization (ESI)-MS/MS and selected reaction monitoring mode, whereas unconjugated bile acids were determined by ESI-MS and selected ion monitoring mode. The within-day and between-day coefficients of variation were below 7% for all bile acids and the recovery rates of the extraction procedure were between 84.9 and 105%. The developed method was applied to a group of 21 healthy volunteers and preliminary reference intervals in serum were established. In patients with drug-induced cholestasis, an elevation of primary bile acids has been shown. PMID:16182619

  13. Optimized ultra performance liquid chromatography tandem high resolution mass spectrometry method for the quantification of paraquat in plasma and urine.

    PubMed

    Lu, Haihua; Yu, Jing; Wu, Linlin; Xing, Jingjing; Wang, Jun; Huang, Peipei; Zhang, Jinsong; Xiao, Hang; Gao, Rong

    2016-08-01

    A simple, sensitive and specific ultra performance liquid chromatography coupled to electrospray tandem high resolution mass spectrometry (UPLC-ESI-HRMS/MS) method has been developed and validated for quantification of paraquat in plasma and urine. The sample preparation was carried out by one-step protein precipitation with acetonitrile. The paraquat was separated with a HILIC column in 10min. Detection was performed using Q Exactive Orbitrap mass spectrometer by Targeted-MS/MS scan mode. Methodological parameters, such as ammonium formate concentration, formic acid concentration, spray voltage, capillary temperature, heater temperature and normalized collision energy were optimized to achieve the highest sensitivity. The calibration curve was linear over the concentration range of LOQ-1000ng/mL. LOD was 0.1 and 0.3ng/mL, LOQ was 0.3 and 0.8ng/mL for urine and plasma, respectively. The intra- and inter-day precisions were <7.97% and 4.78% for plasma and urine. The accuracies were within the range 93.51-100.90%. The plasma and urine matrices had negligible relative matrix effect in this study. This method was successfully applied to determine paraquat concentration in plasma samples with hemoperfusion from 5 suspected paraquat poisoning patients. PMID:27270261

  14. Quantification of monosaccharides through multiple-reaction monitoring liquid chromatography/mass spectrometry using an aminopropyl column.

    PubMed

    Hammad, Loubna A; Derryberry, Dakota Z; Jmeian, Yazen R; Mechref, Yehia

    2010-06-15

    A simple, sensitive, and reproducible quantitative liquid chromatography/tandem mass spectrometry (LC/MS/MS) method was designed for the simultaneous quantification of monosaccharides derived from glycoprotein and blood serum using a multiple-reaction monitoring (MRM) approach. Sialic acids and neutral monosaccharides were efficiently separated using an amino-bonded silica phase column. Neutral monosaccharide molecules were detected as their aldol acetate anion adducts [M + CH(3)CO(2)](-) using electrospray ionization in negative ion MRM mode, while sialic acids were detected as deprotonated ions [M-H](-). The new method did not require a reduction step, and exhibited very high sensitivity to carbohydrates with limits of detection of 1 pg for the sugars studied. The linearity of the described approach spanned over three orders of magnitude (pg to ng). The method was validated for monosaccharides originating from N-linked glycans attached to glycoproteins and glycoproteins found in human blood serum. The method effectively quantified monosaccharides originating from as little as 1 microg of glycoprotein and 5 microL of blood serum. The method was robust, reproducible, and highly sensitive. It did not require reduction, derivatization or postcolumn addition of reagents. PMID:20486252

  15. Interferon-alpha 2b quantification in inclusion bodies using reversed phase-ultra performance liquid chromatography (RP-UPLC).

    PubMed

    Cueto-Rojas, H F; Pérez, N O; Pérez-Sánchez, G; Ocampo-Juárez, I; Medina-Rivero, E

    2010-04-15

    Interferon-alpha 2b (IFN-alpha 2b) is a recombinant therapeutic cytokine produced as inclusion bodies using a strain of Escherichia coli as expression system. After fermentation and recovery, it is necessary to know the amount of recombinant IFN-alpha 2b, in order to determine the yield and the load for solubilization, and chromatographic protein purification steps. The present work details the validation of a new short run-time and fast sample-preparation method to quantify IFN-alpha 2b in inclusion bodies using Reversed Phase-Ultra Performance Liquid Chromatography (RP-UPLC). The developed method demonstrated an accuracy of 100.28%; the relative standard deviations for method precision, repeatability and inter-day precision tests were found to be 0.57%, 1.54% and 1.83%, respectively. Linearity of the method was assessed in the range of concentrations from 0.05 mg/mL to 0.5 mg/mL, the curve obtained had a determination coefficient (r(2)) of 0.9989. Detection and quantification limits were found to be 0.008 mg/mL and 0.025 mg/mL, respectively. The method also demonstrated robustness for changes in column temperature, and specificity against host proteins and other recombinant protein expressed in the same E. coli strain. PMID:20299292

  16. Quantification of atrazine, phenylurea, and sulfonylurea herbicide metabolites in urine by high-performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Nguyen, Johnny V; Olsson, Anders O; Bravo, Roberto; Needham, Larry L; Barr, Dana B

    2007-05-01

    We developed a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS-MS) method to measure metabolites of atrazine, phenylurea, and sulfonylurea herbicides in human urine. The metabolites measured in the method include atrazine mercapturate, desethyl atrazine, and desisopropyl atrazine as markers of atrazine exposure; dichlorophenyl urea, dichlorophenylmethyl urea, diuron, and linuron as markers of phenylurea herbicide exposure; and dimethoxypyrimidine, dimethylpyrimidine, and methoxymethyl triazine as markers for sulfonylurea herbicide exposure. The metabolites were extracted from urine by simple solid-phase extraction using a mixed-bed cartridge and were analyzed by HPLC-MS-MS. Quantification of the atrazine metabolites was achieved using isotope-dilution calibration. The remaining metabolites were quantified using similarly structured chemicals as internal standards. Extraction recoveries ranged from 88% to 104% (n = 5). Limits of detection for the entire method ranged from 0.125 to 1 ng/mL, and the average relative standard deviation of repeat measurements was about 13% (n = 30). PMID:17555640

  17. Quantification of nardosinone in rat plasma using liquid chromatography-tandem mass spectrometry and its pharmacokinetics application.

    PubMed

    Lu, Zhihe; Zhou, Peng; Zhan, Yuzhu; Su, Jingrong; Yi, Deliang

    2015-01-01

    A rapid, sensitive and high-throughput liquid chromatography-tandem mass spectrometry (LC-MS-MS) method was established and validated to assay the concentration of nardosinone, a main active compound isolated from Nardostachys chinensis, in rat plasma. Plasma samples were processed by protein precipitation with acetonitrile and separated on a Venusil MP-C18 column (50 × 2.1 mm, 5 µm) at an isocratic flow rate of 0.6 mL/min using methanol-0.1% formic acid in water (55 : 45, v/v) as mobile phase, and total run time was 2.5 min. MS-MS detection was accomplished in selected reaction monitoring mode with positive electrospray ionization. The calibration curve was linear over the concentration range of 9.60-320 ng/mL with lower limit of quantification of 9.60 ng/mL. The intra- and inter-day precisions were below 12.3% in terms of relative standard deviation, and the accuracy was within ±9.0% in terms of relative error. Extraction recovery, matrix effect and stability were also satisfactory in rat plasma. The developed method was successfully applied to a pharmacokinetic study of nardosinone following an intravenous injection at a dose of 1.04 mg/kg to Sprague-Dawley rats. PMID:26116832

  18. A reversed-phase high performance liquid chromatography method for quantification of methotrexate in cancer patients serum.

    PubMed

    Li, Yuan-dong; Li, Yan; Liang, Ning-sheng; Yang, Fan; Kuang, Zhi-peng

    2015-10-01

    A simple, rapid and sensitive reversed-phase high performance liquid chromatography (HPLC) method has been developed for the determination of methotrexate in human serum. After deproteinization of the serum with 40% silver nitrate solution, methotrexate and internal standard (IS) were separated on a reversed-phase column with a mobile phase consisting of 10mM sodium phosphate buffer (pH6.40)-methanol (78:22%, v/v) and ultraviolet detection at 310nm. The linearity is evaluated by a calibration curve in the concentration range of 0.05-10.0μg/mL and presented a correlation coefficient of 0.9995. The absolute recoveries were 97.52±3.9% and 96.87±3.7% for methotrexate and ferulic acid (internal standard), respectively. The intra- and inter-day precision were less 6.19 and 5.89%, respectively (n=6). The limit of quantitation was 0.02μg/mL and the limit of detection was 0.006μg/mL. The complete analysis was achieved less than 10min with no interference from endogenous components or 22 examined drugs. This method was validated by using serum samples from high-dose methotrexate treated patients with osteosarcoma, breast cancer, acute leukemia and lymphoma. The method was demonstrated to be a simple, rapid and reliable approach in quantification of methotrexate in serum samples from patients with high-dose methotrexate therapy. PMID:26319303

  19. Quantification of triazine herbicides in soil by microwave-assisted extraction and high-performance liquid chromatography.

    PubMed

    Shah, Jasmin; Rasul Jan, M; Ara, Behisht; Shehzad, Farhat-Un-Nisa

    2011-07-01

    A method for the determination of herbicides residues, triazine (atrazine, metribuzin, ametryn, and terbutryn), in soil samples with high-performance liquid chromatography (HPLC)-UV detection is described. The proposed method is based on microwave-assisted extraction (MAE) of soil samples for 4 min at 80% of 850-W magnetron outputs in the presence of mixture of solvents (methanol/acetonitrile/ethylacetate). Related important factors influencing the MAE efficiency, such as the solvent type and volume, irradiation energy, and time, were optimized in detail. Calibration curve ranges established using HPLC for metribuzin, atrazine, ametryn, and terbutryn are 1.0-19.0, 0.9-18.0, 0.6-11.0, and 0.7-11.0 µg mL( -1), respectively. The limits of detection of metribuzin, atrazine, ametryn, and terbutryn are 0.30, 0.24, 0.16, and 0.20 µg mL( -1) while limits of quantification are 1.0, 0.80, 0.50, and 0.60 µg mL( -1), respectively. A Plackett-Burman factorial design was used as a screening method in order to select the variables that influence MAE extraction. The recoveries of the method at three different spiked levels were assessed by analyzing real soil samples and were found to be in the range of 83.33 ± 0.12-96.33 ± 0.23 with good precision (<8%). PMID:20824333

  20. High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

    NASA Astrophysics Data System (ADS)

    Duyck, Christiane Béatrice; Saint'Pierre, Tatiana Dillenburg; Miekeley, Norbert; da Fonseca, Teresa Cristina Oliveira; Szatmari, Peter

    2011-05-01

    A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 μg L - 1 and 8 μg L - 1 . The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

  1. Simultaneous quantification of related substances of perindopril tert-butylamine using a novel stability indicating liquid chromatographic method.

    PubMed

    Szabó, Zoltán-István; Réti, Zenkő-Zsuzsánna; Gagyi, László; Kis, Erika Lilla; Sipos, Emese

    2015-03-01

    A novel stability indicating gradient reverse-phased high-performance liquid chromatographic method has been developed for the quantification of impurities of perindopril tert-butylamine (PER) in pharmaceutical dosage form. Separation of the active substance and its known (Impurities B, C, D, E, F) and unknown impurities was achieved on a BDS Hypersil C18 column (250 mm × 4.6 mm, 5 µm), thermostated at 70°C, using a mobile phase comprised of aqueous solution of sodium 1-heptanesulfonate adjusted to pH 2 with perchloric acid and acetonitrile. The flow rate was maintained at 1.5 mL min(-1), injection volume of 20 µL was utilized and detection of analytes was performed at 215 nm. The developed method was validated in accordance with current ICH Guidelines for all suggested parameters, including forced degradation studies and proved to be linear, accurate, precise and suitable for the impurity testing of PER, being subsequently applied during on-going stability studies of a newly developed generic formulation. PMID:25616989

  2. US and Russian innovative technologies to process low-level liquid radioactive wastes: The Murmansk initiative

    SciTech Connect

    Dyer, R.S.; Penzin, R.; Duffey, R.B.; Sorlie, A.

    1996-12-31

    This paper documents the status of the technical design for the upgrade and expansion to the existing Low-level Liquid Radioactive Waste (LLLRW) treatment facility in Murmansk, the Russian Federation. This facility, owned by the Ministry of Transportation and operated by the Russian company RTP Atomflot in Murmansk, Russia, has been used by the Murmansk Shipping Company (MSCo) to process low-level liquid radioactive waste generated by the operation of its civilian icebreaker fleet. The purpose of the new design is to enable Russia to permanently cease the disposal at sea of LLLRW in the Arctic, and to treat liquid waste and high saline solutions from both the Civil and North Navy Fleet operations and decommissioning activities. Innovative treatments are to be used in the plant which are discussed in this paper.

  3. Calculation of chemical quantities for the radioactive liquid waste treatment facility

    SciTech Connect

    Del Signore, John C.; McClenahan, Robert L.

    2007-03-01

    The Radioactive Liquid Waste Treatment Facility (RLWTF) receives, stores, and treats both low-level and transuranic radioactive liquid wastes (RLW). Treatment of RLW requires the use of different chemicals. Examples include the use of calcium oxide to precipitate metals and radioactive elements from the radioactive liquid waste, and the use of hydrochloric acid to clean membrane filters that are used in the treatment process. The RL WTF is a Hazard Category 2 nuclear facility, as set forth in the LANL Final Safety Analysis Report of October 1995, and a DOE letter of March 11, 1999. A revised safety basis is being prepared for the RLWTF, and will be submitted to the NNSA in early 2007. This set of calculations establishes maximum chemical quantities that will be used in the 2007 safety basis.

  4. Selective identification and quantification of saccharin by liquid chromatography and fluorescence detection.

    PubMed

    Bruno, Sergio N F; Cardoso, Carlos R; Maciel, Márcia Mosca A; Vokac, Lidmila; da Silva Junior, Ademário I

    2014-09-15

    High-pressure liquid chromatography with ultra-violet detection (HPLC-UV) is one of the most commonly used methods to identify and quantify saccharin in non-alcoholic beverages. However, due to the wide variety of interfering UV spectra in saccharin-containing beverage matrices, the same method cannot be used to measure this analyte accurately. We have developed a new, highly effective method to identify and quantify saccharin using HPLC with fluorescence detection (HPLC-FLD). The excitation wavelength (250 nm) and emission wavelength (440 nm) chosen increased selectivity for all matrices and ensured few changes were required in the mobile phase or other parameters. The presence of saccharin in non-diet beverages - a fraud commonly used to replace more expensive sucrose - was confirmed by comparing coincident peaks as well as the emission spectra of standards and samples. PMID:24767060

  5. Proceedings of waste stream minimization and utilization innovative concepts: An experimental technology exchange. Volume 2, Industrial liquid waste processing, industrial gaseous waste processing

    SciTech Connect

    Lee, V.E.; Watts, R.L.

    1993-04-01

    This two-volume proceedings summarize the results of fifteen innovations that were funded through the US Department of Energy`s Innovative Concept Program. The fifteen innovations were presented at the sixth Innovative Concepts Fair, held in Austin, Texas, on April 22--23, 1993. The concepts in this year`s fair address innovations that can substantially reduce or use waste streams. Each paper describes the need for the proposed concept, the concept being proposed, and the concept`s economics and market potential, key experimental results, and future development needs. The papers are divided into two volumes: Volume 1 addresses innovations for industrial solid waste processing and municipal waste reduction/recycling, and Volume 2 addresses industrial liquid waste processing and industrial gaseous waste processing. Individual reports are indexed separately.

  6. FY 1995 separation studies for liquid low-level waste treatment at Oak Ridge National Laboratory

    SciTech Connect

    Bostick, D.T.; Arnold, W.D.; Burgess, M.W.

    1995-01-01

    During FY 1995, studies were continued to develop improved methods for centralized treatment of liquid low-level waste (LLLW) at Oak Ridge National Laboratory (ORNL). Focus in this reporting period was on (1) identifying the parameters that affect the selective removal of {sup 90}Sr and {sup 137}Cs, two of the principal radioactive contaminants expected in the waste; (2) validating the effectiveness of the treatment methods by testing an ac Melton Valley Storage Tank (MVST) supernate; (3) evaluating the optimum solid/liquid separation techniques for the waste; (4) identifying potential treatment methods for removal of technetium from LLLW; and (5) identifying potential methods for stabilizing the high-activity secondary solid wastes generated by the treatment.

  7. Quantification of the resource recovery potential of municipal solid waste incineration bottom ashes.

    PubMed

    Allegrini, Elisa; Maresca, Alberto; Olsson, Mikael Emil; Holtze, Maria Sommer; Boldrin, Alessio; Astrup, Thomas Fruergaard

    2014-09-01

    Municipal solid waste incineration (MSWI) plays an important role in many European waste management systems. However, increasing focus on resource criticality has raised concern regarding the possible loss of critical resources through MSWI. The primary form of solid output from waste incinerators is bottom ashes (BAs), which also have important resource potential. Based on a full-scale Danish recovery facility, detailed material and substance flow analyses (MFA and SFA) were carried out, in order to characterise the resource recovery potential of Danish BA: (i) based on historical and experimental data, all individual flows (representing different grain size fractions) within the recovery facility were quantified, (ii) the resource potential of ferrous (Fe) and non-ferrous (NFe) metals as well as rare earth elements (REE) was determined, (iii) recovery efficiencies were quantified for scrap metal and (iv) resource potential variability and recovery efficiencies were quantified based on a range of ashes from different incinerators. Recovery efficiencies for Fe and NFe reached 85% and 61%, respectively, with the resource potential of metals in BA before recovery being 7.2%ww for Fe and 2.2%ww for NFe. Considerable non-recovered resource potential was found in fine fraction (below 2mm), where approximately 12% of the total NFe potential in the BA were left. REEs were detected in the ashes, but the levels were two or three orders of magnitude lower than typical ore concentrations. The lack of REE enrichment in BAs indicated that the post-incineration recovery of these resources may not be a likely option with current technology. Based on these results, it is recommended to focus on limiting REE-containing products in waste for incineration and improving pre-incineration sorting initiatives for these elements. PMID:24889793

  8. A column-switching method for quantification of the enantiomers of omeprazole in native matrices of waste and estuarine water samples.

    PubMed

    Barreiro, Juliana Cristina; Vanzolini, Kenia Lourenço; Madureira, Tânia Vieira; Tiritan, Maria Elizabeth; Cass, Quezia Bezerra

    2010-06-30

    This work reports the use of a two-dimensional liquid chromatography (2D-LC) system for quantification of the enantiomers of omeprazole in distinct native aqueous matrices. An octyl restricted-access media bovine serum albumin column (RAM-BSA C(8)) was used in the first dimension, while a polysaccharide-based chiral column was used in the second dimension with either ultraviolet (UV-vis) or ion-trap tandem mass spectrometry (IT-MS/MS) detection. An in-line configuration was employed to assess the exclusion capacity of the RAM-BSA columns to humic substances. The excluded macromolecules had a molecular mass in the order of 18 kDa. Good selectivity, extraction efficiency, accuracy, and precision were achieved employing a very small amount (500 microL or 1.00 mL) of native water sample per injection, with detection limits of 5.00 microg L(-1), using UV-vis, and 0.0250 microg L(-1), using IT-MS/MS. The total analysis time was only 35 min, with no time spent on sample preparation. The methods were successfully applied to analyze a series of waste and estuarine water samples. The enantiomers were detected in an estuarine water sample collected from the Douro River estuary (Portugal) and in an influent sample from the wastewater treatment plant (WWTP) of São Carlos (Brazil). As far as we are concerned, this is the first report of the occurrence of (+)-omeprazole and (-)-omeprazole in native aqueous matrices. PMID:20685482

  9. Household hazardous waste quantification, characterization and management in China's cities: a case study of Suzhou.

    PubMed

    Gu, Binxian; Zhu, Weimo; Wang, Haikun; Zhang, Rongrong; Liu, Miaomiao; Chen, Yangqing; Wu, Yi; Yang, Xiayu; He, Sheng; Cheng, Rong; Yang, Jie; Bi, Jun

    2014-11-01

    A four-stage systematic tracking survey of 240 households was conducted from the summer of 2011 to the spring of 2012 in a Chinese city of Suzhou to determine the characteristics of household hazardous waste (HHW) generated by the city. Factor analysis and a regression model were used to study the major driving forces of HHW generation. The results indicate that the rate of HHW generation was 6.16 (0.16-31.74, 95% CI) g/person/day, which accounted for 2.23% of the household solid waste stream. The major waste categories contributing to total HHW were home cleaning products (21.33%), medicines (17.67%) and personal care products (15.19%). Packaging and containers (one-way) and products (single-use) accounted for over 80% of total HHW generation, implying a considerable potential to mitigate HHW generation by changing the packaging design and materials used by manufacturing enterprises. Strong correlations were observed between HHW generation (g/person/day) and the driving forces group of "household structure" and "consumer preferences" (among which the educational level of the household financial manager has the greatest impact). Furthermore, the HHW generation stream in Suzhou suggested the influence of another set of variables, such as local customs and culture, consumption patterns, and urban residential life-style. This study emphasizes that HHW should be categorized at its source (residential households) as an important step toward controlling the HHW hazards of Chinese cities. PMID:25022547

  10. Handling of liquid radioactive wastes produced during the decommissioning of nuclear-powered submarines

    SciTech Connect

    Martynov, B.V.

    1995-10-01

    Liquid radioactive wastes are produced during the standard decontamination of the reactor loop and liquidation of the consequences of accidents. In performing the disassembly work on decommissioned nuclear-powered submarines, the equipment must first be decontaminated. All this leads to the formation of a large quantity of liquid wastes with a total salt content of more then 3l-5 g/liter and total {beta}-activity of up to 1 {center_dot}10{sup {minus}4} Ci/liter. One of the most effective methods for reprocessing these wastes - evaporation - has limitations: The operating expenses are high and the apparatus requires expensive alloyed steel. The methods of selective sorption of radionuclides on inorganic sorbents are used for reprocessing liquid wastes form the nuclear-powered fleet. A significant limitation of the method is the large decrease in sorption efficiency with increasing total salt-content of the wastes. In some works, in which electrodialysis is used for purification of the salt wastes, the total salt content can be decreased by a factor of 10-100 and the same quantity of radionuclides can be removed. We have developed an electrodialysis-sorption scheme for purifying salt wastes that makes it possible to remove radionuclides to the radiation safety standard and chemically harmful substances to the health standards. The scheme includes electrodialysis desalinization (by 90% per pass on the EDMS apparatus), followed by additional purification of the diluent on synthetic zeolites and electro-osmotic concentration (to 200-250 g/liter on the EDK apparatus). The secondard wastes---salt concentrates and spent sorbents---are solidified. (This is the entire text of the article.)

  11. Microbial consortium role in processing liquid waste of vegetables in Keputran Market Surabaya as organic liquid fertilizer ferti-plus

    NASA Astrophysics Data System (ADS)

    Rizqi, Fauziah; Supriyanto, Agus; Lestari, Intan; Lita Indri D., L.; Elmi Irmayanti, A.; Rahmaniyah, Fadilatur

    2016-03-01

    Many activities in this market is directly proportional to increase production of vegetables waste, especially surabaya. Therefore, in this study aims to utilize liquid waste of vegetables into liquid organic fertilizer by mixing microbial consorsium. The microbial consorsium consist of Azotobacter chrococcum, Azospirillum brasilense, Rhizobium leguminosarum, Bacillus subtilis, Bacillus megaterium, Pseudomonas putida, and Pseudomonas fluorescens. Ttreatment of microbial concentrations (5%, 10%, 15%) and the length of the incubation period (7 days, 14 days, 21 days) used in this research. The parameters used are: C/N ratio, levels of CNP, and BOD value. This study uses a standard organic fertilizer value according SNI19-7030-2004, The results show the value of C/N ratio comply with the ISO standards. C levels showed an increase during the incubation period but not compare with standards. N levels that compare with standards are microbial treatment in all group concentration except control group with an incubation period of 21 days is > 7. P levels compare with the existing standards in the group of microbe concentration of 10% and 15% during the incubation period. The value of the initial BOD liquid waste of vegetable is 790.25 mg / L, this value indicates that the waste should not go into the water body. Accordingly, the results of this study can not be used as a liquid organic fertilizer, but potentially if it is used as a natural career or build natural soil. The Building natural soil is defined as the natural ingredients that can be used to improve soil properties.

  12. Method for the simultaneous recovery of radionuclides from liquid radioactive wastes using a solvent

    DOEpatents

    Romanovskiy, Valeriy Nicholiavich; Smirnov, Igor V.; Babain, Vasiliy A.; Todd, Terry A.; Brewer, Ken N.

    2001-01-01

    The present invention relates to solvents, and methods, for selectively extracting and recovering radionuclides, especially cesium and strontium, rare earths and actinides from liquid radioactive wastes. More specifically, the invention relates to extracting agent solvent compositions comprising complex organoboron compounds, substituted polyethylene glycols, and neutral organophosphorus compounds in a diluent. The preferred solvent comprises a chlorinated cobalt dicarbollide, diphenyl-dibutylmethylenecarbamoylphosphine oxide, PEG-400, and a diluent of phenylpolyfluoroalkyl sulfone. The invention also provides a method of using the invention extracting agents to recover cesium, strontium, rare earths and actinides from liquid radioactive waste.

  13. Solvent for the simultaneous recovery of radionuclides from liquid radioactive wastes

    DOEpatents

    Romanovskiy, Valeriy Nicholiavich; Smirnov, Igor V.; Babain, Vasiliy A.; Todd, Terry A.; Brewer, Ken N.

    2002-01-01

    The present invention relates to solvents, and methods, for selectively extracting and recovering radionuclides, especially cesium and strontium, rare earths and actinides from liquid radioactive wastes. More specifically, the invention relates to extracting agent solvent compositions comprising complex organoboron compounds, substituted polyethylene glycols, and neutral organophosphorus compounds in a diluent. The preferred solvent comprises a chlorinated cobalt dicarbollide, diphenyl-dibutylmethylenecarbamoylphosphine oxide, PEG-400, and a diluent of phenylpolyfluoroalkyl sulfone. The invention also provides a method of using the invention extracting agents to recover cesium, strontium, rare earths and actinides from liquid radioactive waste.

  14. Novel Solvent for the Simultaneous recovery of Radioactive Nuclides from Liquid Radioactive Wastes

    SciTech Connect

    Romanovskiy, Valeriy Nicholiavich; Smirnov, Lgor V.; Babain, Vasiliy A.; Todd, Terry A.; Brewer, Ken N.

    1999-10-07

    The present invention relates to solvents, and methods, for selectively extracting and recovering radionuclides, especially cesium and strontium, rare earths and actinides from liquid radioactive wastes. More specifically, the invention relates to extracting agent solvent compositions comprising complex organoboron compounds, substituted polyethylene glycols, and neutral organophosphorus compounds in a diluent. The preferred solvent comprises a chlorinated cobalt dicarbollide, diphenyl-dibutylmethylenecarbamoylphosphine oxide, PEG-400, and a diluent of phenylpolyfluoroalkyl sulfone. The invention also provides a method of using the invention extracting agents to recover cesium, strontium, rare earths and actinides from liquid radioactive waste.

  15. Quantification of nimesulide in human plasma by high-performance liquid chromatography/tandem mass spectrometry. Application to bioequivalence studies.

    PubMed

    Barrientos-Astigarraga, R E; Vannuchi, Y B; Sucupira, M; Moreno, R A; Muscará, M N; De Nucci, G

    2001-12-01

    A method based on liquid chromatography with negative ion electrospray ionization and tandem mass spectrometry is described for the determination of nimesulide in human plasma. Liquid-liquid extraction using a mixture of diethyl ether and dichloromethane was employed and celecoxib was used as an internal standard. The chromatographic run time was 4.5 min and the weighted (1/x) calibration curve was linear in the range 10.0-2000 ng x ml(-1). The limit of quantification was 10 ng x ml(-1), the intra-batch precision was 6.3, 2.1 and 2.1% and the intra-batch accuracy was 3.2, 0.3 and 0.1% for 30, 300 and 1200 ng x ml(-1) respectively. The inter-batch precision was 2.3, 2.8 and 2.7% and the accuracy was 3.3, 0.3 and 0.1% for 30, 300 and 1200 ng x ml(-1) respectively. This method was employed in a bioequivalence study of one nimesulide drop formulation (nimesulide 50 mg x ml(-1) drop, Medley S/A Indústria Farmacêutica, Brazil) against one standard nimesulide drop formulation (Nisulid, 50 mg x ml(-1) drop, Astra Médica, Brazil). Twenty-four healthy volunteers (both sexes) took part in the study and received a single oral dose of nimesulide (100 mg, equivalent to 2 ml of either formulation) in an open, randomized, two-period crossover way, with a 2-week washout interval between periods. The 90% confidence interval (CI) for geometric mean ratios between nimesulide and Nisulid were 93.1-109.6% for C(max), 87.7-99.8% for AUC(last) and 88.1-99.7% for AUC(0-infinity). Since the 90% CI for the above-mentioned parameters were included in the 80-125% interval proposed by the US Food and Drug Administration, the two formulations were considered bioequivalent in terms of both rate and extent of absorption. PMID:11754119

  16. The Murmansk low-level liquid radioactive waste treatment facility

    SciTech Connect

    Duffey, R.B.; Penzin, R.A.; Tumparov, A.; Gussgard, K.; Dyer, R.A.; Ruksha, V.V.

    1996-09-01

    Since May 1994, Russian, Norway and the US have cooperated successfully to develop the design of the LLRW treatment facility. Among the other participating organizations are the Association for Advanced Technologies, the Royal norwegian Ministry of Foreign Affairs and the US Environmental Protection Agency (EPA). The joint US/Norwegian/Russian Technical Team for the Design provide technical review and advice. A major objective of the design is to enable Russian to permanently cease disposing of this waste in Arctic waters and to formally adhere to the London Convention permanent ban. Therefore, the modifications will increase the facility`s capacity from 1,200 m{sup 3} per year to 5,000 m{sup 3} per year, will permit the facility to process high-salt wastes from the Russian Navy`s North Fleet and will improve the stabilization and interim storage of the processed wastes. The plant design utilizes novel technology for the filtration and treatment of the high saline waste streams, as well as waste streams for maintenance and decontamination activities. The discharge streams will meet national and international discharge limits for radionuclides. Following detailed design, the next phase is construction.

  17. Municipal Solid Waste (MSW) to Liquid Fuels Synthesis, Volume 1: Availability of Feedstock and Technology

    SciTech Connect

    Valkenburt, Corinne; Walton, Christie W.; Thompson, Becky L.; Gerber, Mark A.; Jones, Susanne B.; Stevens, Don J.

    2008-12-01

    This report investigated the potential of using municipal solid waste (MSW) to make synthesis gas (syngas) suitable for production of liquid fuels. Issues examined include: • MSW physical and chemical properties affecting its suitability as a gasifier feedstock and for liquid fuels synthesis • expected process scale required for favorable economics • the availability of MSW in quantities sufficient to meet process scale requirements • the state-of-the-art of MSW gasification technology.

  18. Uncertainty quantification in the health consequences of the boiling liquid expanding vapour explosion phenomenon.

    PubMed

    Papazoglou, I A; Aneziris, O N

    1999-06-30

    A methodology for estimating the risk owing to the phenomenon of boiling liquid expanding vapour explosion (BLEVE) in the presence of uncertainties both in the model and in the parameters of the models is presented. BLEVE takes place when a tank containing liquefied petroleum gas (LPG) is exposed to fire and fails catastrophically. Two models have been used in the estimation of the intensity of thermal radiation from the resulting fireball, namely the solid-flame model assuming an emission power independent of the combustion mass and the point-source model that estimates the emissive power as a function of the combustion mass. Three measures of the BLEVE consequences, the intensity of thermal radiation, the dose of thermal radiation and the probability of loss of life as a result of the exposure to the thermal radiation and as a function of the distance from the center of the tank have been considered. Uncertainties in the exact values of the parameters of the models have been quantified and the resulting uncertainties in the three consequence measures have been assessed. A sensitivity analysis on the relative contribution of the uncertainty in each of the input variables to the uncertainties of the consequence measures has been performed. One conclusion is that the uncertainties in the probability of loss of life are mainly due to the uncertainties in the model of the physical phenomenon rather than to the uncertainties of the dose-response model. PMID:10370178

  19. Quantification of faropenem in human plasma by high-performance liquid chromatography.

    PubMed

    Nirogi, Ramakrishna V S; Kandikere, Vishwottam N; Shrivastava, Wishu; Mudigonda, Koteshwara

    2005-01-01

    A simple, sensitive and specific high-performance liquid chromatography (HPLC) method with ultraviolet detection (315 nm) was developed and validated for quantitation of faropenem (CAS 106560-14-9), the newest addition to the group of beta-lactam antimicrobials, in human plasma. Following solid-phase extraction using Waters Oasis SPE cartridges, the analyte and internal standard (hydrochlorothiazide, CAS 58-93-5) were separated using an isocratic mobile phase of 10 mmol/L acetate buffer (pH adjusted to 7.0 with dilute acetic acid) / methanol / triethyl amine (70/30/0.03, v/v/v) on reverse phase Waters symmetry C18 column. The lower limit of quantitation was 200 ng/mL, with a relative standard deviation of less than 2 %. A linear range of 200 to 25000 ng/mL was established. This HPLC method was validated with between-batch and within-batch precision of 1.6 to 2.3 % and 0.4 to 1.6 %, respectively. The between-batch and within-batch bias was -3.1 to 5.3 % and -6.0 to 1.5 %, respectively. Frequently coadministered drugs did not interfere with the described methodology. The stability of faropenem in plasma was excellent, with no evidence of degradation during sample processing (autosampler) and 30 days storage in a freezer. This validated method is sensitive, simple and repeatable enough to be used in pharmacokinetic studies. PMID:16430031

  20. Quantification of X. laevis vitellogenin by liquid chromatography tandem mass spectrometry.

    PubMed

    Luna, Leah G; Coady, Katherine

    2016-02-01

    Over the last several decades, there has been an increase in public awareness and regulatory activity in regard to the presence of emerging contaminants in the environment that may have the potential to interact with the endocrine system of exposed wildlife. Alterations in vitellogenin (VTG), a high density yolk precursor protein, can indicate endocrine activity in oviparous species, including many fish and amphibians. While various methodologies and experiments have been performed to characterize baseline VTG concentrations among commonly studied fish species, fewer methodologies for accurately quantifying amphibian VTG are available. Since there is relatively little information available on background VTG levels in male and female frogs, the present investigation set out to quantify baseline levels of VTG in juvenile as well as adult male and female African clawed frogs (Xenopus laevis) using a newly developed liquid chromatography tandem mass spectrometry method. This new methodology for quantifying VTG in X. laevis frog blood plasma can be applied in mechanistic and toxicity studies with X. laevis to better characterize potential endocrine modes of action. PMID:26562177

  1. Evaluation of interim and final waste forms for the newly generated liquid low-level waste flowsheet

    SciTech Connect

    Abotsi, G.M.K.; Bostick, D.T.; Beck, D.E.

    1996-05-01

    The purpose of this review is to evaluate the final forms that have been proposed for radioactive-containing solid wastes and to determine their application to the solid wastes that will result from the treatment of newly generated liquid low-level waste (NGLLLW) and Melton Valley Storage Tank (MVST) supernate at the Oak Ridge National Laboratory (ORNL). Since cesium and strontium are the predominant radionuclides in NGLLLW and MVST supernate, this review is focused on the stabilization and solidification of solid wastes containing these radionuclides in cement, glass, and polymeric materials-the principal waste forms that have been tested with these types of wastes. Several studies have shown that both cesium and strontium are leached by distilled water from solidified cement, although the leachabilities of cesium are generally higher than those of strontium under similar conditions. The situation is exacerbated by the presence of sulfates in the solution, as manifested by cracking of the grout. Additives such as bentonite, blast-furnace slag, fly ash, montmorillonite, pottery clay, silica, and zeolites generally decrease the cesium and strontium release rates. Longer cement curing times (>28 d) and high ionic strengths of the leachates, such as those that occur in seawater, also decrease the leach rates of these radionuclides. Lower cesium leach rates are observed from vitrified wastes than from grout waste forms. However, significant quantities of cesium are volatilized due to the elevated temperatures required to vitrify the waste. Hence, vitrification will generally require the use of cleanup systems for the off-gases to prevent their release into the atmosphere.

  2. Quantification of the resource recovery potential of municipal solid waste incineration bottom ashes

    SciTech Connect

    Allegrini, Elisa; Maresca, Alberto; Olsson, Mikael Emil; Holtze, Maria Sommer; Boldrin, Alessio; Astrup, Thomas Fruergaard

    2014-09-15

    Highlights: • Ferrous and non-ferrous metals were quantified in MSWI bottom ashes. • Metal recovery system efficiencies for bottom ashes were estimated. • Total content of critical elements was determined in bottom ash samples. • Post-incineration recovery is not viable for most critical elements. - Abstract: Municipal solid waste incineration (MSWI) plays an important role in many European waste management systems. However, increasing focus on resource criticality has raised concern regarding the possible loss of critical resources through MSWI. The primary form of solid output from waste incinerators is bottom ashes (BAs), which also have important resource potential. Based on a full-scale Danish recovery facility, detailed material and substance flow analyses (MFA and SFA) were carried out, in order to characterise the resource recovery potential of Danish BA: (i) based on historical and experimental data, all individual flows (representing different grain size fractions) within the recovery facility were quantified, (ii) the resource potential of ferrous (Fe) and non-ferrous (NFe) metals as well as rare earth elements (REE) was determined, (iii) recovery efficiencies were quantified for scrap metal and (iv) resource potential variability and recovery efficiencies were quantified based on a range of ashes from different incinerators. Recovery efficiencies for Fe and NFe reached 85% and 61%, respectively, with the resource potential of metals in BA before recovery being 7.2%ww for Fe and 2.2%ww for NFe. Considerable non-recovered resource potential was found in fine fraction (below 2 mm), where approximately 12% of the total NFe potential in the BA were left. REEs were detected in the ashes, but the levels were two or three orders of magnitude lower than typical ore concentrations. The lack of REE enrichment in BAs indicated that the post-incineration recovery of these resources may not be a likely option with current technology. Based on these results

  3. Simultaneous quantification of multiple urinary naphthalene metabolites by liquid chromatography tandem mass spectrometry.

    PubMed

    Ayala, Daniel C; Morin, Dexter; Buckpitt, Alan R

    2015-01-01

    Naphthalene is an environmental toxicant to which humans are exposed. Naphthalene causes dose-dependent cytotoxicity to murine airway epithelial cells but a link between exposure and human pulmonary disease has not been established. Naphthalene toxicity in rodents depends on P450 metabolism. Subsequent biotransformation results in urinary elimination of several conjugated metabolites. Glucuronide and sulfate conjugates of naphthols have been used as markers of naphthalene exposure but, as the current studies demonstrate, these assays provide a limited view of the range of metabolites generated from the parent hydrocarbon. Here, we present a liquid chromatography tandem mass spectrometry method for measurement of the glucuronide and sulfate conjugates of 1-naphthol as well as the mercapturic acids and N-acetyl glutathione conjugates from naphthalene epoxide. Standard curves were linear over 2 log orders. On column detection limits varied from 0.91 to 3.4 ng; limits of quantitation from 1.8 to 6.4 ng. The accuracy of measurement of spiked urine standards was -13.1 to + 5.2% of target and intra-day and inter-day variability averaged 7.2 (± 4.5) and 6.8 (± 5.0) %, respectively. Application of the method to urine collected from mice exposed to naphthalene at 15 ppm (4 hrs) showed that glutathione-derived metabolites accounted for 60-70% of the total measured metabolites and sulfate and glucuronide conjugates were eliminated in equal amounts. The method is robust and directly measures several major naphthalene metabolites including those derived from glutathione conjugation of naphthalene epoxide. The assays do not require enzymatic deconjugation, extraction or derivatization thus simplifying sample work up. PMID:25853821

  4. Liquid Nebulization-Ion Mobility Spectrometry Based Quantification of Nanoparticle-Protein Conjugate Formation.

    PubMed

    Jeon, Seongho; Oberreit, Derek R; Van Schooneveld, Gary; Hogan, Christopher J

    2016-08-01

    Despite the importance of examining the formation of nanoparticle-protein conjugates, there is a dearth of routine techniques for nanoparticle-protein conjugate characterization. The most prominent change to a nanoparticle population upon conjugate formation is a shift in the nanoparticle size distribution function. However, commonly employed dynamic light scattering based approaches for size distribution characterization are ineffective for nonmonodisperse samples, and further they are relatively insensitive to size shifts of only several nanometers, which are common during conjugate formation. Conversely, gas phase ion mobility spectrometry (IMS) techniques can be used to reliably examine polydisperse samples, and are sensitive to ∼1 nm size distribution function shifts; the challenge with IMS is to convert nanoparticle-protein conjugates to aerosol particles without bringing about nonspecific aggregation or conjugate formation. Except in limited circumstances, electrospray based aerosolization has proven difficult to apply for this purpose. Here we show that via liquid nebulization (LN) with online, high-flow-rate dilution (with dilution factors up to 10 000) it is possible to aerosolize nanoparticle-protein conjugates, enabling IMS measurements of their conjugate size distribution functions. We specifically employ the LN-IMS system to examine bovine serum albumin binding to gold nanoparticles. Inferred maximum protein surface coverages (∼0.025 nm(-2)) from measurements are shown to be in excellent agreement with reported values for gold from quartz crystal microbalance measurements. It is also shown that LN-IMS measurements can be used to detect size distribution function shifts on the order of 1 nm, even in circumstances where the size distribution function itself has a standard deviation of ∼5 nm. In total, the reported measurements suggest that LN-IMS is a potentially simple and robust technique for nanoparticle-protein conjugate characterization

  5. Simultaneous Quantification of Multiple Urinary Naphthalene Metabolites by Liquid Chromatography Tandem Mass Spectrometry

    PubMed Central

    Ayala, Daniel C.; Morin, Dexter; Buckpitt, Alan R.

    2015-01-01

    Naphthalene is an environmental toxicant to which humans are exposed. Naphthalene causes dose-dependent cytotoxicity to murine airway epithelial cells but a link between exposure and human pulmonary disease has not been established. Naphthalene toxicity in rodents depends on P450 metabolism. Subsequent biotransformation results in urinary elimination of several conjugated metabolites. Glucuronide and sulfate conjugates of naphthols have been used as markers of naphthalene exposure but, as the current studies demonstrate, these assays provide a limited view of the range of metabolites generated from the parent hydrocarbon. Here, we present a liquid chromatography tandem mass spectrometry method for measurement of the glucuronide and sulfate conjugates of 1-naphthol as well as the mercapturic acids and N-acetyl glutathione conjugates from naphthalene epoxide. Standard curves were linear over 2 log orders. On column detection limits varied from 0.91 to 3.4 ng; limits of quantitation from 1.8 to 6.4 ng. The accuracy of measurement of spiked urine standards was -13.1 to + 5.2% of target and intra-day and inter-day variability averaged 7.2 (± 4.5) and 6.8 (± 5.0) %, respectively. Application of the method to urine collected from mice exposed to naphthalene at 15 ppm (4 hrs) showed that glutathione-derived metabolites accounted for 60-70% of the total measured metabolites and sulfate and glucuronide conjugates were eliminated in equal amounts. The method is robust and directly measures several major naphthalene metabolites including those derived from glutathione conjugation of naphthalene epoxide. The assays do not require enzymatic deconjugation, extraction or derivatization thus simplifying sample work up. PMID:25853821

  6. Steviol quantification at the picomole level by high-performance liquid chromatography.

    PubMed

    Minne, Veerle J Y; Compernolle, Frans; Toppet, Suzanne; Geuns, Jan M C

    2004-05-01

    A simple and highly sensitive reversed-phase high-performance liquid chromatographic method (RP-HPLC) has been developed for the determination of steviol (SV) using dihydroisosteviol (DHISV) as an internal standard (IS). SV and DHISV were derivatized by reaction of the acids with 4-(bromomethyl)-7-methoxycoumarin in an aprotic solvent (DMF or acetone). The resulting ester derivatives were separated on an ODS column (250 x 4.6 mm i.d., 5 microm particle size) using fluorescence detection with excitation at 321 nm and emission at 391 nm. The mobile phase consisted of acetonitrile/water (80:20 v/v) with a flow rate of 1 mL min(-)(1). A linear relationship was observed for concentrations between 0.5 and 50 microg/mL of SV, and the detection limit was 100 pg. For application of this method to samples of beer fortified with stevioside, a simple procedure for extraction of the beer with diethyl ether and derivatization in DMF was applied. Whereas beer samples spiked with SV gave a linear response over the range 0.1-15 microg/mL beer, no SV could be detected in beer samples enriched in stevioside that had been stored for over 3 years. The application of the method to plant samples involved preparation of an acid fraction containing the SV analyte, derivatization, and sample cleanup using small silica columns and thin-layer chromatography. A sensitive determination of 594 ng of steviol present in 100 mg of dry plant material was performed with high precision and accuracy. PMID:15113139

  7. Processing industrial wastes with the liquid-phase reduction romelt process

    NASA Astrophysics Data System (ADS)

    Romenets, V.; Valavin, V.; Pokhvisnev, Yu.; Vandariev, S.

    1999-08-01

    The Romelt technology for liquid-phase reduction has been developed for processing metallurgical wastes containing nonferrousmetal components. Thermodynamic calculations were made to investigate the behavior of silver, copper, zinc, manganese, vanadium, chrome, and silicon when reduced from the slag melt into the metallic solution containing iron. The process can be applied to all types of iron-bearing wastes, including electric arc furnace dust. The distribution of elements between the phases can be controlled by adjusting the slag bath temperature. Experiments at a pilot Romelt plant proved the possibility of recovering the metallurgical wastes and obtaining iron.

  8. Development of Advanced Electrochemical Emission Spectroscopy for Monitoring Corrosion in Simulated DOE Liquid Waste

    SciTech Connect

    MacDonal, Digby D.; Marx, Brian M.; Ahn, Sejin; Ruiz, Julio de; Soundararajan, Balaji; Smith, Morgan; Coulson, Wendy

    2005-06-15

    Various forms of general and localized corrosion represent principal threats to the integrity of DOE liquid waste storage tanks. These tanks, which are of a single wall or double wall design, depending upon their age, are fabricated from welded carbon steel and contain a complex waste-form comprised of NaOH and NaNO3, along with trace amounts of phosphate, sulfate, carbonate, and chloride. Because waste leakage can have a profound environmental impact, considerable interest exists in predicting the accumulation of corrosion damage, so as to more effectively schedule maintenance and repair.

  9. Statistical Description of Liquid Low-Level Waste System Transssuranic Wastes at Oak Ridge Nation Laboratory, Oak Ridge, Tennessee

    SciTech Connect

    1996-12-01

    The US DOE has presented plans for processing liquid low-level wastes (LLLW) located at Oak Ridge National Laboratory (ORNL) in the LLLW tank system. These wastes are among the most hazardous on the Oak Ridge reservation and exhibit both RCRA toxic and radiological hazards. The Tennessee Department of Health and Environment has mandated that the processing of these wastes must begin by the year 2002 and the the goal should be permanent disposal at a site off the Oak Ridge Reservation. To meet this schedule, DOE will solicit bids from various private sector companies for the construction of a processing facility on land located near the ORNL Melton Valley Storage Tanks to be operated by the private sector on a contract basis. This report will support the Request for Proposal process and will give potential vendors information about the wastes contained in the ORNL tank farm system. The report consolidates current data about the properties and composition of these wastes and presents methods to calculate the error bounds of the data in the best technically defensible manner possible. The report includes information for only the tank waste that is to be included in the request for proposal.

  10. 30 CFR 250.217 - What solid and liquid wastes and discharges information and cooling water intake information must...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... information and cooling water intake information must accompany the EP? 250.217 Section 250.217 Mineral... What solid and liquid wastes and discharges information and cooling water intake information must accompany the EP? The following solid and liquid wastes and discharges information and cooling water...

  11. 30 CFR 550.248 - What solid and liquid wastes and discharges information and cooling water intake information must...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... information and cooling water intake information must accompany the DPP or DOCD? 550.248 Section 550.248... liquid wastes and discharges information and cooling water intake information must accompany the DPP or DOCD? The following solid and liquid wastes and discharges information and cooling water...

  12. 30 CFR 550.217 - What solid and liquid wastes and discharges information and cooling water intake information must...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... information and cooling water intake information must accompany the EP? 550.217 Section 550.217 Mineral... What solid and liquid wastes and discharges information and cooling water intake information must accompany the EP? The following solid and liquid wastes and discharges information and cooling water...

  13. Status of the ORNL liquid low-level waste management upgrades

    SciTech Connect

    Robinson, S.M.; Kent, T.E.; DePaoli, S.M.

    1995-08-01

    The strategy for management of the Oak Ridge National Laboratory`s (ORNL`s) radioactively contaminated liquid waste was reviewed. The latest information on waste characterization, regulations, US Department of Energy (DOE) budget guidance, and research and development programs was evaluated to determine how the strategy should be revised. Few changes are needed to update the strategy to reflect new waste characterization, research, and regulatory information. However, recent budget guidance from DOE indicates that minimum funding will not be sufficient to accomplish original objectives to upgrade the liquid low-level waste (LLLW) system to be in compliance with the Federal Facilities Agreement compliance, provide long-term LLLW treatment capability, and minimize Environmental Safety & Health risks. Options are presented that might allow the ORNL LLLW system to continue operations temporarily but significantly reduce its capabilities to handle emergency situations, provide treatment for new waste streams, and accommodate waste from the Environmental Restoration Program and from decontamination and decommissioning of surplus facilities. These options are also likely to increase worker radiation exposure, risk of environmental insult, and generation of solid waste for on-site and off-site disposal/storage beyond existing facility capacities. The strategy will be fully developed after receiving additional guidance. The proposed budget limitations are too severe to allow ORNL to meet regulatory requirements or continue operations long term.

  14. Biochemical process of low level radioactive liquid simulation waste containing detergent

    SciTech Connect

    Kundari, Noor Anis Putra, Sugili; Mukaromah, Umi

    2015-12-29

    Research of biochemical process of low level radioactive liquid waste containing detergent has been done. Thse organic liquid wastes are generated in nuclear facilities such as from laundry. The wastes that are cotegorized as hazard and poison materials are also radioactive. It must be treated properly by detoxification of the hazard and decontamination of the radionuclides to ensure that the disposal of the waste meets the requirement of standard quality of water. This research was intended to determine decontamination factor and separation efficiensies, its kinetics law, and to produce a supernatant that ensured the environmental quality standard. The radioactive element in the waste was thorium with activity of 5.10{sup −5} Ci/m{sup 3}. The radioactive liquid waste which were generated in simulation plant contains detergents that was further processed by aerobic biochemical process using SGB 103 bacteria in a batch reactor equipped with aerators. Two different concentration of samples were processed and analyzed for 212 hours and 183 hours respectively at a room temperature. The product of this process is a liquid phase called as supernatant and solid phase material called sludge. The chemical oxygen demand (COD), biological oxygen demand (BOD), suspended solid (SS), and its alpha activity were analyzed. The results show that the decontamination factor and the separation efficiency of the lower concentration samples are higher compared to the samples with high concentration. Regarding the decontamination factor, the result for 212 hours processing of waste with detergent concentration of 1.496 g/L was 3.496 times, whereas at the detergent concentration of 0.748 g/L was 15.305 times for 183 hours processing. In case of the separation efficiency, the results for both samples were 71.396% and 93.465% respectively. The Bacterial growth kinetics equation follow Monod’s model and the decreasing of COD and BOD were first order with the rate constant of 0

  15. Biochemical process of low level radioactive liquid simulation waste containing detergent

    NASA Astrophysics Data System (ADS)

    Kundari, Noor Anis; Putra, Sugili; Mukaromah, Umi

    2015-12-01

    Research of biochemical process of low level radioactive liquid waste containing detergent has been done. Thse organic liquid wastes are generated in nuclear facilities such as from laundry. The wastes that are cotegorized as hazard and poison materials are also radioactive. It must be treated properly by detoxification of the hazard and decontamination of the radionuclides to ensure that the disposal of the waste meets the requirement of standard quality of water. This research was intended to determine decontamination factor and separation efficiensies, its kinetics law, and to produce a supernatant that ensured the environmental quality standard. The radioactive element in the waste was thorium with activity of 5.10-5 Ci/m3. The radioactive liquid waste which were generated in simulation plant contains detergents that was further processed by aerobic biochemical process using SGB 103 bacteria in a batch reactor equipped with aerators. Two different concentration of samples were processed and analyzed for 212 hours and 183 hours respectively at a room temperature. The product of this process is a liquid phase called as supernatant and solid phase material called sludge. The chemical oxygen demand (COD), biological oxygen demand (BOD), suspended solid (SS), and its alpha activity were analyzed. The results show that the decontamination factor and the separation efficiency of the lower concentration samples are higher compared to the samples with high concentration. Regarding the decontamination factor, the result for 212 hours processing of waste with detergent concentration of 1.496 g/L was 3.496 times, whereas at the detergent concentration of 0.748 g/L was 15.305 times for 183 hours processing. In case of the separation efficiency, the results for both samples were 71.396% and 93.465% respectively. The Bacterial growth kinetics equation follow Monod's model and the decreasing of COD and BOD were first order with the rate constant of 0.01 hour-1.

  16. Removal of Radioactive Nuclides from Mo-99 Acidic Liquid Waste - 13027

    SciTech Connect

    Hsiao, Hsien-Ming; Pen, Ben-Li

    2013-07-01

    About 200 liters highly radioactive acidic liquid waste originating from Mo-99 production was stored at INER (Institute of Nuclear Energy Research). A study regarding the treatment of the radioactive acidic liquid waste was conducted to solve storage-related issues and allow discharge of the waste while avoiding environmental pollution. Before discharging the liquid waste, the acidity, NO{sub 3}{sup -} and Hg ions in high concentrations, and radionuclides must comply with environmental regulations. Therefore, the treatment plan was to neutralize the acidic liquid waste, remove key radionuclides to reduce the dose rate, and then remove the nitrate and mercury ions. Bench tests revealed that NaOH is the preferred solution to neutralize the high acidic waste solution and the pH of solution must be adjusted to 9∼11 prior to the removal of nuclides. Significant precipitation was produced when the pH of solution reached 9. NaNO{sub 3} was the major content in the precipitate and part of NaNO{sub 3} was too fine to be completely collected by filter paper with a pore size of approximately 3 μm. The residual fine particles remaining in solution therefore blocked the adsorption column during operation. Two kinds of adsorbents were employed for Cs-137 and a third for Sr-90 removal to minimize cost. For personnel radiation protection, significant lead shielding was required at a number of points in the process. The final process design and treatment facilities successfully treated the waste solutions and allowed for environmentally compliant discharge. (authors)

  17. Quantification of neurotransmitters in mouse brain tissue by using liquid chromatography coupled electrospray tandem mass spectrometry.

    PubMed

    Kim, Tae-Hyun; Choi, Juhee; Kim, Hyung-Gun; Kim, Hak Rim

    2014-01-01

    A simple and rapid liquid chromatography tandem mass spectrometry method has been developed for the determination of BH4, DA, 5-HT, NE, EP, Glu, and GABA in mouse brain using epsilon-acetamidocaproic acid and isotopically labeled neurotransmitters as internal standards. Proteins in the samples were precipitated by adding acetonitrile, and then the supernatants were separated by a Sepax Polar-Imidazole (2.1 mm × 100 mm, i.d., 3 μm) column by adding a mixture of 10 mM ammonium formate in acetonitrile/water (75 : 25, v/v, 300 μl/min) for BH4 and DA. To assay 5-HT, NE, EP, Glu, and GABA; a Luna 3 μ C18 (3.0 mm × 150 mm, i.d., 3 μm) column was used by adding a mixture of 1% formic acid in acetonitrile/water (20 : 80, v/v, 350 μl/min). The total chromatographic run time was 5.5 min. The method was validated for the analysis of samples. The calibration curve was linear between 10 and 2000 ng/g for BH4 (r(2) = 0.995) , 10 and 5000 ng/g for DA (r(2) = 0.997) , 20 and 10000 ng/g for 5-HT (r(2) = 0.994) , NE (r(2) = 0.993) , and EP (r(2) = 0.993) , and 0.2 and 200 μg/g for Glu (r(2) = 0.996) and GABA (r(2) = 0.999) in the mouse brain tissues. As stated above, LC-MS/MS results were obtained and established to be a useful tool for the quantitative analysis of BH4, DA, 5-HT, NE, EP, Glu, and GABA in the experimental rodent brain. PMID:25258696

  18. Amphiphilic antioxidants from "cashew nut shell liquid" (CNSL) waste.

    PubMed

    Amorati, Riccardo; Attanasi, Orazio A; Favi, Gianfranco; Menichetti, Stefano; Pedulli, Gian Franco; Viglianisi, Caterina

    2011-03-01

    Hydrogenated cardanol and cardols, contained in industrial grade cardanol oil and obtained by distillation of the raw "cashew nut shell liquid" (CNSL), are easily transformed into efficient 4-thiaflavane antioxidants bearing a long alkyl chain on A ring and a catechol group on B ring. PMID:21240431

  19. 11-Nor-9-carboxy-∆9-tetrahydrocannabinol quantification in human oral fluid by liquid chromatography-tandem mass spectrometry.

    PubMed

    Scheidweiler, Karl B; Himes, Sarah K; Chen, Xiaohong; Liu, Hua-Fen; Huestis, Marilyn A

    2013-07-01

    Currently, ∆9-tetrahydrocannabinol (THC) is the analyte quantified for oral fluid cannabinoid monitoring. The potential for false-positive oral fluid cannabinoid results from passive exposure to THC-laden cannabis smoke raises concerns for this promising new monitoring technology. Oral fluid 11-nor-9-carboxy-∆9-tetrahydrocannabinol (THCCOOH) is proposed as a marker of cannabis intake since it is not present in cannabis smoke and was not measureable in oral fluid collected from subjects passively exposed to cannabis. THCCOOH concentrations are in the picogram per milliliter range in oral fluid and pose considerable analytical challenges. A liquid chromatography-tandem mass spectrometry (LCMSMS) method was developed and validated for quantifying THCCOOH in 1 mL Quantisal-collected oral fluid. After solid phase extraction, chromatography was performed on a Kinetex C18 column with a gradient of 0.01% acetic acid in water and 0.01% acetic acid in methanol with a 0.5-mL/min flow rate. THCCOOH was monitored in negative mode electrospray ionization and multiple reaction monitoring mass spectrometry. The THCCOOH linear range was 12-1,020 pg/mL (R(2) > 0.995). Mean extraction efficiencies and matrix effects evaluated at low and high quality control (QC) concentrations were 40.8-65.1 and -2.4-11.5%, respectively (n = 10). Analytical recoveries (bias) and total imprecision at low, mid, and high QCs were 85.0-113.3 and 6.6-8.4% coefficient of variation, respectively (n = 20). This is the first oral fluid THCCOOH LCMSMS triple quadrupole method not requiring derivatization to achieve a <15 pg/mL limit of quantification. The assay is applicable for the workplace, driving under the influence of drugs, drug treatment, and pain management testing. PMID:23681203

  20. 11-Nor-9-carboxy-Δ9-tetrahydrocannabinol quantification in human oral fluid by liquid chromatography–tandem mass spectrometry

    PubMed Central

    Scheidweiler, Karl B.; Himes, Sarah K.; Chen, Xiaohong; Liu, Hua-Fen

    2013-01-01

    Currently, Δ9-tetrahydrocannabinol (THC) is the analyte quantified for oral fluid cannabinoid monitoring. The potential for false-positive oral fluid cannabinoid results from passive exposure to THC-laden cannabis smoke raises concerns for this promising new monitoring technology. Oral fluid 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) is proposed as a marker of cannabis intake since it is not present in cannabis smoke and was not measureable in oral fluid collected from subjects passively exposed to cannabis. THCCOOH concentrations are in the picogram per milliliter range in oral fluid and pose considerable analytical challenges. A liquid chromatography–tandem mass spectrometry (LCMSMS) method was developed and validated for quantifying THCCOOH in 1 mL Quantisal-collected oral fluid. After solid phase extraction, chromatography was performed on a Kinetex C18 column with a gradient of 0.01 % acetic acid in water and 0.01 % acetic acid in methanol with a 0.5-mL/min flow rate. THCCOOH was monitored in negative mode electrospray ionization and multiple reaction monitoring mass spectrometry. The THCCOOH linear range was 12–1,020 pg/mL (R2>0.995). Mean extraction efficiencies and matrix effects evaluated at low and high quality control (QC) concentrations were 40.8–65.1 and −2.4–11.5 %, respectively (n=10). Analytical recoveries (bias) and total imprecision at low, mid, and high QCs were 85.0–113.3 and 6.6–8.4 % coefficient of variation, respectively (n=20). This is the first oral fluid THCCOOH LCMSMS triple quadrupole method not requiring derivatization to achieve a <15 pg/mL limit of quantification. The assay is applicable for the workplace, driving under the influence of drugs, drug treatment, and pain management testing. PMID:23681203

  1. Rapid quantification of miglustat in human plasma and cerebrospinal fluid by liquid chromatography coupled with tandem mass spectrometry.

    PubMed

    Guitton, Jérôme; Coste, Sylvie; Guffon-Fouilhoux, Nathalie; Cohen, Sabine; Manchon, Monique; Guillaumont, Marc

    2009-01-15

    Miglustat (OGT 918) is an iminosugar recently introduced in therapeutic as potential alternative therapy in disorders found in several diseases such as Tay-Sachs, Gaucher or Niemann-Pick diseases. A highly sensitive liquid-chromatography-electrospray tandem mass spectrometry (LC-MS/MS) assay was developed for the quantification of miglustat in human plasma and cerebrospinal fluid (CSF). The sample preparation consists in a simple protein precipitation with a mixture of acetonitrile/methanol (75/25) which yields 100% recovery. The isocratic separation utilizes an Atlantis Hilic (3 microm, 150 mm x 2.1 mm) column, with a mobile phase of acetonitrile/water/ammonium acetate buffer (75/10/15, v/v/v) delivered at 230 microl/min. Selected reaction monitoring (SRM) mode was used with the transitions m/z 220-->158 for the miglustat and m/z 208-->m/z 146 for the miglitol (internal standard). Good linearity was observed in a range from 125 to 2500 ng/ml and from 50 to 1000 ng/ml, for plasma and CSF, respectively. The within-run precision of the assay was less than 6%, and the between-run run precision was less than 6.5%, for six replicates at each of three concentrations and evaluated on three separated days for both plasma and CSF mediums. Assay accuracy was in the range of 98-106.5%. Stability of miglustat was reported under a variety of storage conditions. The miglustat concentrations in two children are presented to demonstrate the clinical interest of this new method. PMID:19095507

  2. Quantification of melamine in human urine using cation-exchange based high performance liquid chromatography tandem mass spectrometry.

    PubMed

    Panuwet, Parinya; Nguyen, Johnny V; Wade, Erin L; D'Souza, Priya E; Ryan, P Barry; Barr, Dana Boyd

    2012-03-01

    Melamine and cyanuric acid have been implicated as adulterants in baby formula in China and pet foods in North America. In China, the effect of melamine or melamine-cyanuric acid adulteration lead to kidney stone development and acute renal failure in thousands of Chinese infants. A selective and sensitive analytical method was developed to measure melamine in human urine in order to evaluate the extent of potential health implications resulting from the consumption of these types of adulterated products in the general US population. This method involves extracting melamine from human urine using cation-exchange solid-phase extraction, chromatographically separating it from its urinary matrix co-extractants on a silica-based, strong-cation exchange analytical column using high performance liquid chromatography, and analysis using positive mode electrospray ionization tandem mass spectrometry. Quantification was performed using modified, matrix-based isotope dilution calibration covering the concentration range of 0.50-100 ng/mL. The limit of detection, calculated using replicates of blank and low level spiked samples, was 0.66 ng/mL and the relative standard deviations were between 6.89 and 14.9%. The relative recovery of melamine was 101-106%. This method was tested for viability by analyzing samples collected from the general US population. Melamine was detected in 76% of the samples tested, with a geometric mean of 2.37 ng/mL, indicating that this method is suitable for reliably detecting background exposures to melamine or other chemicals from which it can be derived. PMID:22309774

  3. Ultrasensitive quantification of serum estrogens in postmenopausal women and older men by liquid chromatography-tandem mass spectrometry

    PubMed Central

    Wang, Qingqing; Rangiah, Kannan; Mesaros, Clementina; Snyder, Nathaniel W.; Vachani, Anil; Song, Haifeng; Blair, Ian A.

    2015-01-01

    An ultrasensitive stable isotope dilution liquid chromatography-tandem mass spectrometry method (LC-MS/MS) was developed and validated for multiplexed quantitative analysis of six unconjugated and conjugated estrogens in human serum. The quantification utilized a new derivatization procedure, which formed analytes as pre-ionized N-methyl pyridinium-3-sulfonyl (NMPS) derivatives. This method required only 0.1 mL of human serum, yet was capable of simultaneously quantifying six estrogens within 20 min. The lower limit of quantitation (LLOQ) for estradiol (E2), 16α-hydroxy (OH)-E2, 4-methoxy (MeO)-E2 and 2-MeO-E2 was 1 fg on column, and was 10 fg on column for 4-OH-E2 and 2-OH-E2. All analytes demonstrated a linear response from 0.5 to 200 pg/mL (5–2000 pg/mL for 4-OH-E2 and 2-OH-E2). Using this validated method, the estrogen levels in human serum samples from 20 female patients and 20 male patients were analyzed and compared. The levels found for unconjugated serum E2 from postmenopausal women (mean 2.7 pg/mL) were very similar to those obtained by highly sensitive gas chromatography-mass spectrometry (GC-MS) methodology. However, the level obtained in serum from older men (mean 9.5 pg/mL) was lower than has been reported previously by both GC-MS and LC-MS procedures. The total (unconjugated + conjugated) 4-MeO-E2 levels were significantly higher in female samples compared with males (p<0.05). The enhanced sensitivity offered by the present method will allow for a more specific analysis of estrogens and their metabolites. Our observations might suggest that the level of total 4-MeO-E2 could be a potential biomarker for breast cancer cases. PMID:25637677

  4. Development and validation of a liquid chromatography isotope dilution mass spectrometry method for the reliable quantification of alkylphenols in environmental water samples by isotope pattern deconvolution.

    PubMed

    Fabregat-Cabello, Neus; Sancho, Juan V; Vidal, Andreu; González, Florenci V; Roig-Navarro, Antoni Francesc

    2014-02-01

    We present here a new measurement method for the rapid extraction and accurate quantification of technical nonylphenol (NP) and 4-t-octylphenol (OP) in complex matrix water samples by UHPLC-ESI-MS/MS. The extraction of both compounds is achieved in 30min by means of hollow fiber liquid phase microextraction (HF-LPME) using 1-octanol as acceptor phase, which provides an enrichment (preconcentration) factor of 800. On the other hand we have developed a quantification method based on isotope dilution mass spectrometry (IDMS) and singly (13)C1-labeled compounds. To this end the minimal labeled (13)C1-4-(3,6-dimethyl-3-heptyl)-phenol and (13)C1-t-octylphenol isomers were synthesized, which coelute with the natural compounds and allows the compensation of the matrix effect. The quantification was carried out by using isotope pattern deconvolution (IPD), which permits to obtain the concentration of both compounds without the need to build any calibration graph, reducing the total analysis time. The combination of both extraction and determination techniques have allowed to validate for the first time a HF-LPME methodology at the required levels by legislation achieving limits of quantification of 0.1ngmL(-1) and recoveries within 97-109%. Due to the low cost of HF-LPME and total time consumption, this methodology is ready for implementation in routine analytical laboratories. PMID:24423386

  5. A&M. Hot liquid waste treatment building (TAN616). Camera facing north. ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    A&M. Hot liquid waste treatment building (TAN-616). Camera facing north. Detail of personnel entrance door, stoop, and stairway. Photographer: Ron Paarmann. Date: September 22, 1997. INEEL negative no. HD-20-2-1 - Idaho National Engineering Laboratory, Test Area North, Scoville, Butte County, ID

  6. A&M. Hot liquid waste treatment building (TAN616), south side. Camera ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    A&M. Hot liquid waste treatment building (TAN-616), south side. Camera facing north. Personnel door at left side of wall. Partial view of outdoor stairway to upper level platform. Note concrete construction. Photographer: Ron Paarmann. Date: September 22, 1997. INEEL negative no. HD-20-1-3 - Idaho National Engineering Laboratory, Test Area North, Scoville, Butte County, ID

  7. A&M. Hot liquid waste treatment building (TAN616). Camera facing east. ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    A&M. Hot liquid waste treatment building (TAN-616). Camera facing east. Showing west facades of structure. Photographer: Ron Paarmann. Date: September 22, 1997. INEEL negative no. HD-20-1-1 - Idaho National Engineering Laboratory, Test Area North, Scoville, Butte County, ID

  8. A&M. Hot liquid waste treatment building (TAN616). Camera facing northeast. ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    A&M. Hot liquid waste treatment building (TAN-616). Camera facing northeast. South wall with oblique views of west sides of structure. Photographer: Ron Paarmann. Date: September 22, 1997. INEEL negative no. HD-20-1-2 - Idaho National Engineering Laboratory, Test Area North, Scoville, Butte County, ID

  9. A&M. Liquid waste treatment plant, TAN616. Plan, elevations, sections, and ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    A&M. Liquid waste treatment plant, TAN-616. Plan, elevations, sections, and details. Evaporator pit. Pump room. Room names and numbers. Ralph M. Parsons 902-3-ANP-616-A 297. Date: December 1952. Approved by INEEL Classification Office for public release. INEEL index no. 034-0616-00-693-106889 - Idaho National Engineering Laboratory, Test Area North, Scoville, Butte County, ID

  10. PREDICTION OF TRANSIENT BEHAVIOR DURING BATCH INCINERATION OF LIQUID WASTES IN ROTARY KILNS

    EPA Science Inventory

    The paper discusses a theoretical model which was designed to: (1) provide insight into why, for liquid wastes, "puffs" are very easily generated, and why their magnitudes and intensities increase with increasing kiln temperature and speed of rotation; and (2) predict how the gen...

  11. Optimization of extraction of phenolic acids from a vegetable waste product using a pressurized liquid extractor

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Potato tubers are eaten worldwide for their nutritional value, but potato peels are often disposed as waste. This study identified the phenolic acids content in potato peels, tuber, and developed an optimized method for extraction of phenolic acids from potato peels using a pressurized liquid extrac...

  12. DEVELOPMENT OF ADVANCED ELECTROCHEMICAL EMISSION SPECTROSCOPY FOR MONITORING CORROSION IN SIMULATED DOE LIQUID WASTE

    EPA Science Inventory

    The Department of Energy currently stores millions of gallons of high level liquid radioactive waste in underground, carbon steel-lined concrete tanks at the Hanford Reservation in the state of Washington and at the Savannah River Site in South Carolina. Because of the indefinite...

  13. ANNUAL REPORT. DEVELOPMENT OF ADVANCED ELECTROCHEMICAL EMISSION SPECTROSCOPY FOR MONITORING CORROSION IN SIMULATED DOE LIQUID WASTE

    EPA Science Inventory

    The current report summarizes work performed on the project over the past calendar year (2001). The work concentrated on four areas: the fracture of AISI 4340 steel simulating weld heat affected zones in DOE liquid waste storage tanks, investigation of the passive state on nickel...

  14. Process for the denitrification of high-level radioactive liquid wastes

    NASA Astrophysics Data System (ADS)

    Gattys, F. J.

    1981-07-01

    Commercial paraformaldehyde with a low water content and mean particle size smaller than 60 microns is introduced as denitrifying agent at about 110 C into the liquid waste. A buffer of citric acid and phosphate is added during the denitrification reaction. The escaping gases contain nitrogen oxides which are recombined and concentrated to about 40 percent by weight nitric acid.

  15. Groundwater impact assessment report for the 1325-N Liquid Waste Disposal Facility

    SciTech Connect

    Alexander, D.J.; Johnson, V.G.

    1993-09-01

    In 1943 the Hanford Site was chosen as a location for the Manhattan Project to produce plutonium for use in nuclear weapons. The 100-N Area at Hanford was used from 1963 to 1987 for a dual-purpose, plutonium production and steam generation reactor and related operational support facilities (Diediker and Hall 1987). In November 1989, the reactor was put into dry layup status. During operations, chemical and radioactive wastes were released into the area soil, air, and groundwater. The 1325-N LWDF was constructed in 1983 to replace the 1301-N Liquid Waste Disposal Facility (1301-N LWDF). The two facilities operated simultaneously from 1983 to 1985. The 1301-N LWDF was retired from use in 1985 and the 1325-N LWDF continued operation until April 1991, when active discharges to the facility ceased. Effluent discharge to the piping system has been controlled by administrative means. This report discusses ground water contamination resulting from the 1325-N Liquid Waste Disposal facility.

  16. Getters for Tc and I Removal from Liquid Waste

    NASA Astrophysics Data System (ADS)

    Qafoku, N. P.; Asmussen, M.; Lawter, A.; Neeway, J.; Smith, G.

    2015-12-01

    A cementitious waste form, Cast Stone, is being evaluated as a possible supplemental waste form for the low activity waste (LAW) at the Hanford Site, which contains significant amounts of radioactive 99Tc and 129I, as part of the tank waste cleanup mission. To improve the retention of Tc and/or I in Cast Stone, materials with a high affinity for Tc and/or I, termed "getters," can be added to decrease the rate of contaminant release and diffusivity, and improve Cast Stone performance. A series of kinetic batch sorption experiments was performed to determine the effectiveness of the getter materials. Several Tc getters [blast furnace slag, Sn (II) apatite, SnCl2, nanoporous Sn phosphate, KMS-2 (a potassium-metal-sulfide), and Sn(II) hydroxyapatite] and I getters [layered Bi hydroxide, natural argentite mineral, synthetic argentite, Ag-impregnated carbon, and Ag-exchanged zeolite] were tested in different solution media, 18.2 MΩ DI H2O and a caustic LAW waste simulant containing 6.5 M Na or 7.8 M Na. The experiments were conducted at room temperature in the presence or absence of air. Results indicated that most Tc getters (with the exception of KMS-2) performed better in the DI H2O solution than in the 6.5 and 7.8 M Na LAW simulant. In addition, Tc sequestration may be affected by the presence of other redox sensitive elements that were present in the LAW simulant, such as Cr. The Tc getter materials have been examined through various solid-state characterization techniques such as XRD, SEM/EDS, XANES and EXAFS which provided evidence for plausible mechanisms of aqueous Tc removal. The results indicated that the Tc precipitates differ depending on the getter material and that Tc(VII) is reduced to Tc(IV) in most of the getters but to a differing extents. For the I getters, Ag-exchanged zeolite and synthetic argentite were the most effective ones. The other I getters showed limited effectiveness for sorbing I under the high ionic strength and caustic

  17. Ionic Liquids for Utilization of Waste Heat from Distributed Power Generation Systems

    SciTech Connect

    Joan F. Brennecke; Mihir Sen; Edward J. Maginn; Samuel Paolucci; Mark A. Stadtherr; Peter T. Disser; Mike Zdyb

    2009-01-11

    The objective of this research project was the development of ionic liquids to capture and utilize waste heat from distributed power generation systems. Ionic Liquids (ILs) are organic salts that are liquid at room temperature and they have the potential to make fundamental and far-reaching changes in the way we use energy. In particular, the focus of this project was fundamental research on the potential use of IL/CO2 mixtures in absorption-refrigeration systems. Such systems can provide cooling by utilizing waste heat from various sources, including distributed power generation. The basic objectives of the research were to design and synthesize ILs appropriate for the task, to measure and model thermophysical properties and phase behavior of ILs and IL/CO2 mixtures, and to model the performance of IL/CO2 absorption-refrigeration systems.

  18. Prospects for using membrane distallation for reprocessing liquid radioactive wastes

    SciTech Connect

    Dytnerskii, Y.I.; Karlin, Y.V.; Kropotov, B.N.

    1994-05-01

    Membrane distillation is a promising method for deep desalinization and for removal of impurities of different nature from water. The crux of the method is as follows. The initial (hot) solution, heated up to 30-70{degrees}C, is fed into one side of a hydrophobic microporous membrane. A less heated (cold) distillate moves along the other. Since the membrane is hydrophobic and the pores are small ({approximately}1 {mu}m and less), the liquid phase does not penetrate into the pores in accordance with Kelvin`s law. The vapor evaporating from the surface of the hot solution (the evaporation surface in this case are solution meniscuses forming at the entrance into a pore) penetrates into the pores of the membrane, diffuses through the air layer in the pore, and condenses on the surface of the menisci of cold liquid. In the process rarefaction is produced in the pores, and this accelerates evaporation and therefore increases its efficiency.

  19. Audit of the radioactive liquid waste treatment facility operations at the Los Alamos National Laboratory

    SciTech Connect

    1997-11-19

    Los Alamos National Laboratory (Los Alamos) generates radioactive and liquid wastes that must be treated before being discharged to the environment. Presently, the liquid wastes are treated in the Radioactive Liquid Waste Treatment Facility (Treatment Facility), which is over 30 years old and in need of repair or replacement. However, there are various ways to satisfy the treatment need. The objective of the audit was to determine whether Los Alamos cost effectively managed its Treatment Facility operations. The audit determined that Los Alamos` treatment costs were significantly higher when compared to similar costs incurred by the private sector. This situation occurred because Los Alamos did not perform a complete analysis of privatization or prepare a {open_quotes}make-or-buy{close_quotes} plan for its treatment operations, although a {open_quotes}make-or-buy{close_quotes} plan requirement was incorporated into the contract in 1996. As a result, Los Alamos may be spending $2.15 million more than necessary each year and could needlessly spend $10.75 million over the next five years to treat its radioactive liquid waste. In addition, Los Alamos has proposed to spend $13 million for a new treatment facility that may not be needed if privatization proves to be a cost effective alternative. We recommended that the Manager, Albuquerque Operations Office (Albuquerque), (1) require Los Alamos to prepare a {open_quotes}make-or-buy{close_quotes} plan for its radioactive liquid waste treatment operations, (2) review the plan for approval, and (3) direct Los Alamos to select the most cost effective method of operations while also considering other factors such as mission support, reliability, and long-term program needs. Albuquerque concurred with the recommendations.

  20. On-Site Decontamination System for Liquid Low Level Radioactive Waste - 13010

    SciTech Connect

    OSMANLIOGLU, Ahmet Erdal

    2013-07-01

    This study is based on an evaluation of purification methods for liquid low-level radioactive waste (LLLW) by using natural zeolite. Generally the volume of liquid low-level waste is relatively large and the specific activity is rather low when compared to other radioactive waste types. In this study, a pilot scale column was used with natural zeolite as an ion exchanger media. Decontamination and minimization of LLLW especially at the generation site decrease operational cost in waste management operations. Portable pilot scale column was constructed for decontamination of LLW on site. Effect of temperature on the radionuclide adsorption of the zeolite was determined to optimize the waste solution temperature for the plant scale operations. In addition, effect of pH on the radionuclide uptake of the zeolite column was determined to optimize the waste solution pH for the plant scale operations. The advantages of this method used for the processing of LLLW are discussed in this paper. (authors)

  1. Assessment and analysis of industrial liquid waste and sludge disposal at unlined landfill sites in arid climate

    SciTech Connect

    Al Yaqout, Anwar F

    2003-07-01

    Municipal solid waste disposal sites in arid countries such as Kuwait receive various types of waste materials like sewage sludge, chemical waste and other debris. Large amounts of leachate are expected to be generated due to the improper disposal of industrial wastewater, sewage sludge and chemical wastes with municipal solid waste at landfill sites even though the rainwater is scarce. Almost 95% of all solid waste generated in Kuwait during the last 10 years was dumped in five unlined landfills. The sites accepting liquid waste consist of old sand quarries that do not follow any specific engineering guidelines. With the current practice, contamination of the ground water table is possible due to the close location of the water table beneath the bottom of the waste disposal sites. This study determined the percentage of industrial liquid waste and sludge of the total waste dumped at the landfill sites, analyzed the chemical characteristics of liquid waste stream and contaminated water at disposal sites, and finally evaluated the possible risk posed by the continuous dumping of such wastes at the unlined landfills. Statistical analysis has been performed on the disposal and characterization of industrial wastewater and sludge at five active landfill sites. The chemical analysis shows that all the industrial wastes and sludge have high concentrations of COD, suspended solids, and heavy metals. Results show that from 1993 to 2000, 5.14{+-}1.13 million t of total wastes were disposed per year in all active landfill sites in Kuwait. The share of industrial liquid and sludge waste was 1.85{+-}0.19 million t representing 37.22{+-}6.85% of total waste disposed in all landfill sites. Such wastes contribute to landfill leachate which pollutes groundwater and may enter the food chain causing adverse health effects. Lined evaporation ponds are suggested as an economical and safe solution for industrial wastewater and sludge disposal in the arid climate of Kuwait.

  2. Sensitive quantification of isoprenoid cytokinins in plants by selective immunoaffinity purification and high performance liquid chromatography-quadrupole-time of flight mass spectrometry.

    PubMed

    Liang, Yuan; Zhu, Xiaocui; Zhao, Meiping; Liu, Huwei

    2012-02-01

    In this work, we developed a novel class-specific immunoaffinity column for the natural isoprenoid cytokinins (CTKs) by using trans-zeatin riboside as the hapten to generate a complete antigen. By combination with a mixed-mode solid phase extraction step for pre-cleanup and a high performance liquid chromatography-quadrupole-time of flight mass spectrometry for the quantification, an efficient analytical protocol was established which allowed simultaneous quantification of eight endogenous isoprenoid CTKs in Arabidopsis thaliana leaves with a wide linear range from 25 to 500pg/g fresh weight and a detection limit of 12.5pg/g fresh weight. The method will be very useful for comprehensive research on the networks of signaling interactions of the active phytohormones and their regulation of the plant functions. PMID:21867755

  3. Simultaneous enantioselective quantification of fluoxetine and norfluoxetine in human milk by direct sample injection using 2-dimensional liquid chromatography-tandem mass spectrometry.

    PubMed

    Alvim-Jr, Joel; Lopes, Bianca Rebelo; Cass, Quezia Bezerra

    2016-06-17

    A two-dimensional liquid chromatography system coupled to triple quadrupole tandem mass spectrometer (2D LC-MS/MS) was employed for the simultaneously quantification of fluoxetine (FLX) and norfluoxetine (NFLX) enantiomers in human milk by direct injection of samples. A restricted access media of bovine serum albumin octadecyl column (RAM-BSAC18) was used in the first dimension for the milk proteins depletion, while an antibiotic-based chiral column was used in the second dimension. The results herein described show good selectivity, extraction efficiency, accuracy, and precision with limits of quantification in the order of 7.5ngmL(-1)for the FLX enantiomers and 10.0ngmL(-1) for NFLX enantiomers. Furthermore, it represents a practical tool in terms of sustainability for the sample preparation of such a difficult matrix. PMID:27208983

  4. Development and validation of a liquid chromatography–tandem mass spectrometry assay for the simultaneous quantification of buprenorphine, norbuprenorphine, and metabolites in human urine

    PubMed Central

    Kacinko, Sherri L.; Concheiro-Guisan, Marta; Shakleya, Diaa M.; Huestis, Marilyn A.

    2009-01-01

    A liquid chromatography–tandem mass spec-trometry method for the simultaneous quantification of buprenorphine (BUP), norbuprenorphine (NBUP), buprenorphine glucuronide (BUP-Gluc), and norbuprenorphine glucuronide (NBUP-Gluc) in human urine was developed and fully validated. Extensive endogenous and exogenous interferences were evaluated and limits of quantification were identified empirically. Analytical ranges were 5−1,000 ng/mL for BUP and BUP-Gluc and 25−1,000 ng/mL for NBUP and NBUP-Gluc. Intra-assay and interassay imprecision were less than 17% and recovery was 93−116%. Analytes were stable at room temperature, at 4 °C, and for three freeze–thaw cycles. This accurate and precise assay has sufficient sensitivity and specificity for urine analysis of specimens collected from individuals treated with BUP for opioid dependence. PMID:18758763

  5. The determination and quantification of photosynthetic pigments by reverse phase high-performance liquid chromatography, thin-layer chromatography, and spectrophotometry.

    PubMed

    Pocock, Tessa; Król, Marianna; Huner, Norman P A

    2004-01-01

    Chorophylls and carotenoids are functionally important pigment molecules in photosynthetic organisms. Methods for the determination of chlorophylls a and b, beta-carotene, neoxanthin, and the pigments that are involved in photoprotective cycles such as the xanthophylls are discussed. These cycles involve the reversible de-epoxidation of violaxanthin into antheraxanthin and zeaxanthin, as well as the reversible de-epoxidation of lutein-5,6-epoxide into lutein. This chapter describes pigment extraction procedures from higher plants and green algae. Methods for the determination and quantification using high-performance liquid chromatograpy (HPLC) are described as well as methods for the separation and purification of pigments for use as standards using thin-layer chromatography (TLC). In addition, several spectrophotometric methods for the quantification of chlorophylls a and b are described. PMID:15187276

  6. [Determination of capsaicinoids and eugenol in waste-edible-oil by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry].

    PubMed

    Zhang, Zhong; Ren, Fei; Zhang, Pan

    2012-11-01

    A method was developed for the determination of capsaicinoids (capsaicin, dihydrocapsaicin and synthetic capsaicin) and eugenol in waste-edible-oil extracted by liquid-liquid extraction and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The capsaicinoids and eugenol in waste-edible-oil were extracted by methanol, and then separated by a SUPEL COSIL ABZ + Plus dC18 column (150 mm x4.6 mm, 5 microm). The analysis was performed by MS/MS with electrospray ionization in positive and negative ion modes with multiple reaction monitoring (MRM). The limits of detection for capsaicin, dihydrocapsaicin, synthetic capsaicin and eugenol were 0.02, 0.03, 0.03 and 0.6 microg/L, respectively. The good linear relationships were obtained in certain concentration ranges of capsaicinoids and eugenol. The relative standard deviations (RSDs, n=5) of same-worker and different-worker were less than 5%. The method is exclusive, sensitive and accurate, and can be used in waste-edible-oil determination. PMID:23451511

  7. Assessment and quantification of post-weaning multi-systemic wasting syndrome severity at farm level.

    PubMed

    Alarcon, Pablo; Velasova, Martina; Werling, Dirk; Stärk, Katharina D C; Chang, Yu-Mei; Nevel, Amanda; Pfeiffer, Dirk U; Wieland, Barbara

    2011-01-01

    Post-weaning multi-systemic wasting syndrome (PMWS) causes major economic losses for the English pig industry and severity of clinical signs and economic impact vary considerably between affected farms. We present here a novel approach to quantify severity of PMWS based on morbidity and mortality data and presence of porcine circovirus type 2 (PCV2). In 2008-2009, 147 pig farms across England, non-vaccinating for PCV2, were enrolled in a cross-sectional study. Factor analysis was used to generate variables representing biologically meaningful aspects of variation among qualitative and quantitative morbidity variables. Together with other known variables linked to PMWS, the resulting factors were included in a principal component analysis (PCA) to derive an algorithm for PMWS severity. Factor analysis resulted in two factors: Morbidity Factor 1 (MF1) representing mainly weaner and grower morbidity, and Morbidity Factor 2 (MF2) which mainly reflects variation in finisher morbidity. This indicates that farms either had high morbidity mainly in weaners/growers or mainly in finishers. Subsequent PCA resulted in the extraction of one component representing variation in MF1, post-weaning mortality and percentage of PCV2 PCR positive animals. Component scores were normalised to a value range from 0 to 10 and farms classified into: non or slightly affected farms with a score <4, moderately affected farms with scores 4-6.5 and highly affected farms with a score >6.5. The identified farm level PMWS severities will be used to identify risk factors related to these, to assess the efficacy of PCV2 vaccination and investigating the economic impact of potential control measures. PMID:21036410

  8. Predicting liquid immiscibility in multicomponent nuclear waste glasses

    SciTech Connect

    Peeler, D.K.; Hrma, P.R.

    1994-04-01

    Taylor`s model for predicting amorphous phase separation in complex, multicomponent systems has been applied to high-level (simulated) radioactive waste glasses at the US Department of Energy`s Hanford site. Taylor`s model is primarily based on additions of modifying cations to a Na{sub 2}O-B{sub 2}O{sub 3}-SiO{sub 2} (NBS) submixture of the multicomponent glass. The position of the submixture relative to the miscibility dome defines the development probability of amorphous phase separation. Although prediction of amorphous phase separation in Hanford glasses (via experimental SEM/TEM analysis) is the primary thrust of this work; reported durability data is also provides limited insight into the composition/durability relationship. Using a modified model similar to Taylor`s, the results indicate that immiscibility may be predicted for multicomponent waste glasses by the addition of Li{sub 2}O to the ``alkali`` corner of the NBS submixture.

  9. Utilization of municipal solid and liquid wastes for bioenergy and bioproducts production.

    PubMed

    Chen, Paul; Xie, Qinglong; Addy, Min; Zhou, Wenguang; Liu, Yuhuan; Wang, Yunpu; Cheng, Yanling; Li, Kun; Ruan, Roger

    2016-09-01

    Municipal wastes, be it solid or liquid, are rising due to the global population growth and rapid urbanization and industrialization. Conventional management practice involving recycling, combustion, and treatment/disposal is deemed unsustainable. Solutions must be sought to not only increase the capacity but also improve the sustainability of waste management. Research has demonstrated that the non-recyclable waste materials and bio-solids can be converted into useable heat, electricity, or fuel and chemical through a variety of processes, including gasification, pyrolysis, anaerobic digestion, and landfill gas in addition to combustion, and wastewater streams have the potential to support algae growth and provide other energy recovery options. The present review is intended to assess and analyze the current state of knowledge in the municipal solid wastes and wastewater treatment and utilization technologies and recommend practical solution options and future research and development needs. PMID:26996262

  10. Treatment options and flow sheets for ORNL low-level liquid waste supernate

    SciTech Connect

    Campbell, D.O.; Lee, D.D.

    1991-12-01

    Low-level liquid waste (LLLW) is currently contained in ten 50,000-gal storage and process tanks at Oak Ridge National Laboratory (ORNL) and as residual heels in an number of older tanks that are no longer in active use. Plans are being formulated to treat these wastes, along with similar LLLW that will be generated in the future, to yield decontaminated effluents that can be disposed of and stable solid waste forms that can be permanently stored. The primary purpose of this report is to summarize the performance of the most promising separations processes that are appropriate for treatment of the LLLW supernate solution to remove the two dominant radionuclides, {sup 137}Cs and {sup 90}Sr; to indicate how they can be integrated into an effective flowsheet; and to estimate the expected performance of such flowsheets in comparison to waste treatment requirements.

  11. Enhanced NH3 emission from swine liquid waste

    NASA Astrophysics Data System (ADS)

    Lee, S.; Robarge, W. P.; Walker, J. T.

    2010-12-01

    Swine animal feeding operations are sources of emissions for various gases [ammonia (NH3), hydrogen sulfide (H2S), carbon dioxide (CO2), volatile organic carbons (VOCs)], and fine particulate matter. Gaseous emissions from simple aqueous systems are typically controlled by temperature, pH, wind speed, total dissolved concentration of the chemical species of interest (e.g. NH3+NH4+ = TAN), and the Henry’s law constant. Ammonia emissions from three different sources [ammonium sulfate (AS), swine anaerobic lagoon liquid (SLL), and pit liquid (SPL) from swine housing units] were evaluated using a small flow-through teflon-lined chamber (SFTC; 0.3m × 0.2m × 0.15m) under controlled laboratory conditions. The SFTC was designed for 100% collection efficiency of NH3 gas emitted from the liquids. The internal volume of the chamber, 9 L, was exchanged 1.1 times per minute. All three liquid formulations exhibit the expected response in emissions with changes in temperature and pH. However, NH3 emissions from the SPL and SLL are ~5 times those from pure solutions of AS. Furthermore, the enhancement in NH3 emissions was a function of TAN concentration, decreasing in intensity at higher TAN and approaching rates comparable to the pure solutions of AS. The difference in emissions with solutions of equivalent TAN suggests a synergistic mechanism that is enhancing NH3 emissions in SPL and SLL. Concurrent measurements as part of the National Air Emissions Monitoring Study at the swine operations originally sampled for SPL and SLL document the emissions of CO2, H2S and VOCs (primarily acetic, propionic and butyric acids) at levels that are comparable to observed NH3 emissions. To date, only additions of NaHCO3 to the SPL and SLL have been found to enhance NH3 emissions and exhibit the same response to increasing TAN as exhibited by the original SPL and SLL solutions. Possible reactions that could enhance emissions will be discussed.

  12. Efficiency of inductively torch plasma operating at atmospheric pressure on destruction of chlorinated liquid wastes- A path to the treatment of radioactive organic halogen liquid wastes

    NASA Astrophysics Data System (ADS)

    Kamgang-Youbi, G.; Poizot, K.; Lemont, F.

    2012-12-01

    The performance of a plasma reactor for the degradation of chlorinated hydrocarbon waste is reported. Chloroform was used as a target for a recently patented destruction process based using an inductive plasma torch. Liquid waste was directly injected axially into the argon plasma with a supplied power of ~4 kW in the presence of oxygen as oxidant and carrier gas. Decomposition was performed at CHCl3 feed rates up to 400 g·h-1 with different oxygen/waste molar ratios, chloroform destruction was obtained with at least 99% efficiency and the energy efficiency reached 100 g·kWh-1. The conversion end products were identified and assayed by online FTIR spectroscopy (CO2, HCl and H2O) and redox titration (Cl2). Considering phosgene as representative of toxic compounds, only very small quantities of toxics were released (< 1 g·h-1) even with high waste feed rates. The experimental results were very close to the equilibrium composition predicted by thermodynamic calculations. At the bottom of the reactor, the chlorinated acids were successfully trapped in a scrubber and transformed into mineral salts, hence, only CO2 and H2O have been found in the final off-gases composition.

  13. Industrial Technology of Decontamination of Liquid Radioactive Waste in SUE MosSIA 'Radon' - 12371

    SciTech Connect

    Adamovich, Dmitry V.; Neveykin, Petr P.; Karlin, Yuri V.; Savkin, Alexander E.

    2012-07-01

    SUE MosSIA 'RADON' - this enterprise was created more than 50 years ago, which deals with the recycling of radioactive waste and conditioning of spent sources of radiation in stationary and mobile systems in the own factory and operating organizations. Here is represented the experience SUE MosSIA 'Radon' in the field of the management with liquid radioactive waste. It's shown, that the activity of SUE MosSIA 'RADON' is developing in three directions - improvement of technical facilities for treatment of radioactive waters into SUE MosSIA 'RADON' development of mobile equipment for the decontamination of radioactive waters in other organizations, development of new technologies for decontamination of liquid radioactive wastes as part of various domestic Russian and international projects including those related to the operation of nuclear power and nuclear submarines. SUE MosSIA 'RADON' has processed more than 270 thousand m{sup 3} of radioactive water, at that more than 7000 m{sup 3} in other organizations for more than 50 years. It is shown that a number of directions, particularly, the development of mobile modular units for decontamination of liquid radioactive waste, SUE MosSIA 'RADON' is a leader in the world. (authors)

  14. Treatment of Liquid Radioactive Waste with High Salt Content by Colloidal Adsorbents - 13274

    SciTech Connect

    Lee, Keun-Young; Chung, Dong-Yong; Kim, Kwang-Wook; Lee, Eil-Hee; Moon, Jei-Kwon

    2013-07-01

    Treatment processes have been fully developed for most of the liquid radioactive wastes generated during the operation of nuclear power plants. However, a process for radioactive liquid waste with high salt content, such as waste seawater generated from the unexpected accident at nuclear power station, has not been studied extensively. In this study, the adsorption efficiencies of cesium (Cs) and strontium (Sr) in radioactive liquid waste with high salt content were investigated using several types of zeolite with different particle sizes. Synthesized and commercial zeolites were used for the treatment of simulated seawater containing Cs and Sr, and the reaction kinetics and adsorption capacities of colloidal zeolites were compared with those of bulk zeolites. The experimental results demonstrated that the colloidal adsorbents showed fast adsorption kinetic and high binding capacity for Cs and Sr. Also, the colloidal zeolites could be successfully applied to the static adsorption condition, therefore, an economical benefit might be expected in an actual processes where stirring is not achievable. (authors)

  15. Condition assessment of the Los Alamos National Laboratory radioactive liquid waste collection system.

    SciTech Connect

    Edgemon, G. L.; Moss, W. D.; Worland, V. P.

    2004-01-01

    The radioactive liquid waste collection system (RLWCS) at Los Alamos National Laboratory (LANE) is a site-wide double-encased piping system installed in 1982 that allows radioactive liquid waste (RLW) producing facilities to gravity drain their waste to the radioactive liquid waste treatment facility (RLWTF) through a system of underground high-density polyethylene (HDPE) pipes and vaults. The RLWCS stretches approximately four miles and typically receives approximately 10,000 gallons of RLW per day for treatment at the RLWTF. Uncertainty of the current condition of the RLWCS was recently identified as a potential risk to the future continued availability of the RLW treatment function. A condition assessment was performed in April 2004 to evaluate the risks and estimate the remaining useful life of the existing RLWCS. Several representative and 'worst-case' RLWCS primary piping sections and their associated inspection vaults were selected for direct visual assessment, remote borescopic examination, and in-situ durometer testing. This field investigation combined with an RLWCS materials compatibility review showed that the primary piping of the RLWCS is in relatively good condition, with only a few noteworthy areas of degradation.

  16. Quantification of 8-α-hydroxy-mutilin as marker residue for tiamulin in rabbit tissues by high-performance liquid chromatography-mass spectrometry.

    PubMed

    De Baere, Siegrid; Devreese, Mathias; Maes, An; De Backer, Patrick; Croubels, Siska

    2015-06-01

    For the first time, a sensitive and specific method was developed and fully validated for the quantification of the EU marker residue of tiamulin, 8-α-hydroxy-mutilin, in rabbit muscle and liver tissues using liquid chromatography combined with positive heated electrospray ionization triple quadrupole mass spectrometry. The mass spectrometer was operated in the selected reaction monitoring (SRM) mode with selection of the [M + H](+) ion in both quadrupoles 1 and 3, resulting in the SRM transition m/z 337.25 > 337.25 for quantification. Chromatography was performed using a Hypersil Gold C18 column using a gradient elution program with water and methanol as mobile phases. The sample preparation procedure for the analysis of 8-α-hydroxy-mutilin in liver and muscle samples consisted of three main steps: (1) extraction of the tissue matrix using 0.1 N hydrochloric acid/acetone (50/50, v/v), (2) hydrolysis of tiamulin and metabolites to 8-α-hydroxy-mutilin in alkaline medium at 45 °C, and (3) liquid-liquid extraction in acidic medium using ethyl acetate. This is the first method presenting fully validated results, encompassing a linearity of 50 to 2,000 μg/kg, within-run and between-run accuracy and precision, limit of quantification (50 μg/kg for both muscle and liver tissues), limit of detection (muscle, 11.9 μg/kg; liver, 20.6 μg/kg), extraction recovery (muscle, 66.2%; liver, 75.5%), signal suppression and enhancement (muscle, 51.7%; liver, 43.3%), carryover, applicability and practicability, and stability during storage and analysis. This novel method is therefore sensitive enough to be used for residue depletion studies of tiamulin in rabbits and for food safety monitoring with respect to MRL compliance of residues. PMID:25592328

  17. Development of a liquid chromatography tandem mass spectrometry method for trace analysis of trisiloxane surfactants in the aqueous environment: an alternative strategy for quantification of ethoxylated surfactants.

    PubMed

    Michel, Amandine; Brauch, Heinz-Jürgen; Worch, Eckhard; Lange, Frank T

    2012-07-01

    Trisiloxane surfactants, often referred to as superspreaders or superwetters, are added to pesticides to enhance the activity and the rainfastness of the active substance by promoting rapid spreading over hydrophobic surfaces. To fill the lack of data on the environmental occurrence of these compounds, we have developed and validated a method for their trace analysis in the aqueous environment. The method is based on liquid-liquid extraction followed by liquid chromatography and tandem mass spectrometry. The oligomeric distribution of trisiloxane surfactant in a reference solution was determined by a theoretical calculation and by experimental measurements. Based on these results, the quantification was performed by comparison with a calibration made with a single homologue instead of a mixture of homologues. This approach avoids a time-consuming synthesis of pure homologues and reduces the risk of wrong estimation of the concentration because of different response factors of the sample and the standard. Such an approach could be applied to the quantification of other ethoxylated surfactants following a similar distribution. The validation was performed from 2 to 250 ng/L (total surfactant concentration) in deionized water, tap water, and river water (Rhine water). Knowing the oligomeric distribution of the polymer in the reference solution, the corresponding calibration ranges were estimated for individual homologues. Limits of quantification were found to be between 0.37 ng/L and 15 ng/L. The total recovery of sample preparation was between 77% and 116%. Matrix effects were lower than 10% with river water and the relative standard deviation evaluated over ten identical samples of spiked river water was below 12%. PMID:22658138

  18. The Utilization of Banana Peel in the Fermentation Liquid in Food Waste Composting

    NASA Astrophysics Data System (ADS)

    Kadir, A. A.; Rahman, N. A.; Azhari, N. W.

    2016-07-01

    Municipal solid waste in Malaysia contains a high amount of organic matters, particularly food waste. Food waste represents almost 60% from the total municipal solid waste disposed in the landfill. Food waste can be converted into useful materials such as compost. However, source separation of food waste for recycling is not commonly practiced in Malaysia due to various constraints. These constraints include low awareness among the waste generators and low demand of the products produced from the food waste such as composts. Composting is one of the alternatives that can be used in food waste disposal from Makanan Ringan Mas. The aim of the study is to convert food waste generated from Makanan Ringan Mas which is a medium sale industry located at Parit Kuari Darat, Batu Pahat by using composting method. The parameters which include temperature, pH value, NPK (Nitrogen, Phosphorus, Potassium) values has been examined. Banana peel is being used as the fermentation liquid whilst soil and coconut husk were used as the composting medium. Based on the results during the composting process, most of the pH value in each reactor is above 5 and approximately at neutral. This shown that the microbial respiration in the well controlled composting reactor was inhibited and had approached the mature phase. On the other hand, during the period of composting, the overall temperature range from 25 °C to 47 °C which shown the active phase for composting will occoured. As for NPK content Nitrogen value range is 35325 mg/L to 78775 mg/L, Phosphorus, 195.83 mg/L to 471 mg/L and potassium is 422.3 mg/L to 2046 mg/L which is sufficient to use for agricultural purpose. The comparison was made with available organic compost in the market and only showed slightly difference. Nevertheless, in comparison with common fertilizer, the NPK value of organic compost are considerably very low.

  19. High-temperature vitrification of Hanford residual-liquid waste in a continuous melter

    SciTech Connect

    Barnes, S.M.

    1980-04-01

    Over 270 kg of high-temperature borosilicate glass have been produced in a series of three short-term tests in the High-Temperature Ceramic Melter vitrification system at PNL. The glass produced was formulated to vitrify simulated Hanford residual-liquid waste. The tests were designed to (1) demonstrate the feasibility of utilizing high-temperature, continuous-vitrification technology for the immobilization of the residual-liquid waste, (2) test the airlift draining technique utilized by the high-temperature melter, (3) compare glass produced in this process to residual-liquid glass produced under laboratory conditions, (4) investigate cesium volatility from the melter during waste processing, and (5) determine the maximum residual-liquid glass production rate in the high-temperature melter. The three tests with the residual-liquid composition confirmed the viability of the continuous-melting vitrification technique for the immobilization of this waste. The airlift draining technique was demonstrated in these tests and the glass produced from the melter was shown to be less porous than the laboratory-produced glass. The final glass produced from the second test was compared to a glass of the same composition produced under laboratory conditions. The comparative tests found the glasses to be indistinguishable, as the small differences in the test results fell within the precision range of the characterization testing equipment. The cesium volatility was examined in the final test. This examination showed that 0.44 wt % of the cesium (assumed to be cesium oxide) was volatilized, which translates to a volatilization rate of 115 mg/cm/sup 2/-h.

  20. Simultaneous quantification of 28 synthetic cathinones and metabolites in urine by liquid chromatography-high resolution mass spectrometry.

    PubMed

    Concheiro, Marta; Anizan, Sebastien; Ellefsen, Kayla; Huestis, Marilyn A

    2013-11-01

    Synthetic cathinones are novel stimulants derived from cathinone, with amphetamines or cocaine-like effects, often labeled "not for human consumption" and considered "legal highs". Emergence of these new designer drugs complicate interpretation of forensic and clinical cases, with introduction of many new analogs designed to circumvent legislation and vary effects and potencies. We developed a method for the simultaneous quantification of 28 synthetic cathinones, including four metabolites, in urine by liquid chromatography coupled to high resolution mass spectrometry (LC-HRMS). These cathinones include cathinone, methcathinone, and synthetic cathinones position-3'-substituted, N-alkyl-substituted, ring-substituted, methylenedioxy-substituted, and pyrrolidinyl-substituted. One mL phosphate buffer pH 6 and 25 μL IStd solution were combined with 0.25 mL urine, and subjected to solid phase cation exchange extraction (SOLA SCX). The chromatographic reverse-phase separation was achieved with a gradient mobile phase of 0.1 % formic acid in water and in acetonitrile in 20 min. We employed a Q Exactive high resolution mass spectrometer, with compounds identified and quantified by target-MSMS experiments. The assay was linear from 0.5-1 to 100 μg/L, with limits of detection of 0.25-1 μg/L. Imprecision (n = 20) was <15.9 % and accuracy (n = 20) 85.2-118.1 %. Extraction efficiency was 78.9-116.7 % (CV 1.4-16.7 %, n = 5), process efficiency 57.7-104.9 %, and matrix effects from -29.5 % to 1.5 % (CV 1.9-13.1 %, n = 10). Most synthetic cathinones were stable at 4 °C for 72 h (n = 27) and after 3 freeze-thaw cycles (n = 26), but many (n = 19) were not stable at room temperature for 24 h (losses up to -67.6 %). The method was applied to authentic urine specimens from synthetic cathinone users. This method provides a comprehensive confirmation method for 28 synthetic cathinones in urine, with good selectivity and specificity. PMID:24196122

  1. Preliminary evaluation of evaluation of the efficiency of aircraft liquid waste treatment using resolvable sanitizing liquid: a case study in Changchun.

    PubMed

    Xu, Jianling; Yang, Jiaqi; Zhao, Nan; Sheng, Lianxi; Zhao, Yuanhui; Tang, Zhanhui

    2011-12-01

    The physical, chemical, and biological indices of aircraft liquid wastes collected from multiple airplanes at Longjia Airport, Changchun, China were measured according to "Integrated Wastewater Discharge Standard," evaluating treatment efficiency of resolvable sanitizing liquid. The results indicate that, after being treated by the resolvable sanitizing liquid, the indices of all first-class pollutants met the requirements of the standard, while among the second-class pollutants, the suspension content, biochemical oxygen demand after 5 days, and chemical oxygen demand as well as the contents of amino nitrogen, total phosphorus, anionic surfactants, total copper, absorbable organic halogen, and phenolic compounds did not reach the discharge standard. Particularly, the level of fecal coliform bacteria in the aircraft liquid wastes can meet the standard specification by adding more than 1 mL/L resolvable sanitizing liquid. The aircraft wastewater treated by resolvable sanitizing liquid cannot be directly discharged back into the environment as well as urban drainage systems. PMID:21340546

  2. Validation of the physico-chemical processes determining the state of the components of liquid nuclear wastes in underground repositories

    SciTech Connect

    Kosareva, I.M.; Savushkina, M.K.; Egorov, N.N.; Kudryavtsev, E.G.; Chizhikov, V.S.; Korotkevich, V.M.; Revenko, Yu.A.; Nosukhin, A.V.

    1995-12-31

    This paper presents the results of a study of the physico-chemical properties of liquid nuclear wastes formed during the treatment of wastes of nuclear enterprises and nuclear power plants. The parameters of underground layers which can be used for the disposal of liquid nuclear wastes are discussed. When wastes are injected into a collector layer, various chemical interactions occur which may change the compositions of the wastes and the collector layer. To predict the state of the waste components during the dangerous period of the repository operation, a physico-chemical study of the processes occurring in nuclear waste repositories was carried out. For each type of waste, main peculiarities of possible transformations, including chemical interactions, hydrolysis, thermolysis, radiolysis, and sorption were determined. The disposal of liquid nuclear wastes into deep geological formations is a unique pilot experiment on the concentration of liquid nuclear wastes in a comparatively small area of an underground collector layer. This makes the implementation of the method and the period after the end of the operation of the repositories, i.e., their conservation, essential stages of this work. The development of the method of disposing of liquid nuclear wastes deep in water-bearing layers was carried out along several lines: (1) a comprehensive geohydrological study of the matter; (2) a study of the physico-chemical conditions of the disposal; (3) solution of scientific and technological problems; and (4) control and assessment of sanitary radiation safety. To exercise control over the state of deep underground repositories of liquid nuclear wastes, various mathematical models are being developed.

  3. Savannah River Site, Liquid Waste Program, Savannah River Remediation American Recovery and Reinvestment Act Benefits and Lessons Learned - 12559

    SciTech Connect

    Schmitz, Mark A.; Crouse, Thomas N.

    2012-07-01

    Utilizing funding provided by the American Recovery and Reinvestment Act (ARRA), the Liquid Waste Program at Savannah River site successfully executed forty-one design, procurement, construction, and operating activities in the period from September 2009 through December 2011. Project Management of the program included noteworthy practices involving safety, integrated project teams, communication, and cost, schedule and risk management. Significant upgrades to plant capacity, progress toward waste tank closure and procurement of needed infrastructure were accomplished. Over 1.5 million hours were worked without a single lost work day case. Lessons Learned were continually identified and applied to enhance the program. Investment of Recovery Act monies into the Liquid Waste Program has ensured continued success in the disposition of radioactive wastes and the closure of high level waste tanks at SRS. The funding of a portion of the Liquid Waste Program at SRS by ARRA was a major success. Significant upgrades to plant capacity, progress toward waste tank closure and procurement of needed infrastructure was accomplished. Integrated Project Teams ensured quality products and services were provided to the Operations customers. Over 1.5 million hours were worked without a single lost work day case. Lessons Learned were continually reviewed and reapplied to enhance the program. Investment of Recovery Act monies into the Liquid Waste Program has ensured continued success in the disposition of radioactive wastes and the closure of high level waste tanks at SRS. (authors)

  4. Decontamination of Nuclear Liquid Wastes Status of CEA and AREVA R and D: Application to Fukushima Waste Waters - 12312

    SciTech Connect

    Fournel, B.; Barre, Y.; Lepeytre, C.; Peycelon, H.; Grandjean, A.; Prevost, T.; Valery, J.F.; Shilova, E.; Viel, P.

    2012-07-01

    Liquid wastes decontamination processes are mainly based on two techniques: Bulk processes and the so called Cartridges processes. The first technique has been developed for the French nuclear fuel reprocessing industry since the 60's in Marcoule and La Hague. It is a proven and mature technology which has been successfully and quickly implemented by AREVA at Fukushima site for the processing of contaminated waters. The second technique, involving cartridges processes, offers new opportunities for the use of innovative adsorbents. The AREVA process developed for Fukushima and some results obtained on site will be presented as well as laboratory scale results obtained in CEA laboratories. Examples of new adsorbents development for liquid wastes decontamination are also given. A chemical process unit based on co-precipitation technique has been successfully and quickly implemented by AREVA at Fukushima site for the processing of contaminated waters. The asset of this technique is its ability to process large volumes in a continuous mode. Several chemical products can be used to address specific radioelements such as: Cs, Sr, Ru. Its drawback is the production of sludge (about 1% in volume of initial liquid volume). CEA developed strategies to model the co-precipitation phenomena in order to firstly minimize the quantity of added chemical reactants and secondly, minimize the size of co-precipitation units. We are on the way to design compact units that could be mobilized very quickly and efficiently in case of an accidental situation. Addressing the problem of sludge conditioning, cementation appears to be a very attractive solution. Fukushima accident has focused attention on optimizations that should be taken into account in future studies: - To better take account for non-typical aqueous matrixes like seawater; - To enlarge the spectrum of radioelements that can be efficiently processed and especially short lives radioelements that are usually less present in

  5. Supported liquid membranes in radioactive waste treatment processes: Recent experience and perspective

    SciTech Connect

    Nechaev, A.F.; Projaev, V.V.; Kapranchik, V.P.

    1995-12-31

    Recent experience in practical application of Supported Liquid Membranes (SLM or SUPLIM) both in the hydrometallurgy and nuclear technology has been analyzed. The results obtained allow one to consider SUPLIM as a promising technology for radioactive waste treatment. This statement is based on the evaluation of integrated socioeconomic effects, including quantity of additional chemicals, the volume of secondary technological streams and secondary wastes, simplicity and the low costs of equipment used, potential possibility to organize in situ process, and the level of the harmful impact on personnel. 35 refs.

  6. Drop Dynamics and Speciation in Isolation of Metals from Liquid Wastes by Reactive Scavenging

    SciTech Connect

    Arne J. Pearlstein; Alexander Scheeline

    2002-08-30

    Computational and experimental studies of the motion and dynamics of liquid drops in gas flows were conducted with relevance to reactive scavenging of metals from atomized liquid waste. Navier-Stoke's computations of deformable drops revealed a range of conditions from which prolate drops are expected, and showed how frajectiones of deformable drops undergoing deceleration can be computed. Experimental work focused on development of emission fluorescence, and scattering diagnostics. The instrument developed was used to image drop shapes, soot, and nonaxisymmetric departures from steady flow in a 22kw combustor

  7. Selective separation of hydroxide from alkaline nuclear tank waste by liquid-liquid extraction with weak hydroxy acids.

    PubMed

    Chambliss, C Kevin; Haverlock, Tamara I; Bonnesen, Peter V; Engle, Nancy L; Moyer, Bruce A

    2002-04-15

    Recovery and recycle of caustic reagents in industrial processes offer potential means of pollution prevention, as investigated herein for particular needs related to the cleanup of alkaline nuclear waste. Specifically, the recovery of hydroxide from alkaline media by liquid-liquid extraction can be effected utilizing weak hydroxy acids, as demonstrated for NaOH utilizing a series of lipophilic fluorinated alcohols and alkylated phenols dissolved in 1-octanol. Extraction efficiency follows the expected order of acidity of the hydroxy acids, the phenols being the most efficient extractants among the compounds tested. After extraction, NaOH is effectively recoverable from the organic phase upon contact with water. The weakest hydroxy acids are the most efficiently stripped, NaOH recovery being nearly quantitative in a single contact. In competitive extraction experiments, good selectivity for hydroxide recovery over other anions such as nitrate and chloride was demonstrated. Since the order of extraction favors larger anions, the exceptional preference for hydroxide implies that the extraction occurs by deprotonation of the hydroxy acids in a cation-exchange process. Stripping therefore occurs by hydrolysis to regenerate the neutral hydroxy acid, liberating NaOH to the aqueous phase. Since hydroxide equivalents rather than actual hydroxide ions are transferred to the solvent, the process is termed "pseudohydroxide extraction." Hydroxide recovery from a simulant of alkaline nuclear tank waste (Hanford DSSF simulant) was also demonstrated in repeated extraction and stripping cycles. PMID:11993889

  8. Validated Method for the Quantification of Baclofen in Human Plasma Using Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

    PubMed

    Nahar, Limon Khatun; Cordero, Rosa Elena; Nutt, David; Lingford-Hughes, Anne; Turton, Samuel; Durant, Claire; Wilson, Sue; Paterson, Sue

    2016-03-01

    A highly sensitive and fully validated method was developed for the quantification of baclofen in human plasma. After adjusting the pH of the plasma samples using a phosphate buffer solution (pH 4), baclofen was purified using mixed mode (C8/cation exchange) solid-phase extraction (SPE) cartridges. Endogenous water-soluble compounds and lipids were removed from the cartridges before the samples were eluted and concentrated. The samples were analyzed using triple-quadrupole liquid chromatography-tandem mass spectrometry (LC-MS-MS) with triggered dynamic multiple reaction monitoring mode for simultaneous quantification and confirmation. The assay was linear from 25 to 1,000 ng/mL (r(2) > 0.999; n = 6). Intraday (n = 6) and interday (n = 15) imprecisions (% relative standard deviation) were <5%, and the average recovery was 30%. The limit of detection of the method was 5 ng/mL, and the limit of quantification was 25 ng/mL. Plasma samples from healthy male volunteers (n = 9, median age: 22) given two single oral doses of baclofen (10 and 60 mg) on nonconsecutive days were analyzed to demonstrate method applicability. PMID:26538544

  9. Simultaneous absolute quantification of 11 cytochrome P450 isoforms in human liver microsomes by liquid chromatography tandem mass spectrometry with in silico target peptide selection.

    PubMed

    Kawakami, Hirotaka; Ohtsuki, Sumio; Kamiie, Junichi; Suzuki, Takashi; Abe, Takaaki; Terasaki, Tetsuya

    2011-01-01

    Cytochrome P450 (CYP) proteins are involved in the biological oxidation and reduction of xenobiotics, affecting the pharmacological efficiency of drugs. This study aimed to establish a method to simultaneously quantify 11 CYP isoforms by multiplexed-multiple reaction monitoring analysis with liquid chromatography tandem mass spectrometry and in silico peptide selection to clarify CYP isoform expression profiles in human liver tissue. CYP1A2, 2A6, and 2D6 target peptides were identified by shot-gun proteomic analysis, and those of other isoforms were selected by in silico peptide selection criteria. The established quantification method detected target peptides at 10  fmol, and the dynamic range of calibration curves was at least 500-fold. The quantification value of CYP1A2 in Supersomes was not significantly different between the established method and quantitative immunoblot analysis. The absolute protein expression levels of 11 CYP isoforms were determined from one pooled and 10 individual human liver microsomes. In the individual microsomes, CYP2C9 showed the highest protein expression level, and CYP1A2, 2A6, 2C19, and 3A4 protein expression exhibited more than a 20-fold difference among individuals. This highly sensitive and selective quantification method is a useful tool for the analysis of highly homologous CYP isoforms and the contribution made by each CYP isoform to drug metabolism. PMID:20564338

  10. Possible Overestimation of Surface Disinfection Efficiency by Assessment Methods Based on Liquid Sampling Procedures as Demonstrated by In Situ Quantification of Spore Viability ▿

    PubMed Central

    Grand, I.; Bellon-Fontaine, M.-N.; Herry, J.-M.; Hilaire, D.; Moriconi, F.-X.; Naïtali, M.

    2011-01-01

    The standard test methods used to assess the efficiency of a disinfectant applied to surfaces are often based on counting the microbial survivors sampled in a liquid, but total cell removal from surfaces is seldom achieved. One might therefore wonder whether evaluations of microbial survivors in liquid-sampled cells are representative of the levels of survivors in whole populations. The present study was thus designed to determine the “damaged/undamaged” status induced by a peracetic acid disinfection for Bacillus atrophaeus spores deposited on glass coupons directly on this substrate and to compare it to the status of spores collected in liquid by a sampling procedure. The method utilized to assess the viability of both surface-associated and liquid-sampled spores included fluorescence labeling with a combination of Syto 61 and Chemchrome V6 dyes and quantifications by analyzing the images acquired by confocal laser scanning microscopy. The principal result of the study was that the viability of spores sampled in the liquid was found to be poorer than that of surface-associated spores. For example, after 2 min of peracetic acid disinfection, less than 17% ± 5% of viable cells were detected among liquid-sampled cells compared to 79% ± 5% or 47% ± 4%, respectively, when the viability was evaluated on the surface after or without the sampling procedure. Moreover, assessments of the survivors collected in the liquid phase, evaluated using the microscopic method and standard plate counts, were well correlated. Evaluations based on the determination of survivors among the liquid-sampled cells can thus overestimate the efficiency of surface disinfection procedures. PMID:21742922

  11. Investigation and development of liquid-liquid extraction systems for the removal of pertechnetate from aqueous nuclear waste stream simulants

    NASA Astrophysics Data System (ADS)

    Gansle, Kristina Marie Rohal

    1998-11-01

    The solvent extraction behavior of perrhenate (ReO 4-) and pertechnetate (TcO4- ) from aqueous nuclear waste stream simulants was examined using the anion-exchange reagent Aliquat-336 nitrate. The extraction tendencies of ReO 4- followed those of TcO4- from both acidic and basic media, demonstrating that ReO4 - was a suitable nonradioactive surrogate for TcO4 -. For ICP-AES analysis of Re in high salt solutions, a V-groove nebulizer and 1:1 dilution of the sample and standards with 0.1% Triton X-100 surfactant reduced deposition of solids within the sample introduction system, thus minimizing memory effects. A new approach to waste remediation technology, Redox-Recyclable Extraction and Recovery (R2ER), was also studied. The redox-active species 1,1',3,3'-tetrakis(2-methyl-2-hexyl)ferrocene (HEP) was oxidized to its cationic form for extraction of TcO4 - or ReO4- from aqueous waste and reduced to its neutral form for recovery of the anion. The thermodynamics of liquid-liquid interfacial electron transfer for the oxidation/activation of HEP were shown to be controlled by three factors: the reduction potentials of the redox-active species in the aqueous and organic phases and the transfer of an ion across the liquid-liquid interface. The deactivation/reduction rate of HEP+NO3- by iron was affected by organic solvent diluent and improved by treating the iron with hexanes and 1 M HCl. The volume of solid secondary-waste in the R2ER cycle was reduced by a factor of 3000. In complete extraction/recovery cycles, HEP+NO3- in 2-nonanone removed greater than 99% TcO4- from the 101-SY, 103-SY, 1 M HCl and 1 M NaOH/1.5 M NaNO3 Hanford Tank waste simulants. Another redox-active extractant, bis(hydridotris(1-pyrazolyl)borato)iron(III) nitrate (FeTp2+NO3-), was also selective for ReO4- remediation from simulated aqueous waste. Organic solutions of the alkyl substituted ferricenium extractants were not stable in the presence of nucleophilic anions and/or reducing agents. HEP+NO3

  12. SOLIEX: A Novel Solid-Liquid Method of Radionuclides Extraction from Radioactive Waste Solutions - 13486

    SciTech Connect

    Shilova, E.; Viel, P.; Huc, V.

    2013-07-01

    This paper describes recent developments in new solid-liquid extraction method, called SOLIEX, to remove cesium from alkaline solutions. SOLIEX relies on the use of a reversible complexing system comprising a carbon felt bearing molecular traps (calixarenes). This complexing system exhibits a high selectivity for Cs, and is thus expected to be helpful for the treatment of highly diluted cesium wastes even with a high concentration of competing alkali metal cations. As additional advantage, this complexing system can be adapted by molecular engineering to capture other radionuclides, such as Sr, Eu, Am. Finally, this complexing system can be easily and efficiently regenerated by using a cost effective stripping procedure, which limits further generation of waste to meet 'zero liquid' discharge requirements for nuclear facilities. (authors)

  13. Chemical constituents and antioxidant activities of waste liquid extract from Apostichopus japonicus Selenka processing

    NASA Astrophysics Data System (ADS)

    Li, Chaofeng; Li, Xiancui; Li, Hong; Guo, Shuju; Zhu, Xiaobin

    2013-07-01

    Apos tichopus japonicus Selenka is an ideal tonic food that is used traditionally in many Asian countries, and it contains many bioactive substances, such as antioxidant, antimicrobial, and anticancer materials. To convert waste liquid generated during production into a useful resource, extract from waste liquid was isolated by column chromatography and studied by the pyrogallol autoxidation and 1,10-phenanthroline-Fe2+ oxidation methods. Results show that the extract scavenged about 91% of the superoxide anion radical at a concentration of 1.4 mg/mL and 24% of the hydroxyl radical at 3.3 mg/mL. Four compounds were isolated and identified from the extract: 2,4-dihydroxy-5-methyl-1,3-azine; 2,4-dihydroxy-1,3-diazine; 3-O-[β-D-quinovopranosyl-(1→2)-4-O-sodium sulfate-β-D-xylopranosyl]-holosta-9(11)-ene-3β,12α,17α-triol; and 24-ethyl-5α-cholesta-7-ene-3β-O-β-D-xylopyranoside. All of these compounds are known in A. japonicus, and were found in the waste liquid for the first time.

  14. Disposal of liquid wastes by injection underground--Neither myth nor millennium

    USGS Publications Warehouse

    Piper, Arthur M.

    1969-01-01

    Injecting liquid wastes deep underground is an attractive but not necessarily practical means for disposing of them. For decades, impressive volumes of unwanted oil-field brine have been injected, currently about 10,000 acre-feet yearly. Recently, liquid industrial wastes are being injected in ever-increasing quantity. Dimensions of industrial injection wells range widely but the approximate medians are: depth, 2,660 feet; thickness of injection zone, 185 feet; injection rate, 135 gallons per minute; wellhead injection pressure, 185 pounds per square inch. Effects of deep injection are complex and not all are understood clearly. In a responsible society, injection cannot be allowed to put wastes out of mind. Injection is no more than storage--for all time in the case of the most intractable wastes--in underground space of which little is attainable in some areas and which is exhaustible in most areas. Liquid wastes range widely in character and concentration-some are incompatible one with another or with materials of the prospective injection zone; some which are reactive or chemically unstable would require pretreatment or could not be injected. Standards by which to categorize the wastes are urgently desirable. To the end that injection may be planned effectively and administered in orderly fashion, there is proposed an immediate and comprehensive canvass of all the United States to outline injection provinces and zones according to their capacities to accept waste. Much of the information needed to this end is at hand. Such a canvass would consider (1) natural zone, of groundwater circulation, from rapid to stagnant, (2) regional hydrodynamics, (3) safe injection pressures, and (4) geochemical aspects. In regard to safe pressure, definitive criteria would be sought by which to avoid recurrence of earthquake swarms such as seem to have been triggered by injection at the Rocky Mountain Arsenal well near Denver, Colo. Three of the 50 States--Missouri, .Ohio, and

  15. Deployment of Performance Management Methodology as part of Liquid Waste Program at Savannah River Site - 12178

    SciTech Connect

    Prod'homme, A.; Drouvot, O.; Gregory, J.; Barnes, B.; Hodges, B.; Hart, M.

    2012-07-01

    In 2009, Savannah River Remediation LLC (SRR) assumed the management lead of the Liquid Waste (LW) Program at the Savannah River Site (SRS). The four SRR partners and AREVA, as an integrated subcontractor are performing the ongoing effort to safely and reliably: - Close High Level Waste (HLW) storage tanks; - Maximize waste throughput at the Defense Waste Processing Facility (DWPF); - Process salt waste into stable final waste form; - Manage the HLW liquid waste material stored at SRS. As part of these initiatives, SRR and AREVA deployed a performance management methodology based on Overall Equipment Effectiveness (OEE) at the DWPF in order to support the required production increase. This project took advantage of lessons learned by AREVA through the deployment of Total Productive Maintenance and Visual Management methodologies at the La Hague reprocessing facility in France. The project also took advantage of measurement data collected from different steps of the DWPF process by the SRR team (Melter Engineering, Chemical Process Engineering, Laboratory Operations, Plant Operations). Today the SRR team has a standard method for measuring processing time throughout the facility, a reliable source of objective data for use in decision-making at all levels, and a better balance between engineering department goals and operational goals. Preliminary results show that the deployment of this performance management methodology to the LW program at SRS has already significantly contributed to the DWPF throughput increases and is being deployed in the Saltstone facility. As part of the liquid waste program on Savannah River Site, SRR committed to enhance production throughput of DWPF. Beyond technical modifications implemented at different location of the facility, SRR deployed performance management methodology based on OEE metrics. The implementation benefited from the experience gained by AREVA in its own facilities in France. OEE proved to be a valuable tool in order

  16. Parallel ultra high pressure liquid chromatography-mass spectrometry for the quantification of HIV protease inhibitors using dried spot sample collection format.

    PubMed

    Watanabe, Kyoko; Varesio, Emmanuel; Hopfgartner, Gérard

    2014-08-15

    An assay was developed and validated for the quantification of eight protease inhibitors (indinavir (IDV), ritonavir (RTV), lopinavir (LPV), saquinavir (SQV), amprenavir (APV), nelfinavir (NFV), atazanavir (AZV) and darunavir (DRV)) in dried plasma spots using parallel ultra-high performance liquid chromatography and mass spectrometry detection in the multiple reaction monitoring mode. For each analyte an isotopically labeled internal standard was used and the assay based on liquid-solid extraction the area response ratio (analyte/IS) was found to be linear; from 0.025 μg/ml to 20 μg/ml for IDV, SQV, DRV, AZV, LPV, from 0.025 μg/ml to 10 μg/ml for NFV, APV and from 0.025 μg/ml to 5 μg/ml for RTV using 15 μl of plasma spotted on filter paper placed in a sample tube. The total analysis time was of 4 min and inter-assay accuracies and precisions were in the range of 87.7-109% and 2.5-11.8%, respectively. On dried plasma spots all analytes were found to be stable for at least 7 days. Practicability of the assay to blood was also demonstrated. The sample drying process could be reduced to 5 min using a commercial microwave system without any analyte degradation. Together with quantification, confirmatory analysis was performed on representative clinical samples. PMID:25049214

  17. Ultrapressure liquid chromatography-tandem mass spectrometry assay using atmospheric pressure photoionization (UPLC-APPI-MS/MS) for quantification of 4-methoxydiphenylmethane in pharmacokinetic evaluation.

    PubMed

    Farhan, Nashid; Fitzpatrick, Sean; Shim, Yun M; Paige, Mikell; Chow, Diana Shu-Lian

    2016-09-01

    4-Methoxydiphenylmethane (4-MDM), a selective augmenter of Leukotriene A4 Hydrolase (LTA4H), is a new anti-inflammatory compound for potential treatment of chronic obstructive pulmonary disease (COPD). Currently, there is no liquid chromatography tandem mass spectrometric (LC-MS/MS) method for the quantification of 4-MDM. A major barrier for developing the LC-MS/MS method is the inability of electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) to ionize 4-MDM due to its hydrophobicity and lack of any functional group for ionization. With the advent of atmospheric pressure photoionization (APPI) technique, many hydrophobic compounds have been demonstrated to ionize by charge transfer reactions. In this study, a highly sensitive ultrapressure liquid chromatography tandem mass spectrometry assay using atmospheric pressure photoionization (UPLC-APPI-MS/MS) for the quantifications of 4-MDM in rat plasma has been developed and validated. 4-MDM was extracted from the plasma by solid phase extraction (SPE) and separated chromatographically using a reverse phase C8 column. The photoionization (PI) was achieved by introducing anisole as a dopant to promote the reaction of charge transfer. The assay with a linear range of 5 (LLOQ)-400ngmL(-1) met the regulatory requirements for accuracy, precision and stability. The validated assay was employed to quantify the plasma concentrations of 4-MDM after an oral dosing in Sprague Dawley (SD) rats. PMID:27232150

  18. Simultaneous quantification of the major bile acids in artificial Calculus bovis by high-performance liquid chromatography with precolumn derivatization and its application in quality control.

    PubMed

    Shi, Yan; Xiong, Jing; Sun, Dongmei; Liu, Wei; Wei, Feng; Ma, Shuangcheng; Lin, Ruichao

    2015-08-01

    An accurate and sensitive high-performance liquid chromatography method coupled with ultralviolet detection and precolumn derivatization was developed for the simultaneous quantification of the major bile acids in Artificial Calculus bovis, including cholic acid, hyodeoxycholic acid, chenodeoxycholic acid, and deoxycholic acid. The extraction, derivatization, chromatographic separation, and detection parameters were fully optimized. The samples were extracted with methanol by ultrasonic extraction. Then, 2-bromine-4'-nitroacetophenone and 18-crown ether-6 were used for derivatization. The chromatographic separation was performed on an Agilent SB-C18 column (250 × 4.6 mm id, 5 μm) at a column temperature of 30°C and liquid flow rate of 1.0 mL/min using water and methanol as the mobile phase with a gradient elution. The detection wavelength was 263 nm. The method was extensively validated by evaluating the linearity (r(2) ≥ 0.9980), recovery (94.24-98.91%), limits of detection (0.25-0.31 ng) and limits of quantification (0.83-1.02 ng). Seventeen samples were analyzed using the developed and validated method. Then, the amounts of bile acids were analyzed by hierarchical agglomerative clustering analysis and principal component analysis. The results of the chemometric analysis showed that the contents of these compounds reflect the intrinsic quality of artificial Calculus bovis, and two compounds (hyodeoxycholic acid and chenodeoxycholic acid) were the most important markers for quality evaluating. PMID:26016891

  19. Identification and quantification of the antipsychotics risperidone, aripiprazole, pipamperone and their major metabolites in plasma using ultra-high performance liquid chromatography-mass spectrometry.

    PubMed

    Wijma, Rixt A; van der Nagel, Bart C H; Dierckx, Bram; Dieleman, Gwen C; Touw, Daan J; van Gelder, Teun; Koch, Birgit C P

    2016-06-01

    The antipsychotics risperidone, aripiprazole and pipamperone are frequently prescribed for the treatment in children with autism. The aim of this study was to validate an ultra-high performance liquid chromatography-mass spectrometry method for the quantification of these antipsychotics in plasma. An ultra-high performance liquid chromatography-mass spectrometry assay was developed for the determination of the drugs and metabolites. Gradient elution was performed on a reversed-phase column with a mobile phase consisting of ammonium acetate, formic acid in methanol or in Milli-Q ultrapure water at a flow rate of 0.5 mL/min. The method was validated according to the US Food and Drug Administration guidelines. The analytes were found to be stable enough after reconstitution and injection of only 5 μL improved the accuracy and precision in combination with the internal standard. Calibration curves of all five analytes were linear. All analytes were stable for at least 72 h in the autosampler and the high quality control of 9-OH-risperidone was stable for 48 h. The method allows quantification of all analytes. The advantage of this method is the combination of a minimal injection volume, a short run-time, an easy sample preparation method and the ability to quantify all analytes in one run. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26447610

  20. Quantification of flavan-3-ols and phenolic acids in milk-based food products by reversed-phase liquid chromatography-tandem mass spectrometry.

    PubMed

    Redeuil, Karine; Bertholet, Raymond; Kussmann, Martin; Steiling, Heike; Rezzi, Serge; Nagy, Kornél

    2009-11-20

    This article reports the development and validation of a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the comprehensive quantification of flavan-3-ol and phenolic acid constituents of milk-based food products. Isotope dilution-based sample preparation consisted of protein precipitation using acidic methanol enriched with the stable isotope labelled internal standards and ultrafiltration to preserve overall polyphenol composition, but to eliminate milk proteins in order to comply with LC. Reversed-phase liquid chromatography was optimized to achieve separation of 22 analytes in 8 min in order to reduce suppression effects, achieve a wide dynamic range and, most importantly, to resolve isomeric compounds. Negative-ion electrospray mass spectrometric detection and fragmentation of analytes was optimized, final transitions were selected for maximized selectivity, reliable quantification and reduction of false positives. The quantitative performance of the method was validated, the main features include: (1) range of lower limits of detection 5-15 ng/mL for flavan-3-ols, 60-100 ng/mL for procyanidins, 1-60 ng/mL for other phenolic acids, (2) lower limits of quantification 15-45 ng/mL for flavan-3-ols, 200-300 ng/mL for procyanidins, 3-200 ng/mL for other phenolic acids, (3) averaged intra-day precision 9.5%, (4) calibrated range 60-300,000 ng/mL for flavan-3-ols, 900-900,000 ng/mL for procyanidins, 9-225,000 ng/mL for other phenolic acids, (5) averaged accuracy 99.5%. Applications for yoghurt and ice-cream products are given. The presented data suggest that this method will help to better characterize the polyphenol composition of milk-based food products for quality control, assessment of dietary intake and for polyphenol bioavailability/bioefficacy studies. PMID:19833343

  1. Resistance of class C fly ash belite cement to simulated sodium sulphate radioactive liquid waste attack.

    PubMed

    Guerrero, A; Goñi, S; Allegro, V R

    2009-01-30

    The resistance of class C fly ash belite cement (FABC-2-W) to concentrated sodium sulphate salts associated with low level wastes (LLW) and medium level wastes (MLW) is discussed. This study was carried out according to the Koch and Steinegger methodology by testing the flexural strength of mortars immersed in simulated radioactive liquid waste rich in sulphate (48,000 ppm) and demineralised water (used as a reference), at 20 degrees C and 40 degrees C over a period of 180 days. The reaction mechanisms of sulphate ion with the mortar was carried out through a microstructure study, which included the use of Scanning electron microscopy (SEM), porosity and pore-size distribution and X-ray diffraction (XRD). The results showed that the FABC mortar was stable against simulated sulphate radioactive liquid waste (SSRLW) attack at the two chosen temperatures. The enhancement of mechanical properties was a result of the formation of non-expansive ettringite inside the pores and an alkaline activation of the hydraulic activity of cement promoted by the ingress of sulphate. Accordingly, the microstructure was strongly refined. PMID:18524482

  2. Subsurface disposal of liquid low-level radioactive wastes at Oak Ridge, Tennessee

    SciTech Connect

    Stow, S.H.; Haase, C.S.

    1986-01-01

    At Oak Ridge National Laboratory (ORNL) subsurface injection has been used to dispose of low-level liquid nuclear waste for the last two decades. The process consists of mixing liquid waste with cement and other additives to form a slurry that is injected under pressure through a cased well into a low-permeability shale at a depth of 300 m. The slurry spreads from the injection well along bedding plane fractures and forms solid grout sheets of up to 200 m in radius. Using this process, ORNL has disposed of over 1.5 x 10/sup 6/ Ci of activity; the principal nuclides are /sup 90/Sr and /sup 137/Cs. In 1982, a new injection facility was put into operation. Each injection, which lasts some two days, results in the emplacement of approximately 750,000 liters of slurry. Disposal cost per liter is about $0.30, including capital costs of the facility. This subsurface disposal process is fundamentally different from other operations. Wastes are injected into a low-permeability aquitard, and the process is designed to isolate nuclides, preventing dispersion in groundwaters. The porosity into which wastes are injected is created by hydraulically fracturing the host formation along bedding planes. Investigations are under way to determine the long-term hydrologic isolation of the injection zone and the geochemical impact of saline groundwater on nuclide mobility. Injections are monitored by gamma-ray logging of cased observation wells to determine grout sheet orientation after an injection. Recent monitoring work has involved the use of tiltmeters, surface uplift surveys, and seismic arrays. Recent regulatory constraints may cause permanent cessation of the operation. Federal and state statutes, written for other types of injection facilities, impact the ORNL facility. This disposal process, which may have great applicability for disposal of many wastes, including hazardous wastes, may not be developed for future use.

  3. Digestion of frozen/thawed food waste in the hybrid anaerobic solid-liquid system

    SciTech Connect

    Stabnikova, O. Liu, X.Y.; Wang, J.Y.

    2008-07-01

    The hybrid anaerobic solid-liquid (HASL) system, which is a modified two-phase anaerobic digester, is to be used in an industrial scale operation to minimize disposal of food waste at incineration plants in Singapore. The aim of the present research was to evaluate freezing/thawing of food waste as a pre-treatment for its anaerobic digestion in the HASL system. The hydrolytic and fermentation processes in the acidogenic reactor were enhanced when food waste was frozen for 24 h at -20 deg. C and then thawed for 12 h at 25 deg. C (experiment) in comparison with fresh food waste (control). The highest dissolved COD concentrations in the leachate from the acidogenic reactors were 16.9 g/l on day 3 in the control and 18.9 g/l on day 1 in the experiment. The highest VFA concentrations in the leachate from the acidogenic reactors were 11.7 g/l on day 3 in the control and 17.0 g/l on day 1 in the experiment. The same volume of methane was produced during 12 days in the control and 7 days in the experiment. It gave the opportunity to diminish operational time of batch process by 42%. The effect of freezing/thawing of food waste as pre-treatment for its anaerobic digestion in the HASL system was comparable with that of thermal pre-treatment of food waste at 150 deg. C for 1 h. However, estimation of energy required either to heat the suspended food waste to 150 deg. C or to freeze the same quantity of food waste to -20 deg. C showed that freezing pre-treatment consumes about 3 times less energy than thermal pre-treatment.

  4. Development of Concentration and Calcination Technology For High Level Liquid Waste

    SciTech Connect

    Pande, D.P.

    2006-07-01

    The concentrated medium and high-level liquid radio chemicals effluents contain nitric acid, water along with the dissolved chemicals including the nitrates of the radio nuclides. High level liquid waste contain mainly nitrates of cesium, strontium, cerium, zirconium, chromium, barium, calcium, cobalt, copper, pickle, iron etc. and other fission products. This concentrated solution requires further evaporation, dehydration, drying and decomposition in temperature range of 150 to 700 deg. C. The addition of the calcined solids in vitrification pot, instead of liquid feed, helps to avoid low temperature zone because the vaporization of the liquid and decomposition of nitrates do not take place inside the melter. In our work Differential and thermo gravimetric studies has been carried out in the various stages of thermal treatment including drying, dehydration and conversion to oxide forms. Experimental studies were done to characterize the chemicals present in high-level radioactive waste. A Rotary Ball Kiln Calciner was used for development of the process because this is amenable for continuous operation and moderately good heat transfer can be achieved inside the kiln. This also has minimum secondary waste and off gases generation. The Rotary Ball Kiln Calciner Demonstration facility system was designed and installed for the demonstration of calcination process. The Rotary Ball Kiln Calciner is a slowly rotating slightly inclined horizontal tube that is externally heated by means of electric resistance heating. The liquid feed is sprayed onto the moving bed of metal balls in a slowly rotating calciner by a peristaltic type-metering pump. The vaporization of the liquid occurs in the pre-calcination zone due to counter current flow of hot gases. The dehydration and denitration of the solids occurs in the calcination zone, which is externally heated by electrical furnace. The calcined powder is cooled in the post calcination portion. It has been demonstrated that the

  5. Selection of liquid-level monitoring method for the Oak Ridge National Laboratory inactive liquid low-level waste tanks, remedial investigation/feasibility study

    SciTech Connect

    Not Available

    1994-11-01

    Several of the inactive liquid low-level waste (LLLW) tanks at Oak Ridge National Laboratory contain residual wastes in liquid or solid (sludge) form or both. A plan of action has been developed to ensure that potential environmental impacts from the waste remaining in the inactive LLLW tank systems are minimized. This document describes the evaluation and selection of a methodology for monitoring the level of the liquid in inactive LLLW tanks. Criteria are established for comparison of existing level monitoring and leak testing methods; a preferred method is selected and a decision methodology for monitoring the level of the liquid in the tanks is presented for implementation. The methodology selected can be used to continuously monitor the tanks pending disposition of the wastes for treatment and disposal. Tanks that are empty, are scheduled to be emptied in the near future, or have liquid contents that are very low risk to the environment were not considered to be candidates for installing level monitoring. Tanks requiring new monitoring equipment were provided with conductivity probes; tanks with existing level monitoring instrumentation were not modified. The resulting data will be analyzed to determine inactive LLLW tank liquid level trends as a function of time.

  6. 30 CFR 250.248 - What solid and liquid wastes and discharges information and cooling water intake information must...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... information and cooling water intake information must accompany the DPP or DOCD? 250.248 Section 250.248...) § 250.248 What solid and liquid wastes and discharges information and cooling water intake information... cooling water intake information must accompany your DPP or DOCD: (a) Projected wastes. A table...

  7. 30 CFR 250.217 - What solid and liquid wastes and discharges information and cooling water intake information must...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... information and cooling water intake information must accompany the EP? 250.217 Section 250.217 Mineral... cooling water intake information must accompany the EP? The following solid and liquid wastes and discharges information and cooling water intake information must accompany your EP: (a) Projected wastes....

  8. Direct utilization of human liquid wastes by plants in a closed ecosystem

    NASA Astrophysics Data System (ADS)

    Lisovsky, G. M.; Gitelson, J. I.; Shilenko, M. P.; Gribovskaya, I. V.; Trubachev, I. N.

    1997-01-01

    Model experiments in phytotrons have shown that urea is able to cover 70% of the demand in nitrogen of the conveyer cultivated wheat. At the same time wheat plants can directly utilize human liquid wastes. In this article by human liquid wastes the authors mean human urine only. In a long-term experiment on ``man-higher plants'' system with two crewmen, plants covered 63 m^2, with wheat planted to - 39.6 m^2. For 103 days, complete human urine (total amount - 210.7 l) was supplied into the nutrient solution for wheat. In a month and a half NaCl supply into the nutrient solution stabilized at 0.9-1.65 g/l. This salination had no marked effect on wheat production. The experiment revealed the realistic feasibility to directly involve liquid wastes into the biological turnover of the life support system. The closure of the system, in terms of water, increased by 15.7% and the supply of nutrients for wheat plants into the system was decreased. Closedness of biological turnover of matter in a man-made ``man - higher plants'' ecological system might involve, among other processes, direct utilization of human liquid wastes by plants. The amount of urine comprises 15-20% of the total amount of water cycling within the system including water as part of food, household, hygiene and potable water necessary for man. What is more, it they contains most nitrogen-bearing compounds emitted by man, almost all of the NaCl and some other substances involved in the biological turnover. Human liquid wastes can be utilized either by preliminary physical-chemical treatment (evaporating or freezing out the water, finally oxidizing the organic matter, isolating the mineral components required for plants, etc.) and further involvement of the obtained products or by direct application into the nutrient solution for plants. The challenge of direct utilization is that plants have no need of Na^+ and Cl^-, and also the organic forms of nitrogen emitted by man cannot fully meet the demand of

  9. Performance Assessment Program for the Savannah River Site Liquid Waste Facilities - 13610

    SciTech Connect

    Rosenberger, Kent H.

    2013-07-01

    The Liquid Waste facilities at the U.S. Department of Energy's (DOE) Savannah River Site (SRS) are operated by Liquid Waste Operations contractor Savannah River Remediation LLC (SRR). A separate Performance Assessment (PA) is prepared to support disposal operations at the Saltstone Disposal Facility and closure evaluations for the two liquid waste tank farm facilities at SRS, F-Tank Farm and H-Tank Farm. A PA provides the technical basis and results to be used in subsequent documents to demonstrate compliance with the pertinent requirements identified in operations and closure regulatory guidance. The Saltstone Disposal Facility is subject to a State of South Carolina industrial solid waste landfill permit and the tank farms are subject to a state industrial waste water permit. The three Liquid Waste facilities are also subject to a Federal Facility Agreement approved by the State, DOE and the Environmental Protection Agency (EPA). Due to the regulatory structure, a PA is a key technical document reviewed by the DOE, the State of South Carolina and the EPA. As the waste material disposed of in the Saltstone Disposal Facility and the residual material in the closed tank farms is also subject to reclassification prior to closure via a waste determination pursuant to Section 3116 of the Ronald W. Reagan National Defense Authorization Act of Fiscal Year 2005, the U.S. Nuclear Regulatory Commission (NRC) is also a reviewing agency for the PAs. Pursuant to the Act, the NRC also has a continuing role to monitor disposal actions to assess compliance with stated performance objectives. The Liquid Waste PA program at SRS represents a continual process over the life of the disposal and closure operations. When the need for a PA or PA revision is identified, the first step is to develop a conceptual model to best represent the facility conditions. The conceptual model will include physical dimensions of the closed system, both the engineered and natural system, and modeling

  10. Cellulose-based films prepared directly from waste newspapers via an ionic liquid.

    PubMed

    Xia, Guangmei; Wan, Jiqiang; Zhang, Jinming; Zhang, Xiaoyu; Xu, Lili; Wu, Jin; He, Jiasong; Zhang, Jun

    2016-10-20

    Waste newspapers, composed of cellulose (>60wt%), lignin (∼15wt%), hemicellulose (∼10wt%) and other additives, are one kind of low-cost, easily collected and abundant resources. In order to get value-added products from this waste, in this work an attempt was made to directly convert waste newspapers into cellulose-based films by employing an ionic liquid 1-allyl-3-methylimidazolium chloride (AmimCl) as a solvent. Most of the organic substances in this waste were dissolved quickly in AmimCl under mild conditions, and then coagulated and dried. Although containing lignin, hemicellulose and inorganic additives, the regenerated cellulose-based films were smooth, compact and semi-transparent, and exhibited good mechanical properties. If the newspaper/AmimCl solution was filtered to remove undissolved inorganic substances, the regenerated films became transparent and had a tensile strength of 80MPa. Thus, this work provides a new, simple and highly efficient way to achieve a high-valued utilization of waste newspapers for packaging and wrapping. PMID:27474561

  11. EVALUATION AND SELECTION OF 99TC GETTERS FOR SEQUESTRATION OF LIQUID SECONDARY WASTE RESULTING FROM VITRIFICATION OF RADIOACTIVE WASTE FROM HANFORD

    SciTech Connect

    Mattigod, Shas V.; Westsik, Joseph H.

    2011-03-31

    Getters are most commonly inorganic materials that selectively adsorb radionuclide and metallic contaminants. Typically, these materials have been deployed in two different modes to immobilize and retard contaminant release from monolithic waste forms. One mode is to first use getters to selectively scavenge the radionuclide of interest from a liquid waste stream, and then incorporate the radionuclide-loaded getters in cementitious or other monolithic waste forms. The other mode consists of mixing getters and liquid waste together during formulation of monolithic waste forms. Desirable characteristics for a getter material include, (1) specific adsorption of radionuclide of interest and very high selectivity toward radionuclides of concern in concentrations that would be several orders of magnitude less than the concentrations of competing anions and cations, (2) adsorption capacity that should be sufficient for the mass and volume of the material that will be deployed to be within practicable limits, (3) long-term adsorption and retention of radionuclide, (4) sufficient physical and chemical stability that its radionuclide retention performance will not degrade significantly during the designed life span of the waste form, (5) chemical stability under the range of Eh, pH, and solution conditions that exist in the waste form environment, and (6) should not adversely affect chemical and physical integrity of waste forms. We conducted a literature review to identify getters that are suitable for effectively sequestering 99Tc in monolithic waste forms that are being evaluated for stabilizing secondary liquid waste streams resulting from treatment and vitrification of radioactive tank wastes at Hanford. As a result of this review, we identified a set of getters that warrant further evaluation for this specific application.

  12. Identification and Quantification of the Major Constituents in Egyptian Carob Extract by Liquid Chromatography–Electrospray Ionization-Tandem Mass Spectrometry

    PubMed Central

    Owis, Asmaa Ibrahim; El-Naggar, El-Motaz Bellah

    2016-01-01

    Background: Carob - Ceratonia siliqua L., commonly known as St John's-bread or locust bean, family Fabaceae - is one of the most useful native Mediterranean trees. There is no data about the chromatography methods performed by high performance liquid chromatography (HPLC) for determining polyphenols in Egyptian carob pods. Objective: To establish a sensitive and specific liquid chromatography–electrospray ionization (ESI)-tandem mass spectrometry (MSn) methodology for the identification of the major constituents in Egyptian carob extract. Materials and Methods: HPLC with diode array detector and ESI-mass spectrometry (MS) was developed for the identification and quantification of phenolic acids, flavonoid glycosides, and aglycones in the methanolic extract of Egyptian C. siliqua. The MS and MSn data together with HPLC retention time of phenolic components allowed structural characterization of these compounds. Peak integration of ions in the MS scans had been used in the quantification technique. Results: A total of 36 compounds were tentatively identified. Twenty-six compounds were identified in the negative mode corresponding to 85.4% of plant dry weight, while ten compounds were identified in the positive mode representing 16.1% of plant dry weight, with the prevalence of flavonoids (75.4% of plant dry weight) predominantly represented by two methylapigenin-O-pentoside isomers (20.9 and 13.7% of plant dry weight). Conclusion: The identification of various compounds present in carob pods opens a new door to an increased understanding of the different health benefits brought about by the consumption of carob and its products. SUMMARY This research proposed a good example for the rapid identification of major constituents in complex systems such as herbs using sensitive, accurate and specific method coupling HPLC with DAD and MS, which facilitate the clarification of phytochemical composition of herbal medicine for better understanding of their nature and

  13. Detection of Clostridium botulinum in liquid manure and biogas plant wastes.

    PubMed

    Neuhaus, Jürgen; Schrödl, Wieland; Shehata, Awad A; Krüger, Monika

    2015-09-01

    Biogas plants have been considered as a source for possible amplification and distribution of pathogenic bacteria capable of causing severe infections in humans and animals. Manure and biogas wastes could be sources for spore-forming bacteria such as Clostridium botulinum. In the present study, 24 liquid manure and 84 biogas waste samples from dairies where the majority of the cows suffered from chronic botulism were investigated for the presence of botulinum neurotoxins (BoNT) and C. botulinum spores. The prevalence of BoNT/A, B, C, D, and E in biogas wastes was 16.6, 8.3, 10.7, 7.1, and 10.8 %, respectively, while in manure, the prevalence was 0.0, 0.0, 0.0, 8.3, and 4.1 %, respectively. After enrichment of samples in reinforced cultural medium, they were tested for C. botulinum BoNT/A, B, C, D, and E using ELISA (indirect C. botulinum detection). The prevalence of C. botulinum type A, B, C, D, and E samples in biogas wastes was 20.2, 15.5, 19, 10.7, and 34.8 %, respectively, while the prevalence in liquid manure was 0.0, 0.0, 0.0, 8.3, and 12.5 %, respectively. In conclusion, the occurrence of BoNT and C. botulinum spores in biogas waste of diseased animals indicates an increased and underestimated hygienic risk. Application of digestates from biogas fermentations as fertilizers could lead to an accumulation of long lifespan spores in the environment and could be a possible health hazard. PMID:25753763

  14. LOW LEVEL LIQUID RADIOACTIVE WASTE TREATMENT AT MURMANSK, RUSSIA: FACILITY UPGRADE AND EXPANSION

    SciTech Connect

    BOWERMAN,B.; CZAJKOWSKI,C.; DYER,R.S.; SORLIE,A.

    2000-03-01

    Today there exist many almost overfilled storage tanks with liquid radioactive waste in the Russian Federation. This waste was generated over several years by the civil and military utilization of nuclear power. The current waste treatment capacity is either not available or inadequate. Following the London Convention, dumping of the waste in the Arctic seas is no longer an alternative. Waste is being generated from today's operations, and large volumes are expected to be generated from the dismantling of decommissioned nuclear submarines. The US and Norway have an ongoing co-operation project with the Russian Federation to upgrade and expand the capacity of a treatment facility for low level liquid waste at the RTP Atomflot site in Murmansk. The capacity will be increased from 1,200 m{sup 3}/year to 5,000 m{sup 3} /year. The facility will also be able to treat high saline waste. The construction phase will be completed the first half of 1998. This will be followed by a start-up and a one year post-construction phase, with US and Norwegian involvement for the entire project. The new facility will consist of 9 units containing various electrochemical, filtration, and sorbent-based treatment systems. The units will be housed in two existing buildings, and must meet more stringent radiation protection requirements that were not enacted when the facility was originally designed. The US and Norwegian technical teams have evaluated the Russian design and associated documentation. The Russian partners send monthly progress reports to US and Norway. Not only technical issues must be overcome but also cultural differences resulting from different methods of management techniques. Six to eight hour time differentials between the partners make real time decisions difficult and relying on electronic age tools becomes extremely important. Language difficulties is another challenge that must be solved. Finding a common vocabulary, and working through interpreters make the

  15. Chromium liquid waste inertization in an inorganic alkali activated matrix: leaching and NMR multinuclear approach.

    PubMed

    Ponzoni, Chiara; Lancellotti, Isabella; Barbieri, Luisa; Spinella, Alberto; Saladino, Maria Luisa; Martino, Delia Chillura; Caponetti, Eugenio; Armetta, Francesco; Leonelli, Cristina

    2015-04-01

    A class of inorganic binders, also known as geopolymers, can be obtained by alkali activation of aluminosilicate powders at room temperature. The process is affected by many parameters (curing time, curing temperature, relative humidity etc.) and leads to a resistant matrix usable for inertization of hazardous waste. In this study an industrial liquid waste containing a high amount of chromium (≈ 2.3 wt%) in the form of metalorganic salts is inertized into a metakaolin based geopolymer matrix. One of the innovative aspects is the exploitation of the water contained in the waste for the geopolymerization process. This avoided any drying treatment, a common step in the management of liquid hazardous waste. The evolution of the process--from the precursor dissolution to the final geopolymer matrix hardening--of different geopolymers containing a waste amount ranging from 3 to 20%wt and their capability to inertize chromium cations were studied by: i) the leaching tests, according to the EN 12,457 regulation, at different curing times (15, 28, 90 and 540 days) monitoring releases of chromium ions (Cr(III) and Cr(VI)) and the cations constituting the aluminosilicate matrix (Na, Si, Al); ii) the humidity variation for different curing times (15 and 540 days); iii) SEM characterization at different curing times (28 and 540 days); iv) the trend of the solution conductivity and pH during the leaching test; v) the characterization of the short-range ordering in terms of TOT bonds (where T is Al or Si) by (29)Si and (27)Al solid state magic-angle spinning nuclear magnetic resonance (ss MAS NMR) for geopolymers containing high amounts of waste (10-20%wt). The results show the formation of a stable matrix after only 15 days independently on the waste amount introduced; the longer curing times increase the matrices stabilities and their ability to immobilize chromium cations. The maximum amount of waste that can be inertized is around 10 wt% after a curing time of 28 days

  16. Quantification of the antifungal lipopeptide iturin A by high performance liquid chromatography coupled with aqueous two-phase extraction.

    PubMed

    Yuan, Jun; Raza, Waseem; Huang, Qiwei; Shen, Qirong

    2011-09-15

    Iturin A, a powerful antifungal surfactant, is a kind of bacterial lipopeptide produced by Bacillus strains. This study addresses the use of an aqueous two-phase system (ATPS) using ethanol/ammonium sulfate to extract iturin A from Bacillus amyloliquefaciens NJN-6 fermentation broth and the quantification of iturin A by HPLC. Baseline separation of iturin A homologues was performed using an RP-C(18) column with a mixture of water and acetonitrile. The results showed that the correlation coefficient between integral area and concentration was 0.9961 within the range of 20-140 mg/l. The RSD of the retention time and the peak area were 1.29% and 1.45%, respectively. The effects of some operating parameters in ATPS, e.g., pH, temperature and centrifugation time, were also studied. This method can be successfully used for the rapid quantification of iturin A. PMID:21872538

  17. A validated ultra high pressure liquid chromatographic method for qualification and quantification of folic acid in pharmaceutical preparations.

    PubMed

    Deconinck, E; Crevits, S; Baten, P; Courselle, P; De Beer, J

    2011-04-01

    A fully validated UHPLC method for the identification and quantification of folic acid in pharmaceutical preparations was developed. The starting conditions for the development were calculated starting from the HPLC conditions of a validated method. These start conditions were tested on four different UHPLC columns: Grace Vision HT™ C18-P, C18, C18-HL and C18-B (2 mm × 100 mm, 1.5 μm). After selection of the stationary phase, the method was further optimised by testing two aqueous and two organic phases and by adapting to a gradient method. The obtained method was fully validated based on its measurement uncertainty (accuracy profile) and robustness tests. A UHPLC method was obtained for the identification and quantification of folic acid in pharmaceutical preparations, which will cut analysis times and solvent consumption. PMID:21168299

  18. Liquid digestate from anaerobic treatment of source-separated household waste as fertilizer to barley.

    PubMed

    Haraldsen, Trond Knapp; Andersen, Uno; Krogstad, Tore; Sørheim, Roald

    2011-12-01

    This study examined the efficiency of different organic waste materials as NPK fertilizer, in addition to the risk for leaching losses related to shower precipitation in the first part of the growing season. The experiment was tested in a pot trial on a sandy soil in a greenhouse. Six organic fertilizers were evaluated: liquid anaerobic digestate (LAD) sourced from separated household waste, nitrified liquid anaerobic digestate (NLAD) of the same origin as LAD, meat and bone meal (MBM), hydrolysed salmon protein (HSP), reactor-composted catering waste (CW) and cattle manure (CM). An unfertilized control, calcium nitrate (CN) and Fullgjødsel® 21-4-10 were used as reference fertilizers. At equal amounts of mineral nitrogen both LAD and Fullgjødsel® gave equal yield of barley in addition to equal uptake of N, P, and K in barley grain. NLAD gave significantly lower barley yield than the original LAD due to leaching of nitrate-N after a simulated surplus of precipitation (28 mm) at Zadoks 14. There was significantly increased leaching of nitrate N from the treatments receiving 160 kg N ha(-1) of CN and NLAD in comparison with all the other organic fertilizers. In this study LAD performed to the same degree as Fullgjødsel® NPK fertilizer and it was concluded that LAD can be recommended as fertilizer for cereals. Nitrification of the ammonium N in the digestate caused significantly increased nitrate leaching, and cannot be recommended. PMID:21746761

  19. Liquid and Gaseous Waste Operations Department annual operating report, CY 1992

    SciTech Connect

    Gillespie, M.A.; Maddox, J.J.; Scott, C.B.

    1993-03-01

    A total of 6.05 x 10{sup 7} gal of liquid waste was decontaminated by the Process Waste Treatment Plant (PWTP) ion exchange system during CY 1992. This averaged to 115 gpm throughout the year. When necessary, a wastewater sidestream of 50--80 gpm was treated through the use of a natural zeolite treatment system. An additional 8.00 x 10{sup 6} gal (average of 15 gpm throughout the year) were treated by the zeolite system. Therefore, the average total flow treated at the PWTP for CY 1992 was 130 gpm. In mid-June, the zeolite system was repiped to allow it the capability to treat the ion exchange system`s discharge due to rising Cs problems in the wastewater. While being used to treat the ion exchange system`s discharge, it cannot treat a sidestream of wastewater. During the year, the regeneration of the cation exchange resins resulted in the generation of 7.83 x 10{sup 3} gal of liquid low-level waste (LLLW) concentrate and 1.15 x 10{sup 4} gal of LLLW evaporator feed. The head-end softening process (precipitation/clarification) generated 604 drums (4.40 x 10{sup 3} ft{sup 3}) of solid low-level waste sludge. The zeolite treatment system generated approximately 8.40 x 10{sup 2} ft{sup 3} of spent zeolite resin, which was turned over to the Solid Waste Operations Department for disposal. See Table 1 for a monthly summary of activities at the PWTP. Figures 1, 2, 3, and 4 show a comparison of operations at the PWTP in 1992 with previous years. Figure 5 shows a comparison of annual rainfall at Oak Ridge National Laboratory (ORNL) since 1987. A total of 1.55 x 10{sup 8} gal of liquid waste (average of 294 gpm throughout the year) was treated at the Nonradiological Wastewater Treatment Plant (NRWTP). Of this amount, 1.40 x 10{sup 7} gal were treated by the precipitation/clarification process for removal of heavy metals. Twenty-five boxes (1.60 x 10{sup 3} ft{sup 3}) of solid sludge generated by the precipitation/clarification process were removed from the filter press room.

  20. Liquid and Gaseous Waste Operations Department annual operating report, CY 1992

    SciTech Connect

    Gillespie, M.A.; Maddox, J.J.; Scott, C.B.

    1993-03-01

    A total of 6.05 x 10[sup 7] gal of liquid waste was decontaminated by the Process Waste Treatment Plant (PWTP) ion exchange system during CY 1992. This averaged to 115 gpm throughout the year. When necessary, a wastewater sidestream of 50--80 gpm was treated through the use of a natural zeolite treatment system. An additional 8.00 x 10[sup 6] gal (average of 15 gpm throughout the year) were treated by the zeolite system. Therefore, the average total flow treated at the PWTP for CY 1992 was 130 gpm. In mid-June, the zeolite system was repiped to allow it the capability to treat the ion exchange system's discharge due to rising Cs problems in the wastewater. While being used to treat the ion exchange system's discharge, it cannot treat a sidestream of wastewater. During the year, the regeneration of the cation exchange resins resulted in the generation of 7.83 x 10[sup 3] gal of liquid low-level waste (LLLW) concentrate and 1.15 x 10[sup 4] gal of LLLW evaporator feed. The head-end softening process (precipitation/clarification) generated 604 drums (4.40 x 10[sup 3] ft[sup 3]) of solid low-level waste sludge. The zeolite treatment system generated approximately 8.40 x 10[sup 2] ft[sup 3] of spent zeolite resin, which was turned over to the Solid Waste Operations Department for disposal. See Table 1 for a monthly summary of activities at the PWTP. Figures 1, 2, 3, and 4 show a comparison of operations at the PWTP in 1992 with previous years. Figure 5 shows a comparison of annual rainfall at Oak Ridge National Laboratory (ORNL) since 1987. A total of 1.55 x 10[sup 8] gal of liquid waste (average of 294 gpm throughout the year) was treated at the Nonradiological Wastewater Treatment Plant (NRWTP). Of this amount, 1.40 x 10[sup 7] gal were treated by the precipitation/clarification process for removal of heavy metals. Twenty-five boxes (1.60 x 10[sup 3] ft[sup 3]) of solid sludge generated by the precipitation/clarification process were removed from the filter press room.

  1. Environmental assessment for liquid waste treatment at the Nevada Test Site, Nye County, Nevada

    SciTech Connect

    1997-01-01

    This environmental assessment (EA) examines the potential impacts to the environment from treatment of low-level radioactive liquid and low-level mixed liquid and semi-solid wastes generated at the Nevada Test Site (NTS). The potential impacts of the proposed action and alternative actions are discussed herein in accordance with the National Environmental Policy Act (NEPA) of 1969, as amended in Title 42 U.S.C. (4321), and the US Department of Energy (DOE) policies and procedures set forth in Title 10 Code of Federal Regulations (CFR) Part 1021 and DOE Order 451.1, ``NEPA Compliance Program.`` The potential environmental impacts of the proposed action, construction and operation of a centralized liquid waste treatment facility, were addressed in the Final Environmental Impact Statement for the Nevada Test Site and Off-Site Locations in the State of Nevada. However, DOE is reevaluating the need for a centralized facility and is considering other alternative treatment options. This EA retains a centralized treatment facility as the proposed action but also considers other feasible alternatives.

  2. Isolation of Metals from Liquid Wastes: Reactive Scavenging in Turbulent Thermal Reactors

    SciTech Connect

    William Linak

    2004-12-16

    Sorption of cesium and strontium on kaolinite powders was investigated as a means to minimize the emissions of these metals during certain high temperature processes currently being developed to isolate and dispose of radiological and mixed wastes. In this work, non-radioactive aqueous cesium acetate or strontium acetate was atomized down the center of a natural gas flame supported on a variable-swirl burner in a refractory-lined laboratory-scale combustion facility. Kaolinite powder was injected at a post-flame location in the combustor. Cesium readily vaporizes in the high temperature regions of the combustor, but was reactively scavenged onto dispersed kaolinite. Global sorption mechanisms of cesium vapor on kaolinite were quantified, and are related to those available in the literature for sodium and lead. Both metal adsorption and substrate deactivation steps are important, and so there is an optimum temperature, between 1400 and 1500 K, at which maximum sorption occurs. The presence of chlorine inhibits cesium sorption. In contrast to cesium, and in the absence of chlorine, strontium was only partially vaporized and was, therefore, only partially scavengeable. The strontium data did not allow quantification of global kinetic mechanisms of interaction, although equilibrium arguments provided insight into the effects of chlorine on strontium sorption. These results have implications for the use of sorbents to control cesium and strontium emissions during high temperature waste processing including incineration and vitrification.

  3. Waste Tank Organic Safety Project: Analysis of liquid samples from Hanford waste tank 241-C-103

    SciTech Connect

    Pool, K.H.; Bean, R.M.

    1994-03-01

    A suite of physical and chemical analyses has been performed in support of activities directed toward the resolution of an Unreviewed Safety Question concerning the potential for a floating organic layer in Hanford waste tank 241-C-103 to sustain a pool fire. The analysis program was the result of a Data Quality Objectives exercise conducted jointly with staff from Westinghouse Hanford Company and Pacific Northwest Laboratory (PNL). The organic layer has been analyzed for flash point, organic composition including volatile organics, inorganic anions and cations, radionuclides, and other physical and chemical parameters needed for a safety assessment leading to the resolution of the Unreviewed Safety Question. The aqueous layer underlying the floating organic material was also analyzed for inorganic, organic, and radionuclide composition, as well as other physical and chemical properties. This work was conducted to PNL Quality Assurance impact level III standards (Good Laboratory Practices).

  4. Quantification of typical antipsychotics in human plasma by ultra-high performance liquid chromatography tandem mass spectrometry for therapeutic drug monitoring.

    PubMed

    Gradinaru, Julieta; Vullioud, Astrid; Eap, Chin B; Ansermot, Nicolas

    2014-01-01

    A selective and sensitive method was developed for the simultaneous quantification of seven typical antipsychotic drugs (cis-chlorprothixene, flupentixol, haloperidol, levomepromazine, pipamperone, promazine and zuclopenthixol) in human plasma. Ultra-high performance liquid chromatography (UHPLC) was used for complete separation of the compounds in less than 4.5min on an Acquity UPLC BEH C18 column (2.1mm×50mm; 1.7μm), with a gradient elution of ammonium formate buffer pH 4.0 and acetonitrile at a flow rate of 400μl/min. Detection was performed on a tandem quadrupole mass spectrometer (MS/MS) equipped with an electrospray ionization interface. A simple protein precipitation procedure with acetonitrile was used for sample preparation. Thanks to the use of stable isotope-labeled internal standards for all analytes, internal standard-normalized matrix effects were in the range of 92-108%. The method was fully validated to cover large concentration ranges of 0.2-90ng/ml for haloperidol, 0.5-90ng/ml for flupentixol, 1-450ng/ml for levomepromazine, promazine and zuclopenthixol and 2-900ng/ml for cis-chlorprothixene and pipamperone. Trueness (89.1-114.8%), repeatability (1.8-9.9%), intermediate precision (1.9-16.3%) and accuracy profiles (<30%) were in accordance with the latest international recommendations. The method was successfully used in our laboratory for routine quantification of more than 500 patient plasma samples for therapeutic drug monitoring. To the best of our knowledge, this is the first UHPLC-MS/MS method for the quantification of the studied drugs with a sample preparation based on protein precipitation. PMID:24036032

  5. Identification and Quantification of Fumonisin A1, A2, and A3 in Corn by High-Resolution Liquid Chromatography-Orbitrap Mass Spectrometry

    PubMed Central

    Tamura, Masayoshi; Mochizuki, Naoki; Nagatomi, Yasushi; Harayama, Koichi; Toriba, Akira; Hayakawa, Kazuichi

    2015-01-01

    Three compounds, hypothesized as fumonisin A1 (FA1), fumonisin A2 (FA2), and fumonisin A3 (FA3), were detected in a corn sample contaminated with mycotoxins by high-resolution liquid chromatography-Orbitrap mass spectrometry (LC-Orbitrap MS). One of them has been identified as FA1 synthesized by the acetylation of fumonisin B1 (FB1), and established a method for its quantification. Herein, we identified the two remaining compounds as FA2 and FA3, which were acetylated fumonisin B2 (FB2) and fumonisin B3 (FB3), respectively. Moreover, we examined a method for the simultaneous analysis of FA1, FA2, FA3, FB1, FB2, and FB3. The corn samples were prepared by extraction using a QuEChERS kit and purification using a multifunctional cartridge. The linearity, recovery, repeatability, limit of detection, and limit of quantification of the method were >0.99, 82.9%–104.6%, 3.7%–9.5%, 0.02–0.60 μg/kg, and 0.05–1.98 μg/kg, respectively. The simultaneous analysis of the six fumonisins revealed that FA1, FA2, and FA3 were present in all corn samples contaminated with FB1, FB2, and FB3. The results suggested that corn marketed for consumption can be considered as being contaminated with both the fumonisin B-series and with fumonisin A-series. This report presents the first identification and quantification of FA1, FA2, and FA3 in corn samples. PMID:25690692

  6. Simultaneous quantification of protein phosphorylation sites using liquid chromatography-tandem mass spectrometry-based targeted proteomics: a linear algebra approach for isobaric phosphopeptides.

    PubMed

    Xu, Feifei; Yang, Ting; Sheng, Yuan; Zhong, Ting; Yang, Mi; Chen, Yun

    2014-12-01

    As one of the most studied post-translational modifications (PTM), protein phosphorylation plays an essential role in almost all cellular processes. Current methods are able to predict and determine thousands of phosphorylation sites, whereas stoichiometric quantification of these sites is still challenging. Liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS)-based targeted proteomics is emerging as a promising technique for site-specific quantification of protein phosphorylation using proteolytic peptides as surrogates of proteins. However, several issues may limit its application, one of which relates to the phosphopeptides with different phosphorylation sites and the same mass (i.e., isobaric phosphopeptides). While employment of site-specific product ions allows for these isobaric phosphopeptides to be distinguished and quantified, site-specific product ions are often absent or weak in tandem mass spectra. In this study, linear algebra algorithms were employed as an add-on to targeted proteomics to retrieve information on individual phosphopeptides from their common spectra. To achieve this simultaneous quantification, a LC-MS/MS-based targeted proteomics assay was first developed and validated for each phosphopeptide. Given the slope and intercept of calibration curves of phosphopeptides in each transition, linear algebraic equations were developed. Using a series of mock mixtures prepared with varying concentrations of each phosphopeptide, the reliability of the approach to quantify isobaric phosphopeptides containing multiple phosphorylation sites (≥ 2) was discussed. Finally, we applied this approach to determine the phosphorylation stoichiometry of heat shock protein 27 (HSP27) at Ser78 and Ser82 in breast cancer cells and tissue samples. PMID:25403019

  7. Multi-drug and metabolite quantification in postmortem blood by liquid chromatography-high-resolution mass spectrometry: comparison with nominal mass technology.

    PubMed

    Rosano, Thomas G; Na, Seo; Ihenetu, Kenneth; Swift, Thomas A; Wood, Michelle

    2014-10-01

    High-resolution mass spectrometry (HRMS) is being applied in postmortem drug screening as an alternative to nominal mass spectrometry, and additional evaluation in quantitative casework is needed. We report quantitative analysis of benzoylecgonine, citalopram, cocaethylene, cocaine, codeine, dextromethorphan, dihydrocodeine, diphenhydramine, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine, hydrocodone, hydromorphone, meperidine, methadone, morphine, oxycodone and oxymorphone in postmortem blood by ultra-performance liquid chromatography (UPLC)-MS(E)/time-of-flight (TOF). The method employs analyte-matched deuterated internal standardization and MS(E) acquisition of precursor and product ions at low (6 eV) and ramped (10-40 eV) collision energies, respectively. Quantification was performed using precursor ion data obtained with a mass extraction window of ± 5 ppm. Fragment and residual precursor ion acquisitions at ramped collision energies were evaluated as additional analyte identifiers. Extraction recovery of >60% and matrix effect of <20% were determined for all analytes and internal standards. Defined limits of detection (10 ng/mL) and quantification (25 ng/mL) were validated along with a linearity analytical range of 25-3,000 ng/mL (R(2) > 0.99) for all analytes. Parallel UPLC-MS(E)/TOF and UPLC-MS/MS analysis showed comparable precision and bias along with concordance of 253 positive (y = 1.002x + 1.523; R(2) = 0.993) and 2,269 negative analyte findings in 159 postmortem cases. Analytical performance and correlation studies demonstrate accurate quantification by UPLC-MS(E)/TOF and extended application of HRMS in postmortem casework. PMID:25217537

  8. Quantification of plasma carnitine and acylcarnitines by high-performance liquid chromatography-tandem mass spectrometry using online solid-phase extraction.

    PubMed

    Morand, Réjane; Donzelli, Massimiliano; Haschke, Manuel; Krähenbühl, Stephan

    2013-11-01

    Carnitine is an amino acid derivative that plays a key role in energy metabolism. Endogenous carnitine is found in its free form or esterified with acyl groups of several chain lengths. Quantification of carnitine and acylcarnitines is of particular interest for screening for research and metabolic disorders. We developed a method with online solid-phase extraction coupled to high-performance liquid chromatography and tandem mass spectrometry to quantify carnitine and three acylcarnitines with different polarity (acetylcarnitine, octanoylcarnitine, and palmitoylcarnitine). Plasma samples were deproteinized with methanol, loaded on a cation exchange trapping column and separated on a reversed-phase C8 column using heptafluorobutyric acid as an ion-pairing reagent. Considering the endogenous nature of the analytes, we quantified with the standard addition method and with external deuterated standards. Solid-phase extraction and separation were achieved within 8 min. Recoveries of carnitine and acylcarnitines were between 98 and 105 %. Both quantification methods were equally accurate (all values within 84 to 116 % of target concentrations) and precise (day-to-day variation of less than 18 %) for all carnitine species and concentrations analyzed. The method was used successfully for determination of carnitine and acylcarnitines in different human samples. In conclusion, we present a method for simultaneous quantification of carnitine and acylcarnitines with a rapid sample work-up. This approach requires small sample volumes and a short analysis time, and it can be applied for the determination of other acylcarnitines than the acylcarnitines tested. The method is useful for applications in research and clinical routine. PMID:23995505

  9. Development and validation of high-performance liquid chromatography and high-performance thin-layer chromatography methods for the quantification of khellin in Ammi visnaga seed

    PubMed Central

    Kamal, Abid; Khan, Washim; Ahmad, Sayeed; Ahmad, F. J.; Saleem, Kishwar

    2015-01-01

    Objective: The present study was used to design simple, accurate and sensitive reversed phase-high-performance liquid chromatography RP-HPLC and high-performance thin-layer chromatography (HPTLC) methods for the development of quantification of khellin present in the seeds of Ammi visnaga. Materials and Methods: RP-HPLC analysis was performed on a C18 column with methanol: Water (75: 25, v/v) as a mobile phase. The HPTLC method involved densitometric evaluation of khellin after resolving it on silica gel plate using ethyl acetate: Toluene: Formic acid (5.5:4.0:0.5, v/v/v) as a mobile phase. Results: The developed HPLC and HPTLC methods were validated for precision (interday, intraday and intersystem), robustness and accuracy, limit of detection and limit of quantification. The relationship between the concentration of standard solutions and the peak response was linear in both HPLC and HPTLC methods with the concentration range of 10–80 μg/mL in HPLC and 25–1,000 ng/spot in HPTLC for khellin. The % relative standard deviation values for method precision was found to be 0.63–1.97%, 0.62–2.05% in HPLC and HPTLC for khellin respectively. Accuracy of the method was checked by recovery studies conducted at three different concentration levels and the average percentage recovery was found to be 100.53% in HPLC and 100.08% in HPTLC for khellin. Conclusions: The developed HPLC and HPTLC methods for the quantification of khellin were found simple, precise, specific, sensitive and accurate which can be used for routine analysis and quality control of A. visnaga and several formulations containing it as an ingredient. PMID:26681890

  10. Chemical profiling and quantification of Gua-Lou-Gui-Zhi decoction by high performance liquid chromatography/quadrupole-time-of-flight mass spectrometry and ultra-performance liquid chromatography/triple quadrupole mass spectrometry.

    PubMed

    Xu, Wen; Huang, Mingqing; Li, Huang; Chen, Xianwen; Zhang, Yuqin; Liu, Jie; Xu, Wei; Chu, Kedan; Chen, Lidian

    2015-04-01

    Gua-Lou-Gui-Zhi decoction (GLGZD) is a classical formula of traditional Chinese medicine, which has been commonly used to treat dysfunction after stroke, epilepsy and spinal cord injury. In this study, a systematic method was established for chemical profiling and quantification analysis of the major constituents in GLGZD. For qualitative analysis, a method of high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (Q-TOF MS) was developed. 106 compounds, including monoterpene glycosides, galloyl glucoses, phenolic acids, flavonoids, gingerols and triterpene saponins were identified or tentatively presumed by comparison with reference standards or literature data. According to the qualitative results, a new quantitative analysis method of ultra-performance liquid chromatography/triple quadrupole mass spectrometry (QqQ-MS) was established. 24 representative compounds were simultaneously detected in 10 batches of GLGZD samples in 7.5 min. The calibration curves for all analytes showed good linearity (r>0.9959) within the test ranges. The LODs and the LOQs were less than 30.6 and 70.9 ng/mL, respectively. The RSDs of intra- and inter-day precision, repeatability and stability were below 3.64%, 4.85%, 4.84% and 3.87%, respectively. The overall recoveries ranged from 94.94% to 103.66%, with the RSDs within 5.12%. This study established a high sensitive and efficient method for the integrating quality control, including identification and quantification of Chinese medicinal preparation. PMID:25710597

  11. Wide-scope screening and quantification of 50 pesticides in wine by liquid chromatography/quadrupole time-of-flight mass spectrometry combined with liquid chromatography/quadrupole linear ion trap mass spectrometry.

    PubMed

    He, Zeying; Xu, Yaping; Wang, Lu; Peng, Yi; Luo, Ming; Cheng, Haiyan; Liu, Xiaowei

    2016-04-01

    In this paper, a wide scope screening method of pesticides in wine was established using liquid chromatography/quadrupole time-of-flight mass spectrometry (LC-QTOF MS) and liquid chromatography/quadrupole linear ion trap mass spectrometry (LC-QqLIT MS). Information dependent acquisition (IDA) experiments are used to obtain both MS and MS/MS information for LC-QTOF MS analysis. For LC-QqLIT MS analysis, MS/MS spectra of target pesticides were simultaneously acquired using Enhanced Product Ion (EPI) mode at very low concentrations to increase the confidence in analytical results of multiple reaction monitoring (MRM) by library searching. Method validation was carried out using 50 pesticides commonly used in vineyards. The LOQs, linearity, repeatability were determined and good enough for quantification. The screening and quantification results obtained using LC-QTOF MS and LC-QqLIT MS were compared. Contaminants were screened against libraries containing over 2800 compounds based on accurate mass, isotopic patterns, and MS/MS spectra searching to extend the scope of this methodology to non-target screening. PMID:26593613

  12. Quantification of voriconazole in human plasma by high-performance liquid chromatography-electrospray ionization mass spectrometry: application to a bioequivalence study.

    PubMed

    Cheng, Ying; Zhang, Zun-Jian; Tian, Yuan; Li, Wen-Jing; Wei, Wei

    2011-01-01

    A sensitive and specific liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) method was developed and validated for the identification and quantification of voriconazole (VRC, CAS 137234-62-9) in human plasma. Following liquid-liquid extraction, VRC and loratadine (internal standard, CAS 79794-75-5) were separated using a mobile phase comprised of methanol: water (0.1% formic acid) = 75:25 v/v on a Shimadzu Shim-pack VP-ODS C18 (150 x 2.0 mm ID, 5 microm) column and analyzed by electrospray ionization mass spectrometry. The chromatographic separation was achieved in less than 6 min. The standard curves were linear (r = 0.9994) over the concentration range of 2-2000 ng/mL for VRC and had good accuracy and precision. Both intra- and inter-batch standard deviations were less than 15%. The method was successfully applied to study the comparative bioavailability of VRC tablets test vs. reference in healthy Chinese volunteers through the statistical comparison of pharmacokinetic parameters obtained with the two formulations. PMID:21428249

  13. Quantification of aristolochic acids I and II in herbal dietary supplements by ultra-high-performance liquid chromatography-multistage fragmentation mass spectrometry.

    PubMed

    Vaclavik, Lukas; Krynitsky, Alexander J; Rader, Jeanne I

    2014-01-01

    A rapid, selective and sensitive ultra-high-performance liquid chromatography-multistage fragmentation mass spectrometry (UHPLC-MS³) method was developed and evaluated for the determination of aristolochic acids I and II (AA I and II) in herbal dietary supplements. A hybrid triple quadrupole/linear ion-trap mass spectrometry was used to monitor MS³ ion transitions m/z 359.2 > 298.1 > 268.0 and m/z 329.2 > 268.2 > 238.0 to detect AA I and II, respectively. The extraction and clean-up of target analytes from dry powdered samples was performed using the quick, easy, cheap, effective, rugged and safe (QuEChERS) procedure. Herbal liquid extracts were analysed directly. Average recoveries ranged from 89% to 112%, with relative standard deviations (RSDs) ranging from 3% to 16%. Limits of quantification (LOQs) estimated for three selected matrices were as follows (AA I/II): 5/10 ng g⁻¹ (tablets); 25/50 ng g⁻¹ (capsules); and 2.5/5.0 ng ml⁻¹ (liquid herbal extract). The method was applied in a limited survey of 30 herbal products marketed in the United States via the Internet. AA I and II were detected in 20% and 7%, respectively, of tested samples. PMID:24512293

  14. Simultaneous quantification of olanzapine and its metabolite N-desmethylolanzapine in human plasma by liquid chromatography tandem mass spectrometry for therapeutic drug monitoring.

    PubMed

    Lou, Hong-gang; Ruan, Zou-rong; Jiang, Bo; Chen, Jin-liang

    2015-05-01

    A simple, sensitive, and selective liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed and validated for the simultaneous quantification of olanzapine (OLZ) and its metabolite N-desmethylolanzapine (DMO) in human plasma for therapeutic drug monitoring. Sample preparation was performed by one-step protein precipitation with methanol. The analytes were chromatographed on a reversed-phase YMC-ODS-AQ C18 Column (2.0 × 100 mm,3 µm) by a gradient program at a flow rate of 0.30 mL/min. Quantification was performed on a triple quadrupole tandem mass spectrometer via electrospray ionization in positive ion mode. The method was validated for selectivity, linearity, accuracy, precision, matrix effect, recovery and stability. The calibration curve was linear over the concentration range 0.2-120 ng/mL for OLZ and 0.5-50 ng/mL for DMO. Intra- and interday precisions for OLZ and DMO were <11.29%, and the accuracy ranged from 95.23 to 113.16%. The developed method was subsequently applied to therapeutic drug monitoring for psychiatric patients receiving therapy of OLZ tablets. The method seems to be suitable for therapeutic drug monitoring of patients undergoing therapy with OLZ and might contribute to prediction of the risk of adverse reactions. PMID:25297964

  15. Identification and quantification of 56 targeted phenols in wines, spirits, and vinegars by online solid-phase extraction - ultrahigh-performance liquid chromatography - quadrupole-orbitrap mass spectrometry.

    PubMed

    Barnaba, C; Dellacassa, E; Nicolini, G; Nardin, T; Malacarne, M; Larcher, R

    2015-12-01

    Phenolic compounds seriously affect the sensory and nutritional qualities of food products, both through the positive contribution of wood transfer in barrel-aged products and as off-flavours. A new targeted analytical approach combining on-line solid-phase extraction (SPE) clean-up to reduce matrix interference and rapid chromatographic detection performed with ultrahigh-performance liquid chromatography coupled with quadrupole/high-resolution mass spectrometry (Q-Orbitrap), was developed for the quantification of 56 simple phenols. Considering the advantages of using on-line SPE and a resolving power of 140,000, the proposed method was applied to define phenolic content in red (N=8) and white (8) wines, spirits (8), common (8) and balsamic (8) vinegars. The final method was linear from the limits of quantification (0.0001-0.001μgmL(-1)) up to 10μgmL(-1) with R(2) of at least 0.99. Recovery, used to define method accuracy, ranged from 80 to 120% for 89% of compounds. The method was suitable for analytical requirements in the tested matrices being able to analyse 46 phenols in red wines, 41 phenols in white wines and in spirits, 42 phenols in common vinegars and 44 phenols in balsamic vinegars. PMID:26582576

  16. Development and validation of a generic method for quantification of collagen in food supplement tablets using liquid chromatography coupled with time-of-flight mass spectrometry.

    PubMed

    Vatansever, Bilgin; Senal, Merve Oztug; Akgoz, Muslum; Goren, Ahmet C

    2015-03-01

    A generic method for the quantification of type II collagen in protein-based dietary supplements is described. This quantitative analysis was conducted using liquid chromatography-electrospray ionization-time-of-flight mass spectrometry (LC-ESI-TOF MS). Compared to classical methods with the use of isotope-labeled standards, our method includes, for the first time, the quantification of hydroxyproline using histidine as an internal standard. Separation of the analytes was performed on a Phenomenex Synergi 4 μm Fusion-RP 80 Ǻ column (150 × 2.0 mm, 4.0 μm) with a mobile phase made of 10 mM ammonium formate in water (A) and 10 mM ammonium formate in methanol (B). The assay was fully validated according to FDA guidelines, and the method exhibited sufficient specificity, accuracy, and precision. Intra- and inter-batch accuracy, determined as a deviation between nominal and measured values, ranged from -4.8 to 9.1% and from 0.9 to 6.4 %, respectively. All analytes (hydroxyproline and histidine) at three concentration levels showed extraction recoveries from 89 to 98 %. The method was successfully applied to protein-based dietary supplements of the pharmaceutical industry. PMID:25585887

  17. Simultaneous quantification of neuroactive dopamine serotonin and kynurenine pathway metabolites in gender-specific youth urine by ultra performance liquid chromatography tandem high resolution mass spectrometry.

    PubMed

    Lu, Haihua; Yu, Jing; Wang, Jun; Wu, Linlin; Xiao, Hang; Gao, Rong

    2016-04-15

    Neuroactive metabolites in dopamine, serotonin and kynurenine metabolic pathways play key roles in several physiological processes and their imbalances have been implicated in the pathophysiology of a wide range of disorders. The association of these metabolites' alterations with various pathologies has raised interest in analytical methods for accurate quantification in biological fluids. However, simultaneous measurement of various neuroactive metabolites represents great challenges due to their trace level, high polarity and instability. In this study, an analytical method was developed and validated for accurately quantifying 12 neuroactive metabolites covering three metabolic pathways in youth urine by ultra performance liquid chromatography coupled to electrospray tandem high resolution mass spectrometry (UPLC-ESI-HRMS/MS). The strategy of dansyl chloride derivatization followed by solid phase extraction on C18 cartridges were employed to reduce matrix interference and improve the extraction efficiency. The reverse phase chromatographic separation was achieved with a gradient elution program in 20min. The high resolution mass spectrometer (Q Exactive) was employed, with confirmation and quantification by Target-MS/MS scan mode. Youth urine samples collected from 100 healthy volunteers (Female:Male=1:1) were analyzed to explore the differences in metabolite profile and their turnover between genders. The results demonstrated that the UPLC-ESI-HRMS/MS method is sensitive and robust, suitable for monitoring a large panel of metabolites and for discovering new biomarkers in the medical fields. PMID:26845201

  18. Simultaneous quantification of 25 active constituents in the total flavonoids extract from Herba Desmodii Styracifolii by high-performance liquid chromatography with electrospray ionization tandem mass spectrometry.

    PubMed

    Guo, Panpan; Yan, Wenying; Han, Qingjie; Wang, Chunying; Zhang, Zijian

    2015-04-01

    A sensitive and selective high-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry method has been developed and validated for the simultaneous determination of 25 active constituents, including 21 flavonoids and four phenolic acids in the total flavonoids extract from Herba Desmodii Styracifolii for the first time. Among the 25 compounds, seven compounds including caffeic acid, acacetin, genistein, genistin, diosmetin, diosmin and hesperidin were identified and quantified for the first time in Herba Desmodii Styracifolii. Chromatographic separation was accomplished on a ZORBAX SB-C18 (250 mm×4.6 mm, 5.0 μm) column using gradient elution of methanol and 0.1‰ acetic acid v/v at a flow rate of 1.0 mL/min. The identification and quantification of the analytes were achieved using negative electrospray ionization mass spectrometry in multiple-reaction monitoring mode. The method was fully validated in terms of limits of detection and quantification, linearity, precision and accuracy. The results indicated that the developed method is simple, rapid, specific and reliable. Furthermore, the developed method was successfully applied to quantify the 25 active components in six batches of total flavonoids extract from Herba Desmodii Styracifolii. PMID:25620156

  19. Quantification of acetaminophen and two of its metabolites in human plasma by ultra-high performance liquid chromatography-low and high resolution tandem mass spectrometry.

    PubMed

    Tonoli, David; Varesio, Emmanuel; Hopfgartner, Gérard

    2012-09-01

    The quantification of acetaminophen (APAP) and two of its metabolites, i.e. acetaminophen-glucuronide (APAP-GLUC) and acetaminophen-cysteine (APAP-CYS), is described in human plasma using ultra-high performance liquid chromatography coupled to a triple quadrupole linear ion trap mass spectrometer operating in the selected reaction monitoring (SRM/MS) mode and to a high resolution quadrupole time-of -flight mass spectrometer operating in the MS/MS (HR-SRM/MS) mode. Starting with a 50 μL plasma aliquot, a generic sample preparation was performed using protein precipitation with methanol/ethanol. Both methods were found to be linear over 2.5 orders of magnitude. Similar performances to the SRM/MS assay were obtained for APAP, APAP-CYS and APAP-GLUC using high resolution-selected reaction monitoring mode with LLOQ of 20, 50 and 50 ng/mL, respectively. For all analytes, precision was found to be better than 12% and accuracy in the range 90.3-109%. The present study demonstrates the ability of QqTOF platforms for accurate and precise quantification in MS/MS mode using short duty cycle with similar sensitivity to LC-SRM/MS. Additionally, as full scan data MS(ALL) are available qualitative and quantitative information on metabolites can also be obtained in a single LC-MS run. PMID:22867840

  20. Solvent extraction of [sup 99]Tc from radioactive intermediate liquid waste by dibenzo-18-crown-6.

    SciTech Connect

    Paviet-Hartmann, P.

    2001-01-01

    Technetium is one of the most prominent problems since its most stable specie in the environment, the pertechnetate ion, is highly mobile and considered as a long-term hazard in nuclear waste disposal. Because of the small activities of 99Tc relative to other fission products 137Cso r 90Sr,a nd its long half-life time (t1/2 = 2.1{center_dot}10{sup 5} yrs), 99Tci s one of the key isotopes that should always be analyzed in the radioactive liquid waste streams from the reprocessing industry where the largest concentrations are to be expected. Furthermore, as a pure beta-emitter, Tc has to be isolated from the intermediate level waste (ILW) stream prior to any measurement in such complex media. We have developed a method for 99Tc extraction providing recommendations that will be useful for extracting it from acid and basic ILW. The extraction of 99Tc from L W by dibenzo-18-crown-6 (DB18C6) has been investigated and a simplex optimization of key parameters involved in the procedure has allowed us to set up their best values. Experiments have been carried out on synthetic and real effluents from La Hague reprocessing plant, France, and results show that DB18C6 is highly selective towards 99Tc. The application of this procedure has been successfully demonstrated through the analysis of actual waste streams coming from two reprocessing plants at La Hague and Marcoule, France.

  1. SOLVENT EXTRACTION OF 99Tc FROM RADIOACTIVE INTERMEDIATE LIQUID WASTE BY DIBENZO-18-CROWN-6

    SciTech Connect

    Paviet-Hartmann, P.

    2002-02-25

    Technetium is one of the most prominent problems since its most stable specie in the environment, the pertechnetate ion, is highly mobile and considered as a long-term hazard in nuclear waste disposal. Because of the small activities of 99Tc relative to other fission products 137Cs or 90Sr, and its long half-life time (t1/2 = 2.1 x 105 yrs), 99Tc is one of the key isotopes that should always be analyzed in the radioactive liquid waste streams from the reprocessing industry where the largest concentrations are to be expected. Furthermore, as a pure beta-emitter, 99Tc has to be isolated from the intermediate level waste (ILW) stream prior to any measurement in such complex media. We have developed a method for 99Tc extraction providing recommendations that will be useful for extracting it from acid and basic ILW. The extraction of 99Tc from ILW by dibenzo-18-crown-6 (DB18C6) has been investigated and a simplex optimization of key parameters involved in the procedure has allowed us to set u p their best values. Experiments have been carried out on synthetic and real effluents from La Hague reprocessing plant, France, and results show that DB18C6 is highly selective towards 99Tc. The application of this procedure has been successfully demonstrated through the analysis of actual waste streams coming from two reprocessing plants at La Hague and Marcoule, France.

  2. AN ADVANCED LIQUID WASTE TREATMENT SYSTEM USING A HIGH EFFICIENCY SOLIDIFICATION TECHNIQUE

    SciTech Connect

    Kikuchi, M.; Hirayama, S.; Noshita, K.; Yatou, Y.; Huang, C.T.

    2003-02-27

    An advanced system using High Efficiency Solidification Technology (HEST) was developed to treat PWR liquid waste and the first unit is operating in Taiwan (1) and a detailed design is being carried out for the second unit in Japan. The HEST system consists of two subsystems, a super-concentration subsystem and a solidification subsystem. The super-concentration subsystem is able to concentrate the waste solution to a total boron content as high as 130,000 ppm prior to solidification. The higher boron content will result in greater volume reduction efficiency of solidification. The solidification subsystem consists of an in-drum mixing and a conveyor units. Representative features of this advanced system are as follows. (1) Simple system: The system consists of the super-concentration and cement solidification subsystems; it is as simple as the conventional cement solidification system. (2) High volume reduction efficiency: The number of solidified waste drums is about 1/2.5 that of bitumen solidification. (3) Stable Package: Essentially no organic material is used, and the final package will be stable under the final disposal conditions. (4) Zero secondary waste: Washing water used in the in-drum mixer is recycled. This paper describes the outline of HEST technology, treatment system and pilot plant tests.

  3. Using oxidized liquid and solid human waste as nutrients for Chlorella vulgaris and cyanobacterium Oscillatoria deflexa

    NASA Astrophysics Data System (ADS)

    Trifonov, Sergey V.; Kalacheva, Galina; Tirranen, Lyalya; Gribovskaya, Iliada

    At stationary terrestrial and space stations with closed and partially closed substance exchange not only plants, but also algae can regenerate atmosphere. Their biomass can be used for feeding Daphnia and Moina species, which, in their turn, serve as food for fish. In addition, it is possible to use algae for production of biological fuel. We suggested two methods of human waste mineralization: dry (evaporation with subsequent incineration in a muffle furnace) and wet (oxidation in a reactor using hydrogen peroxide). The research task was to prepare nutrient media for green alga Chlorella vulgaris and cyanobacterium Oscillatoria deflexa using liquid human waste mineralized by dry method, and to prepare media for chlorella on the basis of 1) liquid and 2) liquid and solid human waste mineralized by wet method. The algae were grown in batch culture in a climate chamber with the following parameters: illumination 7 klx, temperature 27-30 (°) C, culture density 1-2 g/l of dry weight. The control for chlorella was Tamiya medium, pH-5, and for oscillstoria — Zarrouk medium, pH-10. Maximum permissible concentrations of NaCl, Cl, urea (NH _{2}) _{2}CO, and native urine were established for algae. Missing ingredients (such as salts and acids) for experimental nutrient media were determined: their addition made it possible to obtain the biomass production not less than that in the control. The estimation was given of the mineral and biochemical composition of algae grown on experimental media. Microbiological test revealed absence of foreign microbial flora in experimental cultures.

  4. Development of US Navy Shipboard Systems for solid and liquid waste thermal treatment. Report for July 1995-April 1996

    SciTech Connect

    Gullet, B.K.

    1996-07-01

    The paper describes the U.S. Navy`s shipboard environmental challenges and a few of its research programs for meeting its needs for solid and liquid waste treatment. This objective is particularly important in environmentally sensitive areas, such as the Mediterranean Sea, where fleet deployment time is significant. Prohibitions on ocean dumping and anticipated requirements on effluent discharge quality have led the Navy to continue the research, development, and demonstration of shipboard systems to treat their unpreventable wastes. For solid, non-hazardous wastes, post-minimization efforts are geared toward long-term development of systems to thermally pyrolyze and oxidize the wastes into significantly reduced volume and weight.

  5. Quantification of Nicotine, Cotinine, trans-3’-Hydroxycotinine, Nornicotine and Norcotinine in Human Meconium by Liquid Chromatography Tandem Mass Spectrometry

    PubMed Central

    Gray, Teresa R.; Shakleya, Diaa M.

    2009-01-01

    There are no analytical methods that simultaneously quantify nicotine, cotinine, trans-3’-hydroxycotinine, nornicotine and norcotinine in human meconium. Such a method could improve identification of in utero tobacco exposure, determine if maternal dose-meconium concentration relationships exist, and whether nicotine meconium concentrations predict neonatal outcomes. The first liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry method for simultaneous quantification of these analytes in meconium was developed and validated. Specimen preparation included homogenization, enzyme hydrolysis and solid phase extraction. The linear range was 1.25 or 5 – 500 ng/g. Method applicability was evaluated with meconium collected from an in utero tobacco exposed infant. PMID:18243821

  6. Quantification of individual phenolic compounds' contribution to antioxidant capacity in apple: a novel analytical tool based on liquid chromatography with diode array, electrochemical, and charged aerosol detection.

    PubMed

    Plaza, Merichel; Kariuki, James; Turner, Charlotta

    2014-01-15

    Phenolics, particularly from apples, hold great interest because of their antioxidant properties. In the present study, the total antioxidant capacity of different apple extracts obtained by pressurized hot water extraction (PHWE) was determined by cyclic voltammetry (CV), which was compared with the conventional antioxidant assays. To measure the antioxidant capacity of individual antioxidants present in apple extracts, a novel method was developed based on high-performance liquid chromatography (HPLC) with photodiode array (DAD), electrochemical (ECD), and charged aerosol (CAD) detection. HPLC-DAD-ECD-CAD enabled rapid, qualitative, and quantitative determination of antioxidants in the apple extracts. The main advantage of using CAD was that this detector enabled quantification of a large number of phenolics using only a few standards. The results showed that phenolic acids and flavonols were mainly responsible for the total antioxidant capacity of apple extracts. In addition, protocatechuic acid, chlorogenic acid, hyperoside, an unidentified phenolic acid, and a quercetin derivative presented the highest antioxidant capacities. PMID:24345041

  7. A rapid method for the simultaneous quantification of the major tocopherols, carotenoids, free and esterified sterols in canola (Brassica napus) oil using normal phase liquid chromatography.

    PubMed

    Flakelar, Clare L; Prenzler, Paul D; Luckett, David J; Howitt, Julia A; Doran, Gregory

    2017-01-01

    A normal phase high performance liquid chromatography (HPLC) method was developed to simultaneously quantify several prominent bioactive compounds in canola oil vis. α-tocopherol, γ-tocopherol, δ-tocopherol, β-carotene, lutein, β-sitosterol, campesterol and brassicasterol. The use of sequential diode array detection (DAD) and tandem mass spectrometry (MS/MS) allowed direct injection of oils, diluted in hexane without derivatisation or saponification, greatly reducing sample preparation time, and permitting the quantification of both free sterols and intact sterol esters. Further advantages over existing methods included increased analytical selectivity, and a chromatographic run time substantially less than other reported normal phase methods. The HPLC-DAD-MS/MS method was applied to freshly extracted canola oil samples as well as commercially available canola, palm fruit, sunflower and olive oils. PMID:27507459

  8. Development and validation of a liquid chromatography mass spectrometry assay for the simultaneous quantification of methadone, cocaine, opiates and metabolites in human umbilical cord

    PubMed Central

    de Castro, Ana; Concheiro, Marta; Shakleya, Diaa M.; Huestis, Marilyn A.

    2011-01-01

    A liquid chromatography mass spectrometric selected reaction monitoring mode (SRM) method for methadone, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), cocaine, benzoylecgonine (BE), 6-acetylmorphine, morphine and codeine quantification in human umbilical cord was developed and fully validated. Analytes were extracted from homogenized tissue (1 g) by solid phase extraction. Linearity was 2.5–500 ng/g, except for methadone (10–2000 ng/g). Method imprecision was <12.7%CV with analytical recovery 85.9–112.7%, extraction efficiency >59.2%, matrix effect 4.5–39.5%, process efficiency 48.6–92.6% and stability >84.6%. Analysis of an umbilical cord following controlled methadone administration and illicit drug use contained in ng/g, 40.3 morphine, 3.6 codeine, 442 BE, 186 methadone and 45.9 EDDP. PMID:19656745

  9. Subsurface disposal of liquid low-level radioactive wastes at Oak Ridge, Tennessee

    SciTech Connect

    Stow, S.H.; Haase, C.S.

    1986-01-01

    At Oak Ridge National Laboratory (ORNL) subsurface injection has been used to dispose of low-level liquid nuclear waste for the last two decades. The process consists of mixing liquid waste with cement and other additives to form a slurry that is injected under pressure through a cased well into a low-permeability shale at a depth of 300 m (1000 ft). The slurry spreads from the injection well along bedding plane fractures and forms solid grout sheets of up to 200 m (660 ft) in radius. Using this process, ORNL has disposed of over 1.5 x 10/sup 6/ Ci of activity; the principal nuclides are /sup 90/Sr and /sup 137/Cs. In 1982, a new injection facility was put into operation. Each injection, which lasts some two days, results in the emplacement of approximately 750,000 l (180,000 gal) of slurry. Disposal cost per liter is approximately $0.30, including capital costs of the facility. This subsurface disposal process is fundamentally different from other operations. Wastes are injected into a low-permeability aquitard, and the process is designed to isolate nuclides, preventing dispersion in groundwaters. The porosity into which wastes are injected is created by hydraulically fracturing the host formation along bedding planes. The site is in the structurally complex Valley and Ridge Province. The stratigraphy consists of lower Paleozoic rocks. Investigations are under way to determine the long-term hydrologic isolation of the injection zone and the geochemical impact of saline groundwater on nuclide mobility. Injections are monitored by gamma-ray logging of cased observation wells to determine grout sheet orientation after an injection. Recent monitoring work has involved the use of tiltmeters, surface uplift surveys, and seismic arrays. 26 refs., 7 figs.

  10. Radwaste desk reference - Volume 3, Part 1: Processing liquid waste. Final report

    SciTech Connect

    Deltete, D.; Fisher, S.; Kelly, J.J.; Mis, F.; Miller, C.; Soto, R.; Vance, J.

    1994-05-01

    EPRI began, late in 1987, to produce a Radwaste Desk Reference that would allow each of the member utilities access to the available information and expertise on radwaste management. EPRI considers this important because radwaste management involves a wide variety of scientific and engineering disciplines. These include chemical and mechanical engineering, chemistry, and health physics. Radwaste management also plays a role in implementing a wide variety of regulatory requirements. These include plant-specific technical specifications, NRC standards for protection against radiation, DOE transportation regulations and major environmental legislation such as the Resource Conservation and Recovery Act. EPRI chose a question and answer format because it could be easily accessed by radwaste professionals with a variety of interests. The questions were generated at two meetings of utility radwaste professionals and EPRI contractors. The names of the participants and their affiliation appear in the acknowledgments. The questions were organized using the matrix which appears in the introduction and below. During the writing phase, some questions were combined and new questions added. To aid the reader, each question was numbered and tied to individual Section Contents. An extensive index provides additional reader assistance. EPRI chose authors who are acknowledged experts in their fields and good communicators. Each author focused her or his energies on specific areas of radwaste management activities, thereby contributing to one or more volumes of the Radwaste Desk Reference. Volume 1, which is already in publication, addresses dry active waste generation, processing and measurement. Volume 2 addresses low level waste storage, transportation and disposal. This volume, Volume 3, is being issued in two parts. Part 1 concentrates on the processing of liquid radioactive waste, whereas Part 2 addresses liquid waste management.

  11. Liquid and gas permeabilities of unsaturated municipal solid waste under compression

    NASA Astrophysics Data System (ADS)

    Stoltz, Guillaume; Gourc, Jean-Pierre; Oxarango, Laurent

    2010-10-01

    A novel set of experimental apparatus was designed and constructed to study the changes in the fluid-flow properties of municipal solid waste (MSW) related to the physical evolution of its structure under compression. The vertical liquid and gas permeabilities of MSW samples were measured in a laboratory-constructed cell termed an oedopermeameter. Another original device, a gas pycnometer, was employed to assess the volumetric gas content of the porous medium. Finally, the horizontal gas permeability of the compressed MSW sample was measured using another laboratory-constructed cell called a transmissivimeter. The results made it possible to characterise the intrinsic gas permeability as a function of porosity. Additionally, gas permeability measurements of samples with different liquid contents allowed the derivation of gas permeability correlations as functions of the physical parameters of the medium. A unique relationship was found between the gas permeability and the volumetric gas content.

  12. Detection of free liquid in drums of radioactive waste. [Patent application

    DOEpatents

    Not Available

    1979-10-16

    A nondestructive thermal imaging method for detecting the presence of a liquid such as water within a sealed container is described. The process includes application of a low amplitude heat pulse to an exterior surface area of the container, terminating the heat input and quickly mapping the resulting surface temperatures. The various mapped temperature values can be compared with those known to be normal for the container material and substances in contact. The mapped temperature values show up in different shades of light or darkness that denote different physical substances. The different substances can be determined by direct observation or by comparison with known standards. The method is particularly applicable to the detection of liquids above solidified radioactive wastes stored in sealed containers.

  13. Environmental sampling program for a solar evaporation pond for liquid radioactive wastes

    SciTech Connect

    Romero, R.; Gunderson, T.C.; Talley, A.D.

    1980-04-01

    Los Alamos Scientific Laboratory (LASL) is evaluating solar evaporation as a method for disposal of liquid radioactive wastes. This report describes a sampling program designed to monitor possible escape of radioactivity to the environment from a solar evaporation pond prototype constructed at LASL. Background radioactivity levels at the pond site were determined from soil and vegetation analyses before construction. When the pond is operative, the sampling program will qualitatively and quantitatively detect the transport of radioactivity to the soil, air, and vegetation in the vicinity. Possible correlation of meteorological data with sampling results is being investigated and measures to control export of radioactivity by biological vectors are being assessed.

  14. A&M. Hot liquid waste treatment building (TAN616). Contextual view, facing ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    A&M. Hot liquid waste treatment building (TAN-616). Contextual view, facing south. Wall of hot shop (TAN-607) with high bay at left of view. Lower-roofed building at left edge of view is TAN- 633, hot cell annex. Complex at center of view is TAN-616. Tall metal building with gable roof is TAN-615. Photographer: Ron Paarmann. Date: September 22, 1997. INEEL negative no. HD-20-2-2 - Idaho National Engineering Laboratory, Test Area North, Scoville, Butte County, ID

  15. Process for converting sodium nitrate-containing, caustic liquid radioactive wastes to solid insoluble products

    DOEpatents

    Barney, Gary S.; Brownell, Lloyd E.

    1977-01-01

    A method for converting sodium nitrate-containing, caustic, radioactive wastes to a solid, relatively insoluble, thermally stable form is provided and comprises the steps of reacting powdered aluminum silicate clay, e.g., kaolin, bentonite, dickite, halloysite, pyrophyllite, etc., with the sodium nitrate-containing radioactive wastes which have a caustic concentration of about 3 to 7 M at a temperature of 30.degree. C to 100.degree. C to thereby entrap the dissolved radioactive salts in the aluminosilicate matrix. In one embodiment the sodium nitrate-containing, caustic, radioactive liquid waste, such as neutralized Purex-type waste, or salts or oxide produced by evaporation or calcination of these liquid wastes (e.g., anhydrous salt cake) is converted at a temperature within the range of 30.degree. C to 100.degree. C to the solid mineral form-cancrinite having an approximate chemical formula 2(NaAlSiO.sub.4) .sup.. xSalt.sup.. y H.sub.2 O with x = 0.52 and y = 0.68 when the entrapped salt is NaNO.sub.3. In another embodiment the sodium nitrate-containing, caustic, radioactive liquid is reacted with the powdered aluminum silicate clay at a temperature within the range of 30.degree. C to 100.degree. C, the resulting reaction product is air dried eitheras loose powder or molded shapes (e.g., bricks) and then fired at a temperature of at least 600.degree. C to form the solid mineral form-nepheline which has the approximate chemical formula of NaAlSiO.sub.4. The leach rate of the entrapped radioactive salts with distilled water is reduced essentially to that of the aluminosilicate lattice which is very low, e.g., in the range of 10.sup.-.sup.2 to 10.sup.-.sup.4 g/cm.sup.2 -- day for cancrinite and 10.sup.-.sup.3 to 10.sup.-.sup.5 g/cm.sup.2 -- day for nepheline.

  16. Detection, quantification and confirmation of anabolic steroids in equine plasma by liquid chromatography and tandem mass spectrometry.

    PubMed

    Guan, Fuyu; Uboh, Cornelius E; Soma, Lawrence R; Luo, Yi; Rudy, Jeffery; Tobin, Thomas

    2005-12-27

    Anabolic androgenic steroids are related to the male sex hormones and are abused in equine sports. In an effort to deter the abuse of anabolic steroids, a sensitive LC-MS/MS method was developed for detection, quantification and confirmation of eight major anabolic steroids (testosterone, normethandrolone, nandrolone, boldenone, methandrostenolone, tetrahydrogestrinone (THG), trenbolone, and stanozolol) in equine plasma. Formation of solvent adduct ions of the analytes was observed under electrospray ionization (ESI) conditions, and desolvation of the solvent adduct ions by source collision-induced decomposition (CID) increased the abundance of the [M+H]+ ions as well as the multiple-reaction monitoring (MRM) signals. ESI (+) and APCI (+) were compared with respect to sensitivity for the analytes and the former provided better sensitivity. The matrix effect on ion suppression or enhancement was evaluated, and was negligible. Confirmation of the analytes was performed using criteria of three ion transitions and LC retention time of each analyte. The limit of detection (LOD) and quantification (LOQ) was 25 pg/mL. The limit of confirmation (LOC) was 25 pg/mL for boldenone; 50 pg/mL for normethandrolone, nandrolone, and methandrostenolone; and 100 pg/mL for testosterone, THG, trenbolone, and stanozolol. The analytes were evaluated for stability and found to be stable in plasma for 24h at room temperature, 13 days at 4 degrees C, and 34 days at -20 and -70 degrees C. The method was successfully applied to analyses of equine plasma samples for pharmacokinetics study. This method is sensitive and useful for detection, quantification and confirmation of these anabolic steroids in equine plasma. PMID:16289956

  17. Conversion of waste polypropylene to liquid fuel using acid-activated kaolin.

    PubMed

    Panda, Achyut K; Singh, R K

    2014-10-01

    Waste polypropylene was subjected to thermal degradation in the presence of kaolin and acid-treated kaolin, with different catalyst-to-plastics ratios, in a semi-batch reactor at a temperature range of 400-550°C to obtain optimized process conditions for the production of liquid fuels. The effects of process temperature, catalyst and feed composition on yield and quality of the oil were determined. For a thermal decomposition reaction at up to 450°C, the major product is volatile oil; and the major products at a higher temperature (475-550°C) are either viscous liquid or wax. The highest yield of condensed fraction in the thermal reaction is 82.85% by weight at 500°C. Use of kaolin and acid-treated kaolin as a catalyst decreased the reaction time and increased the yield of liquid fraction. The major product of catalysed degradation at all temperatures is highly volatile liquid oil. The maximum oil yield using kaolin and acid-treated kaolin is 87.5% and 92%, respectively, at 500°C. The oil obtained was characterized using GC-MS for its composition and different fuel properties by IS methods. PMID:25135440

  18. Buprenorphine and norbuprenorphine quantification in human plasma by simple protein precipitation and ultra-high performance liquid chromatography tandem mass spectrometry.

    PubMed

    Lüthi, Guillaume; Blangy, Valeria; Eap, Chin B; Ansermot, Nicolas

    2013-04-15

    A highly sensitive ultra-high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) method was developed for the quantification of buprenorphine and its major metabolite norbuprenorphine in human plasma. In order to speed up the process and decrease costs, sample preparation was performed by simple protein precipitation with acetonitrile. To the best of our knowledge, this is the first application of this extraction technique for the quantification of buprenorphine in plasma. Matrix effects were strongly reduced and selectivity increased by using an efficient chromatographic separation on a sub-2 μm column (Acquity UPLC BEH C18 1.7 μm, 2.1×50 mm) in 5 min with a gradient of ammonium formate 20 mM pH 3.05 and acetonitrile as mobile phase at a flow rate of 0.4 ml/min. Detection was made using a tandem quadrupole mass spectrometer operating in positive electrospray ionization mode, using multiple reaction monitoring. The procedure was fully validated according to the latest Food and Drug Administration guidelines and the Société Française des Sciences et Techniques Pharmaceutiques. Very good results were obtained by using a stable isotope-labeled internal standard for each analyte, to compensate for the variability due to the extraction and ionization steps. The method was very sensitive with lower limits of quantification of 0.1 ng/ml for buprenorphine and 0.25 ng/ml for norbuprenorphine. The upper limit of quantification was 250 ng/ml for both drugs. Trueness (98.4-113.7%), repeatability (1.9-7.7%), intermediate precision (2.6-7.9%) and internal standard-normalized matrix effects (94-101%) were in accordance with international recommendations. The procedure was successfully used to quantify plasma samples from patients included in a clinical pharmacogenetic study and can be transferred for routine therapeutic drug monitoring in clinical laboratories without further development. PMID:23357637

  19. Quantification of landfill methane using modified Intergovernmental Panel on Climate Change's waste model and error function analysis.

    PubMed

    Govindan, Siva Shangari; Agamuthu, P

    2014-10-01

    Waste management can be regarded as a cross-cutting environmental 'mega-issue'. Sound waste management practices support the provision of basic needs for general health, such as clean air, clean water and safe supply of food. In addition, climate change mitigation efforts can be achieved through reduction of greenhouse gas emissions from waste management operations, such as landfills. Landfills generate landfill gas, especially methane, as a result of anaerobic degradation of the degradable components of municipal solid waste. Evaluating the mode of generation and collection of landfill gas has posted a challenge over time. Scientifically, landfill gas generation rates are presently estimated using numerical models. In this study the Intergovernmental Panel on Climate Change's Waste Model is used to estimate the methane generated from a Malaysian sanitary landfill. Key parameters of the model, which are the decay rate and degradable organic carbon, are analysed in two different approaches; the bulk waste approach and waste composition approach. The model is later validated using error function analysis and optimum decay rate, and degradable organic carbon for both approaches were also obtained. The best fitting values for the bulk waste approach are a decay rate of 0.08 y(-1) and degradable organic carbon value of 0.12; and for the waste composition approach the decay rate was found to be 0.09 y(-1) and degradable organic carbon value of 0.08. From this validation exercise, the estimated error was reduced by 81% and 69% for the bulk waste and waste composition approach, respectively. In conclusion, this type of modelling could constitute a sensible starting point for landfills to introduce careful planning for efficient gas recovery in individual landfills. PMID:25323145

  20. Use of textile waste water along with liquid NPK fertilizer for production of wheat on saline sodic soils.

    PubMed

    Yaseen, Muhammad; Aziz, Muhammad Zahir; Jafar, Abdul Aleem; Naveed, Muhammad; Saleem, Muhammad

    2016-05-01

    A field experiment in collaboration with a private textile industry (Noor Fatima Fabrics Private (Ltd.), Faisalabad) was conducted to evaluate the effect of disposed water from bleaching unit, printing unit and end drain for improving growth and yield of wheat under saline sodic soil. Textile waste water along with canal water (control) was applied with and without liquid NPK fertilizer. The application of liquid NPK fertilizer with end drain waste water increased plant height, spike length, flag leaf length, root length, number of tillers (m(-2)), number of fertile tillers (m(-2)), 1000 grain weight, grain yield, straw yield and biological yield up to 21, 20, 20, 44, 17, 20, 14, 44, 40 and 41%, respectively compared to canal water (control). Similarly, the NPK uptake in grain was increased up to 15, 30 and 28%, respectively by liquid fertilizer treated end drain water as compare to canal water with liquid fertilizer. Moreover, concentration of different heavy metals particularly Cu, Cr, Pb and Cd was decreased in grains by application of waste water along with liquid NPK. The result may imply that waste water application along with liquid-NPK could be a novel approach for improving growth and yield of wheat in saline sodic soils. PMID:26515426

  1. High performance liquid chromatography for quantification of gatifloxacin in rat plasma following automated on-line solid phase extraction.

    PubMed

    Tasso, Leandro; Dalla Costa, Teresa

    2007-05-01

    An automated system using on-line solid phase extraction and HPLC with fluorimetric detection was developed and validated for quantification of gatifloxacin in rat plasma. The extraction was carried out using C(18) cartridges (BondElut), with a high extraction yield. After washing, gatifloxacin was eluted from the cartridge with mobile phase onto a C(18) HPLC column. The mobile phase consisted of a mixture of phosphoric acid (2.5mM), methanol, acetonitrile and triethylamine (64.8:15:20:0.2, v/v/v/v, apparent pH(app.) 2.8). All samples and standard solutions were chromatographed at 28 degrees C. The method developed was selective and linear for drug concentrations ranging between 20 and 600 ng/ml. Gatifloxacin recovery ranged from 95.6 to 99.7%, and the limit of quantification was 20 ng/ml. The intra and inter-assay accuracy were up to 94.3%. The precision determined not exceed 5.8% of the CV. High extraction yield up to 95% was obtained. Drug stability in plasma was shown in freezer at -20 degrees C up to 1 month, after three freeze-thaw cycles and for 24h in the autosampler after processing. The assay has been successfully applied to measure gatifloxacin plasma concentrations in pharmacokinetic study in rats. PMID:17403594

  2. Comparison of a high-performance liquid chromatography method for quantification of carbamazepine with chemiluminescent microparticle immunoassay.

    PubMed

    Guerrero Garduño, Óscar; González-Esquivel, Dinora F; Escalante-Membrillo, Carmen; Fernández, Ángeles; Rojas-Tomé, Irma Susana; Jung Cook, Helgi; Castro, Nelly

    2016-06-01

    Carbamazepine is an antiepileptic drug widely used for the treatment of epilepsy. In the National Institute of Neurology, monitoring has been performed using the technique chemiluminescent microparticle immunoassay (CMIA) in an automated way during the last five years. The aim of this study was to develop a simple and rapid HPLC analytical method coupled to DAD-UV detection for the determination of plasma concentrations of carbamazepine and compare its feasibility with those used in routine analysis. The developed HPLC method was fully validated and the applicability of the proposed method was verified through the analysis of plasma samples of patients and later compared with the quantification of the same plasma samples with the CMIA method. The limit of quantification obtained was 0.5 μg/mL. The mean value for recovery was 99.05% and the coefficient of variation (CV) was 5.6%. The precision and accuracy of this method were within the acceptable limits; inter- and intraday CV values were <10%. The correlation between the CMIA method and the developed HPLC method was very good (r ≈ 0.999). A Bland-Altman plot showed no significant bias between the results. The HPLC-DAD method may be an alternative to determine and monitoring the carbamazepine levels in human plasma or serum. Copyright © 2015 John Wiley & Sons, Ltd. PMID:26433002

  3. High-performance liquid chromatographic method for the quantification of Mitragyna inermis alkaloids in order to perform pharmacokinetic studies.

    PubMed

    Sinou, Veronique; Fiot, Julien; Taudon, Nicolas; Mosnier, Joël; Martelloni, Maryse; Bun, Sok S; Parzy, Daniel; Ollivier, Evelyne

    2010-06-01

    In Africa, Mitragyna inermis (Willd.) O. Kuntze (Rubiaceae) is commonly used in traditional medicine to treat malaria. Antimalarial activity is mostly due to the hydromethanolic extract of M. inermis leaves and especially to the main alkaloids, uncarine D and isorhynchophilline. In the present study, we describe for the first time an HPLC method for the simultaneous quantification of uncarine D and isorhynchophylline in biological matrices. SPE was used to extract the components and the internal standard naphthalene from human and pig plasma samples. Chromatographic separation was performed on a C-18 reversed column at a flow rate of 1 mL/min, using methanol-phosphate buffer (10:90, pH 7), as a mobile phase. Good linearity was observed over the concentration ranges of 0.0662-3.31 microg/mL for uncarine D and 0.0476-2.38 microg/mL for isorynchophylline. The precision was less than 12% and the accuracy was from 86 to 107% without any discrepancy between the two species. Uncarine D and isorhynchophylline recoveries were over 80%. These results allowed the quantification of both uncarine D and isorhynchophylline in pig plasma after intravenous administration of M. inermis extract. PMID:20437411

  4. Liquid chromatography/electrospray ionisation-tandem mass spectrometry quantification of GM2 gangliosides in human peripheral cells and plasma.

    PubMed

    Fuller, Maria; Duplock, Stephen; Hein, Leanne K; Rigat, Brigitte A; Mahuran, Don J

    2014-08-01

    GM2 gangliosidosis is a group of inherited neurodegenerative disorders resulting primarily from the excessive accumulation of GM2 gangliosides (GM2) in neuronal cells. As biomarkers for categorising patients and monitoring the effectiveness of developing therapies are lacking for this group of disorders, we sought to develop methodology to quantify GM2 levels in more readily attainable patient samples such as plasma, leukocytes, and cultured skin fibroblasts. Following organic extraction, gangliosides were partitioned into the aqueous phase and isolated using C18 solid-phase extraction columns. Relative quantification of three species of GM2 was achieved using LC/ESI-MS/MS with d35GM1 18:1/18:0 as an internal standard. The assay was linear over the biological range, and all GM2 gangliosidosis patients were demarcated from controls by elevated GM2 in cultured skin fibroblast extracts. However, in leukocytes only some molecular species could be used for differentiation and in plasma only one was informative. A reduction in GM2 was easily detected in patient skin fibroblasts after a short treatment with media from normal cells enriched in secreted β-hexosaminidase. This method may show promise for measuring the effectiveness of experimental therapies for GM2 gangliosidosis by allowing quantification of a reduction in the primary storage burden. PMID:24769373

  5. Waste Characterization Data Manual for the inactive liquid low-level waste tank systems at Oak Ridge National Laboratory, Oak Ridge, Tennessee. Environmental Restoration Program

    SciTech Connect

    Not Available

    1993-06-01

    This Waste Characterization Data Manual contains the results of an analysis of the contents of liquid low-level waste (LLLW) tanks that have been removed from service in accordance with the requirements of the Oak Ridge National Laboratory (ORNL) Federal Facility Agreement (FFA), Section IX.G.1. Section IX.G.1 of the FFA requires waste characterizations be conducted and provided to EPA and TDEC for all LLLW tanks that are removed from service. These waste characterizations shall include the results of sampling and analysis of the tank contents, including wastes, liquids, and sludges. This manual was first issued as ORNL/ER-80 in June 1992. The waste characterization data were extracted from ORNL reports that described tank sampling and analysis conducted in 1988 for 32 out-of-service tanks. This revision of the manual contains waste characterization data for 54 tanks, including the 32 tanks from the 1988 sampling campaign (Sects. 2.1 through 2.32) and the 22 additional tanks from a subsequent sampling campaign in 1992 and 1993 (Sects. 2.33 through 2.54). Data are presented from analyses of volatile organic compounds, semivolatile organic compounds, polychlorinated biphenyls (PCBs), pesticides, radiochemical compounds, and inorganic compounds. As additional data resulting from analyses of out-of-service tank samples become available, they will be added to this manual.

  6. Scale up issues involved with the ceramic waste form : ceramic-container interactions and ceramic cracking quantification.

    SciTech Connect

    Bateman, K. J.; DiSanto, T.; Goff, K. M.; Johnson, S. G.; O'Holleran, T.; Riley, W. P., Jr.

    1999-05-03

    Argonne National Laboratory is developing a process for the conditioning of spent nuclear fuel to prepare the material for final disposal. Two waste streams will result from the treatment process, a stainless steel based form and a ceramic based form. The ceramic waste form will be enclosed in a stainless steel container. In order to assess the performance of the ceramic waste form in a repository two factors must be examined, the surface area increases caused by waste form cracking and any ceramic/canister interactions that may release toxic material. The results indicate that the surface area increases are less than the High Level Waste glass and any toxic releases are below regulatory limits.

  7. Pyrolysis characteristics and pyrolysis products separation for recycling organic materials from waste liquid crystal display panels.

    PubMed

    Wang, Ruixue; Xu, Zhenming

    2016-01-25

    Waste liquid crystal display (LCD) panels mainly contain inorganic materials (glass substrate with indium-tin oxide film), and organic materials (polarizing film and liquid crystal). The organic materials should be removed beforehand since the organic matters would hinder the indium recycling process. In the present study, pyrolysis process is used to remove the organic materials and recycle acetic as well as and triphenyl phosphate (TPP) from waste LCD panels in an environmental friendly way. Several highlights of this study are summarized as follows: (i) Pyrolysis characteristics and pyrolysis kinetics analysis are conducted which is significant to get a better understanding of the pyrolysis process. (ii) Optimum design is developed by applying Box-Behnken Design (BBD) under response surface methodology (RSM) for engineering application which is significant to guide the further industrial recycling process. The oil yield could reach 70.53 wt% and the residue rate could reach 14.05 wt% when the pyrolysis temperature is 570 °C, nitrogen flow rate is 6 L min(-1) and the particle size is 0.5 mm. (iii) Furthermore, acetic acid and TPP are recycled, and then separated by rotary evaporation, which could reduce the consumption of fossil energy for producing acetic acid, and be reused in electronics manufacturing industry. PMID:26444486

  8. Double liquid membrane system for the removal of actinides and lanthanides from acidic nuclear wastes

    SciTech Connect

    Chiarizia, R.; Danesi, P.R.

    1985-01-01

    Supported liquid membranes (SLM), consisting of an organic solution of n-octyl-(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO) and tributyl-phosphate (TBP) in decalin are able to perform selective separation and concentration of actinide and lanthanide ions from aqueous nitrate feed solutions and synthetic nuclear wastes. In the membrane process a possible strip solution is a mixture of formic acid and hydroxylammonium formate (HAF). The effectiveness of this strip solution is reduced and eventually nullified by the simultaneous transfer through the SLM of nitric acid which accumulates in the strip solution. A possible way to overcome this drawback is to make use of a second SLM consisting of a primary amine which is able to extract only HNO/sub 3/ from the strip solution. In this work the results obtained by experimentally studying the membrane system: synthetic nuclear waste/CMPO-TBP membrane/HCOOH-HAF strip solution/primary amine membrane/NaOH solution, are reported. They show that the use of a second liquid membrane is effective in controlling the HNO/sub 3/ concentration in the strip solution, thus allowing the actinide and lanthanide ions removal from the feed solution to proceed to completion. 15 refs., 10 figs., 1 tab.

  9. Double liquid membrane system for the removal of actinides and lanthanides from acidic nuclear wastes

    SciTech Connect

    Chiarizia, R.; Danesi, P.R.

    1987-01-01

    Supported liquid membranes (SLM), consisting of an organic solution of n-octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide (CMPO) and tributyl-phosphate (TBP) in decalin are able to perform selective separation and concentration of actinide and lanthanide ions from aqueous nitrate feed solutions and synthetic nuclear wastes. In the membrane process a possible strip solution is a mixture of formic acid and hydroxylammonium formate (HAF). The effectiveness of this strip solution is reduced and eventually nullified by the simultaneous transfer through the SLM of HNO3 which accumulates in the strip solution. A possible way to overcome this drawback is to make use of a second SLM consisting of a primary amine which is able to extract only HNO3 from the strip solution. In this work the results obtained by experimentally studying the membrane system: synthetic nuclear waste/CMPO-TBP membrane/HCOOH-HAF strip solution/primary amine membrane/NaOH solution, are reported. They show that the use of a second liquid membrane is effective in controlling the HNO3 concentration in the strip solution, thus allowing the actinide and lanthanide ions removal from the feed solution to proceed to completion.

  10. Nitrous oxide supersaturation at the liquid/air interface of animal waste.

    PubMed

    Makris, Konstantinos C; Andra, Syam S; Hardy, Michael; Sarkar, Dibyendu; Datta, Rupali; Bach, Stephan B H; Mullens, Conor P

    2009-12-01

    Concentrated animal feeding operations around the globe generate large amounts of nitrous oxide (N(2)O) in the surrounding atmosphere. Liquid animal waste systems have received little attention with respect to N(2)O emissions. We hypothesized that the solution chemistry of animal waste aqueous suspensions would promote conditions that lead to N(2)O supersaturation at the liquid/air interface. The concentration of dissolved N(2)O in poultry litter (PL) aqueous suspensions at 25 degrees C was 0.36 microg N(2)O mL(-1), at least an order of magnitude greater than that measured in water in equilibrium with ambient air, suggesting N(2)O supersaturation. There was a nonlinear increase in the N(2)O Henry constants of PL from 2810 atm/mole fraction at 35 degrees C to 17 300 atm/mole fraction at 41 degrees C. The extremely high N(2)O Henry constants were partially ascribed to N(2)O complexation with aromatic moieties. Complexed N(2)O structures were unstable at temperatures > 35 degrees C, supplying the headspace with additional free N(2)O concentrations. PMID:19573962

  11. Some methods of human liquid and solid wastes utilization in bioregenerative life support systems

    NASA Astrophysics Data System (ADS)

    Tikhomirova, N. A.; Ushakova, S. Á.; Tikhomirov, A. Á.; Zolotukhin, I. G.; Gribovskaya, I. V.; Gros, J. B.

    The possibility of stepwise utilization of human liquid and solid wastes with the purpose of an increase of a closure degree of bioregenerative life support systems BLSS and sodium chloride inclusion in the organic matter turnover was investigated On the first stage urine and faeces were subjected to oxidation by Yu A Kudenko physicochemical method On the next stage the products of human liquid and solid wastes oxidation were used for roots nutrition of wheat grown by substrate culture method Soil-like substrate the technology of which was described earlier was used as a substrate After the wheat cultivation the irrigational solution and the solution obtained in the result of substrate washing containing mineral elements not absorbed by the plants were used for cultivation of salt-tolerant Salicornia europaea plants The above-ground biomass of these vegetables can be used as a food and roots washed from dissoluble mineral elements can be added to the soil-like substrate Four consecutive wheat and Salicornia europaea vegetations were cultivated In the result of this complex technology of wheat and Salicornia europaea cultivation the soil-like substrate salinization by NaCl introduced into the irrigational solution together with the products of urine oxidation has considerably decreased

  12. Catalytic conversion of carbohydrates to 5-hydroxymethylfurfural from the waste liquid of acid hydrolysis NCC.

    PubMed

    Sun, Yonghui; Liu, Pengtao; Liu, Zhong

    2016-05-20

    The principal goal of this work was to reuse the carbohydrates and recycle sulfuric acid in the waste liquid of acid hydrolysis nanocrystalline cellulose (NCC). Therefore, in this work, the optimizations of further hydrolysis of waste liquid of acid hydrolysis NCC and catalytic conversion of L4 to 5-hydroxymethylfurfural (5-HMF) were studied. Sulfuric acid was separated by spiral wound diffusion dialysis (SWDD). The results revealed that cellulose can be hydrolyze to glucose absolutely under the condition of temperature 35 °C, 3 h, and sulfuric acid's concentration 62 wt%. And 78.3% sulfuric acid was recovered by SWDD. The yield of 5-HMF was highest in aqueous solution under the optimal condition was as follows, temperature 160 °C, 3 h, and sulfuric acid's concentration 12 wt%. Then the effect of biphasic solvent systems catalytic conversion and inorganic salt as additives were still examined. The results showed that both of them contributed to prepare 5-HMF. The yield and selectivity of 5-HMF was up to 21.0% and 31.4%, respectively. PMID:26917388

  13. Spanish LLW and MLW disposal: durability of cemented materials in (Na, K)Cl simulated radioactive liquid waste.

    PubMed

    Goñi, S; Guerrero, A; Hernández, M S

    2001-01-01

    The microstructural stability or durability of a specific backfilling pozzolanic-cement mortar, which is employed in Spain, in concrete containers for the storage of low level liquid wastes (LLW) and medium level liquid wastes (MLW), has been studied by means of the Koch-Steinegger test at the temperatures of 20 and 40 degrees C during a period of 365 days. Mortar samples were immersed in salt solutions of 3.46 M NaCl and 3.46 M KCl to simulate the salinity of some radioactive liquid waste matrices. The resistance of the mortar to the saline solution attack is evaluated by the development of the relative flexural strength. The changes of the microstructure were followed by mercury intrusion porosimetry (MIP), scanning electron microscopy (SEM) and X-ray diffraction (XRD). Pore solution was extracted and analyzed at different periods of time to know the possible diffusion of sodium, chloride and potassium inside the microstructure. PMID:11150135

  14. Hanford Facility dangerous waste permit application, liquid effluent retention facility and 200 area effluent treatment facility

    SciTech Connect

    Coenenberg, J.G.

    1997-08-15

    The Hanford Facility Dangerous Waste Permit Application is considered to 10 be a single application organized into a General Information Portion (document 11 number DOE/RL-91-28) and a Unit-Specific Portion. The scope of the 12 Unit-Specific Portion is limited to Part B permit application documentation 13 submitted for individual, `operating` treatment, storage, and/or disposal 14 units, such as the Liquid Effluent Retention Facility and 200 Area Effluent 15 Treatment Facility (this document, DOE/RL-97-03). 16 17 Both the General Information and Unit-Specific portions of the Hanford 18 Facility Dangerous Waste Permit Application address the content of the Part B 19 permit application guidance prepared by the Washington State Department of 20 Ecology (Ecology 1987 and 1996) and the U.S. Environmental Protection Agency 21 (40 Code of Federal Regulations 270), with additional information needs 22 defined by the Hazardous and Solid Waste Amendments and revisions of 23 Washington Administrative Code 173-303. For ease of reference, the Washington 24 State Department of Ecology alpha-numeric section identifiers from the permit 25 application guidance documentation (Ecology 1996) follow, in brackets, the 26 chapter headings and subheadings. A checklist indicating where information is 27 contained in the Liquid Effluent Retention Facility and 200 Area Effluent 28 Treatment Facility permit application documentation, in relation to the 29 Washington State Department of Ecology guidance, is located in the Contents 30 Section. 31 32 Documentation contained in the General Information Portion is broader in 33 nature and could be used by multiple treatment, storage, and/or disposal units 34 (e.g., the glossary provided in the General Information Portion). Wherever 35 appropriate, the Liquid Effluent Retention Facility and 200 Area Effluent 36 Treatment Facility permit application documentation makes cross-reference to 37 the General Information Portion, rather than duplicating

  15. Quantification of parameters influencing methane generation due to biodegradation of municipal solid waste in landfills and laboratory experiments.

    PubMed

    Fei, Xunchang; Zekkos, Dimitrios; Raskin, Lutgarde

    2016-09-01

    The energy conversion potential of municipal solid waste (MSW) disposed of in landfills remains largely untapped because of the slow and variable rate of biogas generation, delayed and inefficient biogas collection, leakage of biogas, and landfill practices and infrastructure that are not geared toward energy recovery. A database consisting of methane (CH4) generation data, the major constituent of biogas, from 49 laboratory experiments and field monitoring data from 57 landfills was developed. Three CH4 generation parameters, i.e., waste decay rate (k), CH4 generation potential (L0), and time until maximum CH4 generation rate (tmax), were calculated for each dataset using U.S. EPA's Landfill Gas Emission Model (LandGEM). Factors influencing the derived parameters in laboratory experiments and landfills were investigated using multi-linear regression analysis. Total weight of waste (W) was correlated with biodegradation conditions through a ranked classification scheme. k increased with increasing percentage of readily biodegradable waste (Br0 (%)) and waste temperature, and reduced with increasing W, an indicator of less favorable biodegradation conditions. The values of k obtained in the laboratory were commonly significantly higher than those in landfills and those recommended by LandGEM. The mean value of L0 was 98 and 88L CH4/kg waste for laboratory and field studies, respectively, but was significantly affected by waste composition with ranges from 10 to 300L CH4/kg. tmax increased with increasing percentage of biodegradable waste (B0) and W. The values of tmax in landfills were higher than those in laboratory experiments or those based on LandGEM's recommended parameters. Enhancing biodegradation conditions in landfill cells has a greater impact on improving k and tmax than increasing B0. Optimizing the B0 and Br0 values of landfilled waste increases L0 and reduces tmax. PMID:26525969

  16. Data requirements for simulation of hydrogeologic effects of liquid waste injection, Harrison and Jackson Counties, Mississippi

    USGS Publications Warehouse

    Rebich, Richard A.

    1994-01-01

    Available literature and data were reviewed to quantify data requirements for computer simulation of hydrogeologic effects of liquid waste injection in southeastern Mississippi. Emphasis of each review was placed on quantifying physical properties of current Class I injection zones in Harrison and Jackson Counties. Class I injection zones are zones that are used for injection of hazardous or non-hazardous liquid waste below a formation containing the lowermost underground source of drinking water located within one-quarter of a mile of the injection well. Several mathematical models have been developed to simulate injection effects. The Basic Plume Method was selected because it is commonly used in permit applications, and the Intercomp model was selected because it is generally accepted and used in injection-related research. The input data requirements of the two models were combined into a single data requirement list inclusive of physical properties of injection zones only; injected waste and well properties are not included because such information is site-specific by industry, which is beyond the scope of this report. Results of the reviews of available literature and data indicated that Class I permit applications and standard-reference chemistry and physics texts were the primary sources of information to quantify physical properties of injection zones in Harrison and Jackson Counties. With the exception of a few reports and supplementary data for one injection zone in Jackson County, very little additional information pertaining to physical properties of the injection zones was available in sources other than permit applications and standard-reference texts.

  17. Design and Testing of a Solid-Liquid Interface Monitor for High-Level Waste Tanks

    SciTech Connect

    McDaniel, D.; Awwad, A.; Roelant, D.; Srivastava, R.

    2008-07-01

    A high-level waste (HLW) monitor has been designed, fabricated and tested at full-scale for deployment inside a Hanford tank. The Solid-Liquid Interface Monitor (SLIM) integrates a commercial sonar system with a mechanical deployment system for deploying into an underground waste tank. The system has undergone several design modifications based upon changing requirements at Hanford. We will present the various designs of the monitor from first to last and will present performance data from the various prototype systems. We will also present modeling of stresses in the enclosure under 85 mph wind loading. The system must be able to function at winds up to 15 mph and must withstand a maximum loading of 85 mph. There will be several examples presented of engineering tradeoffs made as FIU analyzed new requirements and modified the design to accommodate. We will present our current plans for installing into the Cold Test Facility at Hanford and into a double-shelled tank at Hanford. Finally, we will present our vision for how this technology can be used at Hanford and Savannah River Site to improve the filling and emptying of high-level waste tanks. In conclusion: 1. The manually operated first-generation SLIM is a viable option on tanks where personnel are allowed to work on top of the tank. 2. The remote controlled second-generation SLIM can be utilized on tanks where personnel access is limited. 3. The totally enclosed fourth-generation SLIM, when the design is finalized, can be used when the possibility exists for wind dispersion of any HLW that maybe on the system. 4. The profiling sonar can be used effectively for real-time monitoring of the solid-liquid interface over a large area. (authors)

  18. Sampling and analysis plan for sampling of liquid waste streams generated by 222-S Laboratory Complex operations

    SciTech Connect

    Benally, A.B.

    1997-08-14

    This Sampling and Analysis Plan (SAP) establishes the requirements and guidelines to be used by the Waste Management Federal Services of Hanford, Inc. personnel in characterizing liquid waste generated at the 222-S Laboratory Complex. The characterization process to verify the accuracy of process knowledge used for designation and subsequent management of wastes consists of three steps: to prepare the technical rationale and the appendix in accordance with the steps outlined in this SAP; to implement the SAP by sampling and analyzing the requested waste streams; and to compile the report and evaluate the findings to the objectives of this SAP. This SAP applies to portions of the 222-S Laboratory Complex defined as Generator under the Resource Conservation and Recovery Act (RCRA). Any portion of the 222-S Laboratory Complex that is defined or permitted under RCRA as a treatment, storage, or disposal (TSD) facility is excluded from this document. This SAP applies to the liquid waste generated in the 222-S Laboratory Complex. Because the analytical data obtained will be used to manage waste properly, including waste compatibility and waste designation, this SAP will provide directions for obtaining and maintaining the information as required by WAC173-303.

  19. Development and testing of ion exchangers for treatment of liquid wastes at Oak Ridge National Laboratory

    SciTech Connect

    Collins, J.L.; Davidson, D.J.; Chase, C.W.; Egan, B.Z.; Ensor, D.D.; Bright, R.M.; Glasgow, D.C.

    1993-03-01

    This report addresses three areas of waste treatment: (1) treatment of newly generated low-level liquid waste and Melton Valley Storage Tank (MVST) supernate using inorganic ion exchangers; (2) treatment of processing streams at the Radiochemical Engineering Development Center (REDC); and (3) removal of radionuclides from organic solutions. Distribution of various radionuclides between simulated waste solutions and several sorbents was determined in batch tests. Inorganic ion exchangers were prepared in the form of microspheres by an intemal gelation process. Microspheres of hydrous titania, hydrous zirconia, hydrous titania containing embedded sodium cobalt hexacyanoferrate, and the corresponding phosphate forms of these materials were prepared. Several zeolites (PDZ-140, PDZ-300, EE-96, CBV-10A) and inorganic ion exchangers (hydrous titania, hydrous zirconia, polyantimanic acid, sodium cobalt hexacyanoferrate) were tested for the removal of cesium and strontium from the acidic simulated Cleanex raffinate generated at REDC. A resorcinol-based ion-exchange resin and three types of sodium titanate were tested for removal of cesium and strontium from the REDC caustic dissolver solution. Hydrous titania, hydrous zirconia, and their corresponding phosphates were tested for the removal of Eu{sup 3+} from various solutions of di-2-ethylbexyl phosphoric acid (HDEHP) in toluene or dodecane.

  20. EXPLORING ENGINEERING CONTROL THROUGH PROCESS MANIPULATION OF RADIOACTIVE LIQUID WASTE TANK CHEMICAL CLEANING

    SciTech Connect

    Brown, A.

    2014-04-27

    One method of remediating legacy liquid radioactive waste produced during the cold war, is aggressive in-tank chemical cleaning. Chemical cleaning has successfully reduced the curie content of residual waste heels in large underground storage tanks; however this process generates significant chemical hazards. Mercury is often the bounding hazard due to its extensive use in the separations process that produced the waste. This paper explores how variations in controllable process factors, tank level and temperature, may be manipulated to reduce the hazard potential related to mercury vapor generation. When compared using a multivariate regression analysis, findings indicated that there was a significant relationship between both tank level (p value of 1.65x10{sup -23}) and temperature (p value of 6.39x10{sup -6}) to the mercury vapor concentration in the tank ventilation system. Tank temperature showed the most promise as a controllable parameter for future tank cleaning endeavors. Despite statistically significant relationships, there may not be confidence in the ability to control accident scenarios to below mercury’s IDLH or PAC-III levels for future cleaning initiatives.

  1. Characterization and monitoring of 300 Area Facility liquid waste streams: Status report

    SciTech Connect

    Manke, K.L.; Riley, R.G.; Ballinger, M.Y.; Damberg, E.G.; Evans, J.C.; Ikenberry, A.S.; Olsen, K.B.; Ozanich, R.M.; Thompson, C.J.

    1994-09-01

    This report summarizes the results of characterizing and monitoring the following sources during a portion of this year: liquid waste streams from Buildings 331, 320, and 3720; treated and untreated Columbia River water; and water at the confluence of the waste streams (that is, end-of-pipe). Characterization and monitoring data were evaluated for samples collected between March 22 and June 21, 1994, and subsequently analyzed for hazardous chemicals, radioactivity, and general parameters. Except for bis(2-ethylhexyl)phthalate, concentrations of chemicals detected and parameters measured at end-of-pipe were below the US Environmental Protection Agency existing and proposed drinking water standards. The source of the chemicals, except bis(2-ethylhexyl)phthalate, is not currently known. The bis(2-ethylhexyl)phthalate is probably an artifact of the plastic tubing used in the early stages of the sampling program. This practice was stopped. Concentrations and clearance times for contaminants at end-of-pipe depended strongly on source concentration at the facility release point, waste stream flow rates, dispersion, and the mechanical action of sumps. When present, the action of sumps had the greatest impact on contaminant clearance times. In the absence of sump activity, dispersion and flow rate were the controlling factors.

  2. A NEW, SMALL DRYING FACILITY FOR WET RADIOACTIVE WASTE AND LIQUIDS

    SciTech Connect

    Oldiges, Olaf; Blenski, Hans-Juergen

    2003-02-27

    Due to the reason, that in Germany every Waste, that is foreseen to be stored in a final disposal facility or in a long time interim storage facility, it is necessary to treat a lot of waste using different drying technologies. In Germany two different drying facilities are in operation. The GNS Company prefers a vacuum-drying-technology and has built and designed PETRA-Drying-Facilities. In a lot of smaller locations, it is not possible to install such a facility because inside the working areas of that location, the available space to install the PETRA-Drying-Facility is too small. For that reason, GNS decided to design a new, small Drying-Facility using industrial standard components, applying the vacuum-drying-technology. The new, small Drying-Facility for wet radioactive waste and liquids is presented in this paper. The results of some tests with a prototype facility are shown in chapter 4. The main components of that new facility are described in chapter 3.

  3. Development and testing of ion exchangers for treatment of liquid wastes at Oak Ridge National Laboratory

    SciTech Connect

    Collins, J.L.; Davidson, D.J.; Chase, C.W.; Egan, B.Z. ); Ensor, D.D.; Bright, R.M.; Glasgow, D.C. )

    1993-03-01

    This report addresses three areas of waste treatment: (1) treatment of newly generated low-level liquid waste and Melton Valley Storage Tank (MVST) supernate using inorganic ion exchangers; (2) treatment of processing streams at the Radiochemical Engineering Development Center (REDC); and (3) removal of radionuclides from organic solutions. Distribution of various radionuclides between simulated waste solutions and several sorbents was determined in batch tests. Inorganic ion exchangers were prepared in the form of microspheres by an intemal gelation process. Microspheres of hydrous titania, hydrous zirconia, hydrous titania containing embedded sodium cobalt hexacyanoferrate, and the corresponding phosphate forms of these materials were prepared. Several zeolites (PDZ-140, PDZ-300, EE-96, CBV-10A) and inorganic ion exchangers (hydrous titania, hydrous zirconia, polyantimanic acid, sodium cobalt hexacyanoferrate) were tested for the removal of cesium and strontium from the acidic simulated Cleanex raffinate generated at REDC. A resorcinol-based ion-exchange resin and three types of sodium titanate were tested for removal of cesium and strontium from the REDC caustic dissolver solution. Hydrous titania, hydrous zirconia, and their corresponding phosphates were tested for the removal of Eu[sup 3+] from various solutions of di-2-ethylbexyl phosphoric acid (HDEHP) in toluene or dodecane.

  4. Liquid chromatography with tandem mass spectrometry quantification of urinary proanthocyanin A2 dimer and its potential use as a biomarker of cranberry intake.

    PubMed

    Walsh, Jason M; Ren, Xiaobai; Zampariello, Carly; Polasky, Daniel A; McKay, Diane L; Blumberg, Jeffrey B; Chen, C-Y Oliver

    2016-01-01

    The lack of a biomarker for the consumption of cranberries has confounded the interpretation of several studies investigating the effect of cranberry products, especially juices, on health outcomes. The objectives of this pilot study were to develop a liquid chromatography tandem mass spectrometric method for the quantification of the proanthocyanin dimer A-2 in human urine and validate urinary proanthocyanin dimer A-2 as a biomarker of cranberry intake. Five healthy, nonsmoking, premenopausal women (20-30 years of age, body mass index: 18.5-25 kg/m(2) ) were assigned to consume a cranberry beverage containing 140 mg proanthocyanin and 35 kilocalories at 237 mL/day, according to a weekly dosing schedule for 7 weeks. Eleven 24 h and morning spot urine samples each were collected from each subject. A reliable, sensitive method for the detection of proanthocyanin dimer A-2 in urine using liquid chromatography with tandem mass spectrometry was developed with a limit of quantitation of 0.25 ng/mL and a relative standard deviation of 7.26%, precision of 5.7%, and accuracy of 91.7%. While proanthocyanin dimer A-2 was quantifiable in urine, it did not appear to be excreted in a concentration that corresponded to the dosing schedule and intake of cranberry juice. PMID:26573891

  5. Method for the quantification of vanadyl porphyrins in fractions of crude oils by High Performance Liquid Chromatography-Flow Injection-Inductively Coupled Plasma Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Wandekoken, Flávia G.; Duyck, Christiane B.; Fonseca, Teresa C. O.; Saint'Pierre, Tatiana D.

    2016-05-01

    High performance liquid chromatography hyphenated by flow injection to inductively coupled plasma mass spectrometry (HPLC-FI-ICP-MS) was used to investigate V linked to porphyrins present in fractions of crude oil. First, the crude oil sample was submitted to fractionation by preparative liquid chromatography with UV detection, at the porphyrin Soret band wavelength (400 nm). The obtained porphyrin fractions were then separated in a 250 mm single column, in the HPLC, and eluted with different mobile phases (methanol or methanol:toluene (80:20; v:v)). The quantification of V-porphyrins in the fractions eluted from HPLC was carried out by online measuring the 51V isotope in the ICP-MS, against vanadyl octaethylporphine standard solutions (VO-OEP), prepared in the same solvent as the mobile phase, and injected post-column directly into the plasma. A 20 μg L- 1 Ge in methanol was used as internal standard for minimizing non-spectral interference, such as short-term variations due to injection. The mathematical treatment of the signal based on Fast Fourier Transform smoothing algorithm was employed to improve the precision. The concentrations of V as V-porphyrins were between 2.7 and 11 mg kg- 1 in the fractions, which were close to the total concentration of V in the porphyrin fractions of the studied crude oil.

  6. Quantification of selected synthetic cannabinoids and Δ9-tetrahydrocannabinol in oral fluid by liquid chromatography-tandem mass spectrometry.

    PubMed

    de Castro, Ana; Piñeiro, Beatriz; Lendoiro, Elena; Cruz, Angelines; López-Rivadulla, Manuel

    2013-06-21

    An LC-MS/MS method for the quantification of the synthetic cannabinoids JWH-200, JWH-250, JWH-073, JWH-018, HU-211, CP 47,497 and CP 47,497-C8, and THC in oral fluid was developed and validated. Samples (0.5 mL) were extracted using Strata X cartridges (Phenomenex). Chromatographic separation was achieved with a Sunfire™ IS column (20×2.1 mm, 3.5 μm) (Waters Corp.), with formic acid 0.1% and acetonitrile as mobile phase. A different chromatographic gradient was applied for the separation of the analytes depending on the ionization mode employed, with a total chromatographic run of 14 min. Detection was performed in a Quattro Micro™ API ESCI (Waters Corp.), using electrospray in the positive mode (ESI+) for JWH-200, JWH-250, JWH-073, JWH-018 and THC, and ESI- for HU-211, CP 47,497, and CP 47,497-C8. Validation of the method included the assessment of selectivity, linearity (0.1-2.5 to 200 ng/mL), limits of detection (0.025-1 ng/mL) and quantification (0.1-2.5 ng/mL), imprecision (%CV≤14.4%), accuracy (91.8-109.7% of target concentration), extraction recovery (65.4-105.6%) and Quantisal recovery (56.1-66.7%), and matrix effect (neat oral fluid: -56.0% to 38.5%; oral fluid in Quantisal buffer: -15.1% to -71.7%). The application of this method to oral fluid samples from roadside testing will provide unique information on the use of these new synthetic drugs by Spanish drivers. PMID:23680386

  7. Quantification of 15 bile acids in lake charr feces by ultra-high performance liquid chromatography–tandem mass spectrometry

    USGS Publications Warehouse

    Li, Ke; Buchinger, Tyler J.; Bussy, Ugo; Fissette, Skye D; Johnson, Nicholas; Li, Weiming

    2015-01-01

    Many fishes are hypothesized to use bile acids (BAs) as chemical cues, yet quantification of BAs in biological samples and the required methods remain limited. Here, we present an UHPLC–MS/MS method for simultaneous, sensitive, and rapid quantification of 15 BAs, including free, taurine, and glycine conjugated BAs, and application of the method to fecal samples from lake charr (Salvelinus namaycush). The analytes were separated on a C18 column with acetonitrile–water (containing 7.5 mM ammonium acetate and 0.1% formic acid) as mobile phase at a flow rate of 0.25 mL/min for 12 min. BAs were monitored with a negative electrospray triple quadrupole mass spectrometer (Xevo TQ-S™). Calibration curves of 15 BAs were linear over the concentration range of 1.00–5,000 ng/mL. Validation revealed that the method was specific, accurate, and precise. The method was applied to quantitative analysis of feces extract of fry lake charr and the food they were eating. The concentrations of analytes CA, TCDCA, TCA, and CDCA were 242.3, 81.2, 60.7, and 36.2 ng/mg, respectively. However, other taurine conjugated BAs, TUDCA, TDCA, and THDCA, were not detected in feces of lake charr. Interestingly, TCA and TCDCA were detected at high concentrations in food pellets, at 71.9 and 38.2 ng/mg, respectively. Application of the method to feces samples from lake charr supported a role of BAs as chemical cues, and will enhance further investigation of BAs as chemical cues in other fish species.

  8. Quantification of 11 thyroid hormones and associated metabolites in blood using isotope-dilution liquid chromatography tandem mass spectrometry.

    PubMed

    Hansen, Martin; Luong, Xuan; Sedlak, David L; Helbing, Caren C; Hayes, Tyrone

    2016-08-01

    This paper describes a novel analytical methodology for the simultaneous determination of absolute and total concentrations of 11 native thyroid hormones and associated metabolites, viz. thyroxine (T4), 3,3', 5-triiodothyronine (T3), 3,3', 5'-triiodothyronine (rT3), 3,5-diiodothyronine (3,5-T2), 3,3'- diiodothyronine (3,3'-T2), 3-iodothyronine (T1), thyronine (T0), 3-iodothyronamine (T1AM), tetraiodothyroacetic acid (Tetrac), triiodothyroacetic acid (Triac), and diiodothyroacetic acid (Diac), in 50-μL of plasma or serum. The method was optimized using four isotopic labeled surrogate and internal standards in combination with solid-phase extraction and LC-MS/MS. The methodology was further evaluated using amphibian plasma and serum with matrix-matched calibration applied for quantification. Method detection limits are 3.5 pg T4, 1.5 pg T3, 2.9 pg rT3, 1.7 pg 3,3'-T2, 2.3 pg 3,5-T2, and between 0.3 and 7.5 pg for the remaining six metabolites in 50 μL aliquots of blood sera or plasma. Accuracies and repeatabilities for all analytes were between 88 and 103 % and 1.31 and 17.2 %, respectively. Finally, we applied the method on adult frog (Xenopus laevis) plasma and tadpole (Rana (Lithobates) catesbeiana) serum. We observed up to seven different thyroid hormones and associated metabolites in tadpole serum. This method will enable researchers to improve the assessment of thyroid homeostasis and endocrine disruption in animals and humans. Graphical Abstract Quantification of 11 thyroid hormones and metabolites from 50 μL plasma or serum using protein denaturation in combination with solid-phase extraction followed by LC-MS/MS. PMID:27215639

  9. Identification and Quantification of Glycoproteins Using Ion-Pairing Normal-phase Liquid Chromatography and Mass Spectrometry*

    PubMed Central

    Ding, Wen; Nothaft, Harald; Szymanski, Christine M.; Kelly, John

    2009-01-01

    Glycoprotein structure determination and quantification by MS requires efficient isolation of glycopeptides from a proteolytic digest of complex protein mixtures. Here we describe that the use of acids as ion-pairing reagents in normal-phase chromatography (IP-NPLC) considerably increases the hydrophobicity differences between non-glycopeptides and glycopeptides, thereby resulting in the reproducible isolation of N-linked high mannose type and sialylated glycopeptides from the tryptic digest of a ribonuclease B and fetuin mixture. The elution order of non-glycopeptides relative to glycopeptides in IP-NPLC is predictable by their hydrophobicity values calculated using the Wimley-White water/octanol hydrophobicity scale. O-linked glycopeptides can be efficiently isolated from fetuin tryptic digests using IP-NPLC when N-glycans are first removed with PNGase. IP-NPLC recovers close to 100% of bacterial N-linked glycopeptides modified with non-sialylated heptasaccharides from tryptic digests of periplasmic protein extracts from Campylobacter jejuni 11168 and its pglD mutant. Label-free nano-flow reversed-phase LC-MS is used for quantification of differentially expressed glycopeptides from the C. jejuni wild-type and pglD mutant followed by identification of these glycoproteins using multiple stage tandem MS. This method further confirms the acetyltransferase activity of PglD and demonstrates for the first time that heptasaccharides containing monoacetylated bacillosamine are transferred to proteins in both the wild-type and mutant strains. We believe that IP-NPLC will be a useful tool for quantitative glycoproteomics. PMID:19525481

  10. An ultrasensitive LC-MS/MS method with liquid phase extraction to determine paclitaxel in both cell culture medium and lysate promising quantification of drug nanocarriers release in vitro.

    PubMed

    Baati, Tarek; Schembri, Thérèse; Villard, Claude; Correard, Florian; Braguer, Diane; Estève, Marie-Anne

    2015-11-10

    The quantification of paclitaxel, a chemotherapy drug used to treat different types of cancers, has been performed from complete cell culture medium and cell lysate samples using a simple liquid-liquid extraction procedure in conjunction with liquid chromatography tandem mass spectrometry (LC-MS/MS). A simple sample preparation using methanol and acetic acid as a weaker acid was applied to avoid paclitaxel destruction and to achieve recovery exceeding 80 % from both matrices spiked with paclitaxel and docetaxel used as internal standard. This rapid, simple, selective and sensitive method enabled the quantification of paclitaxel within the linear range of 1-250nM in culture medium and 5-250nM in cell lysate. The lower limit of quantification was achieved in cell culture medium and cell lysates at 0.2 and 1pmol, respectively. This method was successfully applied to human non-small cell lung carcinoma cells (A549 cells) in order to quantify the amount of paclitaxel in both cell culture medium and lysate after incubation with 5, 50 and 100nM of paclitaxel. This ultra-sensitive method promises the quantification of ultra-low concentrations of paclitaxel released from any nanocarriers, allowing the determination of the kinetic profile of drug release, which is an essential parameter to validate the use of nanocarriers for drug delivery in cancer therapy. PMID:26263058

  11. Analysis of free amino acids in fermented shrimp waste by high-performance liquid chromatography.

    PubMed

    López-Cervantes, J; Sánchez-Machado, D I; Rosas-Rodríguez, J A

    2006-02-10

    This work presents an HPLC method for the quantification of free amino acids in lyophilized protein fraction from shrimp waste hydrolysate which is obtained by acid lactic fermentation and analyzed using pre-column derivatization with 9-fluorenylmethyl-chloroformate. The amino acids were separated in a Hypersil ODS 5 microm column (250 mm x 4.6 mm) at 38 degrees C. The mobile phase was a mixture of phase A: 30 mM ammonium phosphate (pH 6.5) in 15:85 (v/v) methanol/water; phase B: 15:85 (v/v) methanol/water; and phase C: 90:10 (v/v) acetonitrile/water, with flow rate 1.2 ml/min. Fluorescence detection was used at an excitation wavelength of 270 nm and an emission wavelength of 316 nm. Method precisions for the different amino acids were between 4.4 and 7.1% (relative standard deviation, RSD); detection limits were between 23 and 72 ng/ml; and the recoveries were between 89.0 and 95.0%. The amino acid present at the highest concentration was tyrosine. PMID:16439254

  12. Sampling and analysis of radioactive liquid wastes and sludges in the Melton Valley and evaporator facility storage tanks at ORNL

    SciTech Connect

    Sears, M.B.; Botts, J.L.; Ceo, R.N.; Ferrada, J.J.; Griest, W.H.; Keller, J.M.; Schenley, R.L.

    1990-09-01

    The sampling and analysis of the radioactive liquid wastes and sludges in the Melton Valley Storage Tanks (MVSTs), as well as two of the evaporator service facility storage tanks at ORNL, are described. Aqueous samples of the supernatant liquid and composite samples of the sludges were analyzed for major constituents, radionuclides, total organic carbon, and metals listed as hazardous under the Resource Conservation and Recovery Act (RCRA). Liquid samples from five tanks and sludge samples from three tanks were analyzed for organic compounds on the Environmental Protection Agency (EPA) Target Compound List. Estimates were made of the inventory of liquid and sludge phases in the tanks. Descriptions of the sampling and analytical activities and tabulations of the results are included. The report provides data in support of the design of the proposed Waste Handling and Packaging Plant, the Liquid Low-Level Waste Solidification Project, and research and development activities (R D) activities in developing waste management alternatives. 7 refs., 8 figs., 16 tabs.

  13. Quantification of Viscosity and Capillary Pressure Anomalies for Polar Liquids in 2D Hydrophilic Nano-Confinements

    NASA Astrophysics Data System (ADS)

    Kelly, S. A.; Torres-Verdin, C.; Balhoff, M.

    2014-12-01

    Interest in liquid and interfacial behavior within nano-confinements spans many disciplines. Geophysical interest originates from a desire to understand flow mechanisms through hydrocarbon-rich nano-porous shale media, especially communication between fractures and the adjacent nano-porous matrix (imbibition). This work investigates the extent of boundary layer nucleation during polar liquid flows in hydrophilic nano-confinements via discrepancies seen in viscosity and capillary pressure from their bulk values. We perform our experiments in two-dimensional nanochannels of varying size and as small as 30 nm x 60 nm in cross section and still obtain visual data with reflected differential interference contrast (DIC) microscopy. The simple geometry of the nanochannels enables the comparison against analytical transport solutions. By designing a nanochannel experiment that allows us to monitor the rate of fluid imbibition and volume loss of a trapped air pocket the liquid is imbibing into, we are able to decouple capillary pressure and viscosity from imbibition data, as well as gain information about gas partitioning at the meniscus interface. Our current experiments are performed with organic solvents within siliceous nanochannels and the results of the decoupling scheme indicate that for rectangular nanochannels with heights of 60 nm and varying widths, effective viscosity is consistently between 4-12 times higher than the bulk value and capillary pressure is around 50% less than the macroscopic Young-Laplace equation prediction. These results equate to the nucleation of wall boundary layers on the order of tens of molecular layers thick. Structured boundary layers have an inherently increased viscosity compared to the liquid bulk value, resulting in a significant reduction in imbibition efficacy. This presence of approximately 15 nm boundary layers in on the threshold of two different theories - thin bimolecular boundary layers and exclusion zones (thick boundary

  14. Development of the SREX process for the treatment of ICPP liquid wastes

    SciTech Connect

    Wood, D.J.; Law, J.D.; Garn, T.G.; Tillotson, R.D.; Tullock, P.A.; Todd, T.A.

    1997-12-01

    The removal of {sup 90}Sr from actual and simulated wastes at the Idaho Chemical Processing Plant (ICPP) at the Idaho National Engineering and Environmental Laboratory (INEEL) has been demonstrated with the SREX process. This solvent extraction process employs the extractant 4{prime},4{prime}(5{prime}) di-(t-butylcyclohexano)-18-crown-6 in 1-octanol or a mixture of tributyl phosphate and a hydrocarbon diluent called Isopar L{reg_sign}. Process flowsheets have been designed for testing in countercurrent experiments with centrifugal contractors. The flowsheets have been designed using batch contract solvent extraction methods. The extraction of Sr as well as other interfering ions has been studied. The effect of various parameters including nitric acid dependence, extractant concentration dependence, hydronium ion concentration, and interferent concentrations upon the extraction efficiency of the process has been evaluated. The radiolysis of the SREX solvent has also been investigated as a function of absorbed gamma radiation. The extraction efficiency of the solvent has been shown to be only slightly dependent upon absorbed dose in the range 0--1,000 kGy. The decontamination of actual sodium-bearing waste and dissolved calcine solutions has been accomplished in batch contact flowsheets. Decontamination factors as high as 10E3 have been obtained with sequential batch contacts. Flowsheets have been developed to accomplish decontamination of the liquid wastes with respect to {sup 90}Sr as well as the removal of Pb and Hg. Pb may be partitioned from the Sr fraction in a separate stripping procedure using ammonium citrate. This work has led to the formulation of countercurrent flowsheets which have been tested in centrifugal contractors with actual waste and reported in the document INEEL/EXT-97-00832.

  15. Development of the SREX Process for the Treatment of ICPP Liquid Wastes

    SciTech Connect

    D. J. Wood; Garn, T. G.; J. D. Law; P. A. Tullock; R. D. Tillotson; T. A. Todd

    1997-10-01

    The removal of Sr-90 from actual and simulated wastes at the Idaho Chemical Processing Plant (ICPP) at the Idaho National Engineering and Environmental Laboratory (INEEL) has been demonstrated with the SREX process. This solvent extraction process employs the extractant 4',4' (5') de-(t-butylcyclohexano)-18-crown-6 in 1-octanol or a mixture of tributyl phosphate and a hydrocarbon diluent called Isopar L. This development work is based upon earlier work performed by Horwitz, et al. at Argonne National Laboratory. Process flowsheets have been designed for testing in countercurrent experiments with centrifugal contactors. The flowsheets have been designed using batch contact solvent extraction methods. The extraction of Sr as well as other interfering ions has been studied. The effect of various parameters including nitric acid dependence, extractant concentration dependence, Hydronium ion concentration, and interferent concentrations upon the extraction efficiency of the process has been evaluated. The radiolysis of the SREX solvent has also been investigated as a function of absorbed gamma radiation. The extraction efficiency of the solvent has been shown to be only slightly dependent upon absorbed dose in the range 0-1000 kGy. The decontamination of actual sodium-bearing waste and dissolved calcine solutions has been accomplished in batch contact flowsheets. Decontamination factors as high as 10E3 have been obtained with sequential batch contacts. Flowsheets have been developed to accomplish decontamination of the liquid wastes with respect to Sr-90, as well as the removal of Pb and Hg. Pb may be partitioned from the Sr fraction in a separate stripping procedure using ammonium citrate. This work has led to the formulation of countercurrent flowsheets which have been tested in centrifugal contactors with actual waste and reported in the document INEEL/EXT-97-00832.

  16. Application of thermogravimetric analysis to study the thermal degradation of solid and liquid organic wastes

    SciTech Connect

    E.S. Lygina; A.F. Dmitruk; S.B. Lyubchik; V.F. Tret'yakov

    2009-07-01

    In this work, the thermolysis of composite binary mixtures of refinery or coal-processing waste with waste biomass and D-grade (long-flame) coal was analyzed in order to increase the efficiency of the cothermolysis of chemically different organic wastes mainly because of the synergism of the thermolysis of mixture components and, correspondingly, the selectivity of formation of high-quality by-products (solid, gaseous, or liquid). A new approach to the analysis of thermogravimetric data was proposed and developed as applied to complex binary mixtures of carbon-containing materials. This approach was based on (1) the preliminary separation of the thermal degradation of individual carbon-containing mixture components into individual structural constituents and (2) the monitoring of the conversion of each particular structure fragment as a constituent of the mixtures in the course of the cothermolysis of the mixtures of starting components. Based on the approach developed, data on the main synergism effects in the course of cothermolysis in the binary test systems were obtained: the temperature regions of the appearance of these effects were distinguished, the main conclusions were made with respect to particular structure fragments in complex organic wastes responsible for the interaction of components in composite systems, and the directions (positive or negative) of changes in the yields of solid by-products and the degrees of effects (difference between the yields of cothermolysis by-products in each particular region of the appearance of synergistic effects in the systems) were determined. Additionally, the influence of alkali metal carbonate additives on synergistic effects in the interaction between binary system components under the process conditions of cothermolysis was analyzed.

  17. Development studies for the treatment of ORNL low-level liquid waste

    SciTech Connect

    Campbell, D.O.; Lee, D.D.; Dillow, T.A.

    1991-11-01

    An experimental program is under way to investigate potential separation methods for application to specific problems relating to the management of low-level liquid wastes (LLLWs) at ORNL. This report summarizes experimental results that were acquired during fiscal year 1990 and have not been previously reported elsewhere. Measurements are presented for cesium and strontium removal from simulated high-salt waste compositions, using both inorganic ion- exchange sorbents and organic ion-exchange resins, and for one experiment with actual LLLW supernate solution from Melton Valley Storage Tank W-26, using inorganic sorbents. The purpose of the study was to acquire an extensive data base to support the development of flowsheets for decontamination of the LLLW currently stored at ORNL. Experimental measurements with inorganic ion exchangers focused on batch separations of cesium using several transition-metal hexacyanoferrate(2) compositions (ferrocyanides) and of strontium using titanium oxide-based sorbents. Cesium distribution coefficients in the range of 1 {times} 10{sup 6} were generally observed with nickel and cobalt ferrocyanides at pH values {le}11, yielding DFs of about 100 with 100 ppm sorbent in a single-stage batch separation. Most organic ion-exchange resins are not very effective for cesium removal from such high salt concentrations, but a new resorcinol-based resin developed at the Savannah River Site was found to be considerably superior to any other such material tested. Several chelating resins were effective for removing strontium from the waste simulants. An ion-exchange column test successfully demonstrated the simultaneous removal of both cesium and strontium from a waste simulant solution.

  18. Quantification of Quercetin and Rutin from Benincasa hispida Seeds and Carissa Congesta Roots by High-performance Thin Layer Chromatography and High-performance Liquid Chromatography

    PubMed Central

    Doshi, Gaurav Mahesh; Une, Hemant Devidas

    2016-01-01

    Objective: In Indian Ayurvedic system, Benincasa hispida (BH) and Carissa congesta (CC) are well-known plants used for major and minor ailments. BH has been regarded as Kushmanda, whereas CC has been used in immune-related disorders of the human system. Quercetin and rutin identified from the vast plethora of plant extracts have proved to possess ethnopharmacological relevance. Materials and Methods: In present studies, we have determined quercetin and rutin in terms of percentage in BH seeds and CC roots by high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC). After extraction and phytochemical screening, the extracts were subjected to quantification for the presence of quercetin and rutin by HPTLC and HPLC. Results: HPTLC showed quercetin as 44.60, 27.13% and rutin as 32.00, 36.31% w/w, whereas HPLC revealed quercetin as 34.00, 35.00% and rutin as 21.99, 45.03% w/v in BH and CC extracts, respectively. Conclusion: The BH and CC extracts have elucidated peaks that were corresponding with standard peaks on undertaking chromatographic studies. SUMMARY Quercetin and rutin are isolated from BH seeds and CC roots by High Performance. Thin Layer Chromatography and High Performance Liquid Chromatography. HPTLC revealed presence of quercetin as 44.60, 27.13 % and rutin as 32.00, 36.31 % w/w. HPLC revealed presence of quercetin as 34.00, 35.00 % and rutin as 21.99, 45.03 % w/v. Abbreviation Used: HPTLC: High Performance Thin Layer Chromatography; HPLC: High Pressure Liquid Chromatography, UV: Ultraviolet, CC: Carissa congesta, BH: Benincasa hispida PMID:26941534

  19. The use of dried blood spots for quantification of 15 antipsychotics and 7 metabolites with ultra-high performance liquid chromatography - tandem mass spectrometry.

    PubMed

    Patteet, Lisbeth; Maudens, Kristof E; Stove, Christophe P; Lambert, Willy E; Morrens, Manuel; Sabbe, Bernard; Neels, Hugo

    2015-06-01

    Therapeutic drug monitoring of antipsychotics is important in optimizing individual therapy. In psychiatric populations, classical venous blood sampling is experienced as frightening. Interest in alternative techniques, like dried blood spots (DBS), has consequently increased. A fast and easy to perform DBS method for quantification of 16 antipsychotics (amisulpride, aripiprazole, asenapine, bromperidol, clozapine, haloperidol, iloperidone, levosulpiride, lurasidone, olanzapine, paliperidone, pipamperone, quetiapine, risperidone, sertindole and zuclopenthixol) and 8 metabolites was developed. DBS were prepared using 25 μL of whole blood and extraction of complete spots was performed using methanol: methyl-t-butyl-ether (4:1). After evaporation, the extract was reconstituted in the mobile phase and 10 μL were injected on an ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Separation using a C18 column and gradient elution with a flow rate of 0.5 mL/min resulted in a 6-min run-time. Ionization was performed in positive mode and a dynamic MRM method was applied. Median recovery was 66.4 % (range 28.7-84.5%). Accuracy was within the acceptance criteria, except for pipamperone (LLOQ and low concentration) and lurasidone (low concentration). Imprecision was only aberrant for lurasidone at low and medium concentration. All compounds were stable during 1 month at room temperature, 4 °C and -18 °C. Lurasidone was unstable when the extract was stored for 12 h on the autosampler. Absolute matrix effects (ME) (median 66.1%) were compensated by the use of deuterated IS (median 98.8%). The DBS method was successfully applied on 25-μL capillary DBS from patients and proved to be a reliable alternative for quantification of all antipsychotics except for olanzapine and N-desmethylolanzapine. PMID:25132670

  20. Development and validation of an in-house quantitative analysis method for cylindrospermopsin using hydrophilic interaction liquid chromatography-tandem mass spectrometry: Quantification demonstrated in 4 aquatic organisms.

    PubMed

    Esterhuizen-Londt, Maranda; Kühn, Sandra; Pflugmacher, Stephan

    2015-12-01

    The cyanobacterial toxin cylindrospermopsin (CYN) is of great concern in aquatic environments because of its incidence, multiple toxicity endpoints, and, therefore, the severity of health implications. It may bioaccumulate in aquatic food webs, resulting in high exposure concentrations to higher-order trophic levels, particularly humans. Because of accumulation at primary levels resulting from exposure to trace amounts of toxin, a sensitive analytical technique with proven aquatic applications is required. In the present study, a hydrophilic interaction liquid chromatographic-tandem mass spectrometric method with a lower limit of detection of 200 fg on column (signal-to-noise ratio = 3, n = 9) and a lower limit of quantification of 1 pg on column (signal-to-noise ratio = 11, n = 9) with demonstrated application in 4 aquatic organisms is described. The analytical method was optimized and validated with a linear range (r(2) = 0.999) from 0.1 ng mL(-1) to 100 ng mL(-1) CYN. Mean recovery of the extraction method was 98 ± 2%. Application of the method was demonstrated by quantifying CYN uptake in Scenedesmus subspicatus (green algae), Egeria densa (Brazilian waterweed), Daphnia magna (water flea), and Lumbriculus variegatus (blackworm) after 24 h of static exposure to 50 μg L(-1) CYN. Uptake ranged from 0.05% to 0.11% of the nominal CYN exposure amount. This constitutes a sensitive and reproducible method for extraction and quantification of unconjugated CYN with demonstrated application in 4 aquatic organisms, which can be used in further aquatic toxicological investigations. PMID:26126753

  1. Simultaneous quantification of crocetin esters and picrocrocin changes in Chinese saffron by high-performance liquid chromatography-diode array detector during 15 years of storage

    PubMed Central

    Tong, Yingpeng; Yan, Yongqiu; Zhu, Xingyi; Liu, Ruoxi; Gong, Feng; Zhang, Ling; Wang, Ping

    2015-01-01

    Background: Saffron, which is made up of the dried stigmas of Crocus sativus L., has been successfully cultivated in China since 1970s and Zhejiang province is now the largest producing area in China, but the contents of crocetin esters and picrocrocin in saffron from Zhejiang province has not been determined simultaneously by high-performance liquid chromatography (HPLC) and changes of these constituents in Chinese saffron during storage for years has not been studied. Object: To establish a simple method quantification of the five main compounds including picrocrocin and four crocetin esters in saffron from main producing areas of China and study the influence of storage time on the changes of saffron constituents. Materials and Methods: A simple, sensitive, and accurate HPLC method was developed for simultaneous determination of five major active components in saffron and eight samples which collected from the same farm of Zhejiang province in different years were analyzed. Results: The correlation coefficient values (R2 > 0.9997) indicated good correlations between the investigated compounds’ concentrations and their peak areas within the test ranges. The limits of quantification and detection of the five compounds were 0.53–2.76 μg/mL and 0.11–0.77 μg/mL, respectively. The recoveries ranged from 94.67% to 101.31%, and the overall relative standard deviations for intra-day and inter-day were lower than 3.49%. The method was applied to study the changes of crocetin esters and picrocrocin contents in saffron samples during 15 years of storage. The losses of crocetin esters and picrocrocin in saffron with 1 -year storage were 52.2% and 54.3%, respectively. The trend then declined during subsequent storage. Conclusion: The developed method can be applied to the intrinsic quality control of saffron. PMID:26246729

  2. Suspect screening and target quantification of multi-class pharmaceuticals in surface water based on large-volume injection liquid chromatography and time-of-flight mass spectrometry.

    PubMed

    Vergeynst, Leendert; Van Langenhove, Herman; Joos, Pieter; Demeestere, Kristof

    2014-04-01

    The ever-growing number of emerging micropollutants such as pharmaceuticals requests rapid and sensitive full-spectrum analytical techniques. Time-of-flight high-resolution mass spectrometry (TOF-HRMS) is a promising alternative for the state-of-the-art tandem mass spectrometry instruments because of its ability to simultaneously screen for a virtually unlimited number of suspect analytes and to perform target quantification. The challenge for such suspect screening is to develop a strategy, which minimizes the false-negative rate without restraining numerous false-positives. At the same time, omitting laborious sample enrichment through large-volume injection ultra-performance liquid chromatography (LVI-UPLC) avoids selective preconcentration. A suspect screening strategy was developed using LVI-UPLC-TOF-MS aiming the detection of 69 multi-class pharmaceuticals in surface water without the a priori availability of analytical standards. As a novel approach, the screening takes into account the signal-intensity-dependent accurate mass error of TOF-MS, hereby restraining 95 % of the measured suspect pharmaceuticals present in surface water. Application on five Belgian river water samples showed the potential of the suspect screening approach, as exemplified by a false-positive rate not higher than 15 % and given that 30 out of 37 restrained suspect compounds were confirmed by the retention time of analytical standards. Subsequently, this paper discusses the validation and applicability of the LVI-UPLC full-spectrum HRMS method for target quantification of the 69 pharmaceuticals in surface water. Analysis of five Belgian river water samples revealed the occurrence of 17 pharmaceuticals in a concentration range of 17 ng L(-1) up to 3.1 μg L(-1). PMID:24633561

  3. Simultaneous quantification of flavonoids in blood plasma by a high-performance liquid chromatography method after oral administration of Blumea balsamifera leaf extracts in rats.

    PubMed

    Nessa, Fazilatun; Ismail, Zhari; Mohamed, Nornisah; Karupiah, Sundram

    2013-03-01

    The leaves of Blumea balsamifera are used as a folk medicine in kidney stone diseases in South-East Asia. Phytochemical investigation revealed leaves contained a number of flavonoids. In view of these, the present work was aimed to quantify and preliminary pharmacokinetic investigation of five flavonoids viz. dihydroquercetin-7,4¢-dimethyl ether (I), dihydroquercetin-4¢-methyl ether (II), 5,7,3¢,5¢-tetrahydroxyflavanone (III), blumeatin (IV) and quercetin (V) in rat plasma following oral administration (0.5g/Kg) of B. balsamifera leaf extract in rats. Quantification was achieved by using a validated, reproducible high-performance liquid chromatographic method. The mean recoveries of I, II, III, IV and V were 90.6, 93.4, 93.5, 91.2 and 90.3% respectively. The limit of quantification was 25 ng/mL for I and IV, 10 ng/mL for II and III and 100 ng/mL for V respectively. The within day and day-to-day precision for all the compounds were < 10%. The validated HPLC method herein was applied for pharmacokinetic studies and the main pharmacokinetic parameters were: t1/2 (hr) 5.8, 4.3, 2.9, 5.7 and 7.3, Cmax (ng/mL) 594.9, 1542.9 1659.9, 208.9 and 3040.4; Tmax (hr) 4.7, 1.0, 1.0, 3.5 and 2.3; AUC0-oo (ng hr/mL) 5040, 5893, 9260, 1064 and 27233 for I, II, III, IV and V respectively. The developed method was suitable for pharmacokinetic studies and this preliminary study also revealed significant absorption after oral dosing in rats. PMID:23455210

  4. An integrated metabolomics workflow for the quantification of sulfur pathway intermediates employing thiol protection with N-ethyl maleimide and hydrophilic interaction liquid chromatography tandem mass spectrometry.

    PubMed

    Ortmayr, Karin; Schwaiger, Michaela; Hann, Stephan; Koellensperger, Gunda

    2015-11-21

    The sulfur metabolic pathway is involved in basic modes of cellular metabolism, including methylation, cell division, respiratory oscillations and stress responses. Hence, the implicated high reactivity of the sulfur pathway intermediates entails challenges for their quantitative analysis. In particular the unwanted oxidation of the thiol group-containing metabolites glutathione, cysteine, homocysteine, γ-glutamyl cysteine and cysteinyl glycine must be prevented in order to obtain accurate snapshots of this important part of cellular metabolism. Suitable analytical methodologies are therefore needed to support studies of drug metabolism and metabolic engineering. In this work, a novel sample preparation strategy targeting thiolic metabolites was established by implementing thiol group protection with N-ethyl maleimide using a cold methanol metabolite extraction procedure. It was shown that N-ethyl maleimide derivatization is compatible with typical metabolite extraction procedures and also allowed for the stabilization of the instable thiolic metabolites in a fully (13)C-labeled yeast cell extract. The stable isotope labeled metabolite analogs could be used for internal standardization to achieve metabolite quantification with high precision. Furthermore, a dedicated hydrophilic interaction liquid chromatography tandem mass spectrometry method for the separation of sulfur metabolic pathway intermediates using a sub-2 μm particle size stationary phase was developed. Coupled with tandem mass spectrometry, the presented methodology proved to be robust, and sensitive (absolute detection limits in the low femtomole range), and allowed for the quantification of cysteine, cysteinyl glycine, cystathionine, cystine, glutamic acid, glutamyl cysteine, reduced glutathione, glutathione disulfide, homocysteine, methionine, S-adenosyl homocysteine and serine in a human ovarian carcinoma cell model. PMID:26451393

  5. Simultaneous quantification of amino acids and Amadori products in foods through ion-pairing liquid chromatography-high-resolution mass spectrometry.

    PubMed

    Troise, Antonio Dario; Fiore, Alberto; Roviello, Giovanni; Monti, Simona Maria; Fogliano, Vincenzo

    2015-01-01

    The formation of the Amadori products (APs) is the first key step of Maillard reaction. Only few papers have dealt with simultaneous quantitation of amino acids and corresponding APs (1-amino-1-deoxy-2-ketose). Chromatographic separation of APs is affected by several drawbacks mainly related to their poor retention in conventional reversed phase separation. In this paper, a method for the simultaneous quantification of amino acids and their respective APs was developed combining high-resolution mass spectrometry with ion-pairing liquid chromatography. The limit of detection was 0.1 ng/mL for tryptophan, valine and arginine, while the limit of quantification ranged from 2 to 5 ng/mL according to the specific sensitivity of each analyte. The relative standard deviation % was lower than 10 % and the coefficient of correlation was higher than 0.99 for each calibration curve. The method was applied to milk, milk-based products, raw and processed tomato. Among the analyzed products, the most abundant amino acid was glutamic acid (16,646.89 ± 1,385.40 µg/g) and the most abundant AP was fructosyl-arginine in tomato puree (774.82 ± 10.01 µg/g). The easiness of sample preparation coupled to the analytical performances of the proposed method introduced the possibility to use the pattern of free amino acids and corresponding APs in the evaluation of the quality of raw food as well as the extent of thermal treatments in different food products. PMID:25323735

  6. Self-aliquoting micro-grooves in combination with laser ablation-ICP-mass spectrometry for the analysis of challenging liquids: quantification of lead in whole blood.

    PubMed

    Nischkauer, Winfried; Vanhaecke, Frank; Limbeck, Andreas

    2016-08-01

    We present a technique for the fast screening of the lead concentration in whole blood samples using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS). The whole blood sample is deposited on a polymeric surface and wiped across a set of micro-grooves previously engraved into the surface. The engraving of the micro-grooves was accomplished with the same laser system used for LA-ICP-MS analysis. In each groove, a part of the liquid blood is trapped, and thus, the sample is divided into sub-aliquots. These aliquots dry quasi instantly and are then investigated by means of LA-ICP-MS. For quantification, external calibration against aqueous standard solutions was relied on, with iron as an internal standard to account for varying volumes of the sample aliquots. The (208)Pb/(57)Fe nuclide ratio used for quantification was obtained via a data treatment protocol so far only used in the context of isotope ratio determination involving transient signals. The method presented here was shown to provide reliable results for Recipe ClinChek® Whole Blood Control levels I-III (nos. 8840-8842), with a repeatability of typically 3 % relative standard deviation (n = 6, for Pb at 442 μg L(-1)). Spiked and non-spiked real whole blood was analysed as well, and the results were compared with those obtained via dilution and sectorfield ICP-MS. A good agreement between both methods was observed. The detection limit (3 s) for lead in whole blood was established to be 10 μg L(-1) for the laser ablation method presented here. Graphical Abstract Micro-grooves are filled with whole blood, dried, and analyzed by laser ablation ICP-mass spectrometry. Notice that the laser moves in perpendicular direction with regard to the micro-grooves. PMID:27363841

  7. Simultaneous quantification of buprenorphine, naloxone and phase I and II metabolites in plasma and breastmilk by liquid chromatography-tandem mass spectrometry.

    PubMed

    Swortwood, Madeleine J; Scheidweiler, Karl B; Barnes, Allan J; Jansson, Lauren M; Huestis, Marilyn A

    2016-05-13

    Opioid abuse during pregnancy is associated with fetal growth restriction, placental abruption, preterm labor, fetal death, and Neonatal Abstinence Syndrome. Current guidelines for medication-assisted opioid addiction treatment during pregnancy are methadone or buprenorphine monotherapy. Buprenorphine/naloxone combination therapy (Suboxone(®)) has not been thoroughly evaluated during pregnancy and insufficient naloxone safety data exist. While methadone- and buprenorphine-treated mothers are encouraged to breastfeed, no studies to date investigated naloxone concentrations during breastfeeding following Suboxone administration. For this reason, we developed and fully validated a liquid chromatography-tandem mass spectrometry method for the simultaneous quantification of buprenorphine, buprenorphine-glucuronide, norbuprenorphine, norbuprenorphine-glucuronide, naloxone, naloxone-glucuronide and naloxone-N-oxide in 100μL human plasma and breastmilk in a single injection following protein precipitation and solid-phase extraction. Lowest limits of quantification were 0.1-2μg/L with 20-100μg/L upper limits of linearity. Bias and imprecision were <±16%. Matrix effects ranged from -57.9 to 11.2 and -84.6 to 29.3% in plasma and breastmilk, respectively. All analytes were stable (within ±20% change from baseline) under all tested conditions (24h room temperature, 72h at 4°C, 3 freeze/thaw cycles at -20°C, and in the autosampler for 72h at 4°C). For proof of concept, buprenorphine and its metabolites were successfully quantified in authentic positive maternal and infant plasma and paired breastmilk specimens. This comprehensive, highly sensitive and specific method detects multiple buprenorphine markers in a small specimen volume. PMID:27083254

  8. Simultaneous quantification of 11 cannabinoids and metabolites in human urine by liquid chromatography tandem mass spectrometry using WAX-S tips.

    PubMed

    Andersson, Maria; Scheidweiler, Karl B; Sempio, Cristina; Barnes, Allan J; Huestis, Marilyn A

    2016-09-01

    A comprehensive cannabinoid urine quantification method may improve clinical and forensic result interpretation and is necessary to support our clinical research. A liquid chromatography tandem mass spectrometry quantification method for ∆(9)-tetrahydrocannabinol (THC), 11-hydroxy-THC (11-OH-THC), 11-nor-9-carboxy-THC (THCCOOH), ∆(9)-tetrahydrocannabinolic acid (THCAA), cannabinol (CBN), cannabidiol (CBD), cannabigerol (CBG), ∆(9)-tetrahydrocannabivarin (THCV), 11-nor-9-carboxy-THCV (THCVCOOH), THC-glucuronide (THC-gluc), and THCCOOH-glucuronide (THCCOOH-gluc) in urine was developed and validated according to the Scientific Working Group on Toxicology guidelines. Sample preparation consisted of disposable pipette extraction (WAX-S) of 200 μL urine. Separation was achieved on a Kinetex C18 column using gradient elution with flow rate 0.5 mL/min, mobile phase A (10 mM ammonium acetate in water), and mobile phase B (15 % methanol in acetonitrile). Total run time was 14 min. Analytes were monitored in both positive and negative ionization modes by scheduled multiple reaction monitoring. Linear ranges were 0.5-100 μg/L for THC and THCCOOH; 0.5-50 μg/L for 11-OH-THC, CBD, CBN, THCAA, and THC-gluc; 1-100 μg/L for CBG, THCV, and THCVCOOH; and 5-500 μg/L for THCCOOH-gluc (R (2) > 0.99). Analytical biases were 88.3-113.7 %, imprecisions 3.3-14.3 %, extraction efficiencies 42.4-81.5 %, and matrix effect -10 to 32.5 %. We developed and validated a comprehensive, simple, and rapid LC-MS/MS cannabinoid urine method for quantification of 11 cannabinoids and metabolites. This method is being used in a controlled cannabis administration study, investigating urine cannabinoid markers documenting recent cannabis use, chronic frequent smoking, or route of drug administration and potentially improving urine cannabinoid result interpretation. PMID:27422645

  9. An improved method for retrospective quantification of sulfur mustard exposure by detection of its albumin adduct using ultra-high pressure liquid chromatography-tandem mass spectrometry.

    PubMed

    Liu, ChangCai; Liang, LongHui; Xiang, Yu; Yu, HuiLan; Zhou, ShiKun; Xi, HaiLing; Liu, ShiLei; Liu, JingQuan

    2015-09-01

    Sulfur mustard (HD) adduct to human serum albumin (ALB) at Cys-34 residue has become an important and long-term retrospective biomarker of HD exposure. Here, a novel, sensitive, and convenient approach for retrospective quantification of HD concentration exposed to plasma was established by detection of the HD-ALB adduct using ultra-high pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) with a novel non-isotope internal standard (IS). The HD-ALB adduct was isolated from HD-exposed plasma with blue Sepharose. The adduct was digested with proteinase K to form sulfur-hydroxyethylthioethyl ([S-HETE])-Cys-Pro-Phe tripeptide biomarker. The tripeptide adduct could be directly analyzed by UHPLC-MS/MS without an additional solid phase extraction (SPE), which was considered as a critical procedure in previous methods. The easily available 2-chloroethyl ethylsulfide (2-CEES) as HD surrogate was first reported to be used as IS in place of traditional d8-HD for quantification of HD exposure. Furthermore, 2-CEES was also confirmed to be a good IS alternative for quantification of HD exposure by investigation of product ion spectra for their corresponding tripeptide adducts which exhibited identical MS/MS fragmentation behaviors. The method was found to be linear between 1.00 and 250 ng•mL(-1) HD exposure (R(2)>0.9989) with precision of <4.50% relative standard deviation (%RSD), accuracy range between 96.5% and 114%, and a calculated limit of detection (LOD) of 0.532 ng•mL(-1). The lowest reportable limit (LRL) is 1.00 ng•mL(-1), over seven times lower than that of the previous method. The entire method required only 0.1 mL of plasma sample and took under 7 h without special sample preparation equipment. It is proven to be a sensitive, simple, and rugged method, which is easily applied in international laboratories to improve the capabilities for the analysis of biomedical samples related to verification of the Chemical Weapon Convention (CWC). PMID

  10. Quantification of urinary uric acid in the presence of thymol and thimerosal by high-performance liquid chromatography

    NASA Technical Reports Server (NTRS)

    Chen, Y.; Pietrzyk, R. A.; Whitson, P. A.

    1997-01-01

    A high-performance liquid chromatographic method was developed as an alternative to automated enzymatic analysis of uric acid in human urine preserved with thymol and/or thimerosal. Uric acid (tR = 10 min) and creatinine (tR = 5 min) were separated and quantified during isocratic elution (0.025 M acetate buffer, pH 4.5) from a mu Bondapak C18 column. The uric-acid peak was identified chemically by incubating urine samples with uricase. The thymol/thimerosal peak appeared at 31 min during the washing step and did not interfere with the analysis. We validated the high-performance liquid chromatographic method for linearity, precision and accuracy, and the results were found to be excellent.

  11. Identification and quantification of cannabinoids in Cannabis sativa L. plants by high performance liquid chromatography-mass spectrometry.

    PubMed

    Aizpurua-Olaizola, Oier; Omar, Jone; Navarro, Patricia; Olivares, Maitane; Etxebarria, Nestor; Usobiaga, Aresatz

    2014-11-01

    High performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) has been successfully applied to cannabis plant extracts in order to identify cannabinoid compounds after their quantitative isolation by means of supercritical fluid extraction (SFE). MS conditions were optimized by means of a central composite design (CCD) approach, and the analysis method was fully validated. Six major cannabinoids [tetrahydrocannabinolic acid (THCA), tetrahydrocannabinol (THC), cannabidiol (CBD), tetrahydrocannabivarin (THCV), cannabigerol (CBG), and cannabinol (CBN)] were quantified (RSD < 10%), and seven more cannabinoids were identified and verified by means of a liquid chromatograph coupled to a quadrupole-time-of-flight (Q-ToF) detector. Finally, based on the distribution of the analyzed cannabinoids in 30 Cannabis sativa L. plant varieties and the principal component analysis (PCA) of the resulting data, a clear difference was observed between outdoor and indoor grown plants, which was attributed to a higher concentration of THC, CBN, and CBD in outdoor grown plants. PMID:25338935

  12. Quantification of Fatty Acid Oxidation Products Using On-line High Performance Liquid Chromatography Tandem Mass Spectrometry

    PubMed Central

    Levison, Bruce S.; Zhang, Renliang; Wang, Zeneng; Fu, Xiaoming; DiDonato, Joseph A.; Hazen, Stanley L.

    2013-01-01

    Oxidized fatty acids formed via lipid peroxidation are implicated in pathological processes such as inflammation and atherosclerosis. A number of methods may be used to detect specific oxidized fatty acids containing a single or multiple combinations of epoxide, hydroxyl, ketone and hydroperoxide moieties on varying carbon chain lengths from C8 up to C30. Some of these methods are nonspecific and their use in biological systems is fraught with difficulty. Measures of specific-oxidized fatty acid derivatives help in identifying oxidation pathways in pathological processes. We used liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-MS/MS) as efficient, selective and sensitive methods for identifying and analyzing multiple specific fatty acid peroxidation products in human plasma and other biological matrices. We then distilled the essential components of a number of these analyses to provide an efficient protocol by which fatty acid oxidation products and their parent compounds can be determined. In this protocol, addition of synthetic internal standard to the sample, followed by base hydrolysis at elevated temperature, and liquid-liquid phase sample extraction with lighter than water solvents facilitates isolation of the oxidized fatty acid species. These species can be identified and accurately quantified using stable isotope dilution and multiple reaction monitoring. Use of a coupled multiplexed gradient HPLC system on the front end enables high-throughput chromatography and more efficient use of mass spectrometer time. PMID:23499838

  13. Surfactant-based ionic liquids for extraction of phenolic compounds combined with rapid quantification using capillary electrophoresis.

    PubMed

    Huang, Fangzhi; Berton, Paula; Lu, Chengfei; Siraj, Noureen; Wang, Chun; Magut, Paul K S; Warner, Isiah M

    2014-09-01

    A rapid liquid phase extraction employing a novel hydrophobic surfactant-based room temperature ionic liquid (RTIL), tetrabutylphosphonium dioctyl sulfosuccinate ([4C4 P][AOT]), coupled with capillary electrophoretic-UV (CE-UV) detection is developed for removal and determination of phenolic compounds. The long-carbon-chain RTIL used is sparingly soluble in most solvents and can be used to replace volatile organic solvents. This fact, in combination with functional-surfactant-anions, is proposed to reduce the interfacial energy of the two immiscible liquid phases, resulting in highly efficient extraction of analytes. Several parameters that influence the extraction efficiencies, such as extraction time, RTIL type, pH value, and ionic strength of aqueous solutions, were investigated. It was found that, under acidic conditions, most of the investigated phenols were extracted from aqueous solution into the RTIL phase within 12 min. Good linearity was observed over the concentration range of 0.1-80.0 μg/mL for all phenols investigated. The precision of this method, expressed as RSD, was determined to be within 3.4-5.3% range. The LODs (S/N = 3) of the method were in the range of 0.047-0.257 μg/mL. The proposed methodology was successfully applied to determination of phenols in real water samples. PMID:24798689

  14. Quantification of L-ergothioneine in whole blood by hydrophilic interaction ultra-performance liquid chromatography and UV-detection.

    PubMed

    Sotgia, Salvatore; Zinellu, Angelo; Pintus, Gianfranco; Pinna, Gerard Aime; Deiana, Luca; Carru, Ciriaco

    2013-03-01

    A new hydrophilic interaction ultra-performance LC method was established for the whole blood measurement of L-ergothioneine. Chromatographic separation was achieved in a fairly short time, less than 4 min, on a 100 × 2.1 mm Acquity UPLC BEH HILIC 1.7 μm column with a mobile phase consisting of a mixture of 100 mmol/L ammonium acetate/ACN/water (5:85:10, v/v/v) that flowed isocratically at 0.250 mL/min. The LOD and the limit of quantification were 3.85 and 11.67 μmol/L, respectively. The method exhibited linearity in a concentration range of 15.63-1000 μmol/L (R(2) > 0.999). Mean recovery was 96.34% whereas intraassay and interassay precision were 1.52 and 1.82% RSD, respectively. On the whole, the developed method is simple, fast, precise, accurate, and sensitive and may be useful for routine analyses. PMID:23418129

  15. Simultaneous quantification of nicotine, opioids, cocaine, and metabolites in human fetal postmortem brain by liquid chromatography tandem mass spectrometry

    PubMed Central

    Shakleya, Diaa M.

    2011-01-01

    A validated method for simultaneous LCMSMS quantification of nicotine, cocaine, 6-acetylmorphine (6AM), codeine, and metabolites in 100 mg fetal human brain was developed and validated. After homogenization and solid-phase extraction, analytes were resolved on a Hydro-RP analytical column with gradient elution. Empirically determined linearity was from 5–5,000 pg/mg for cocaine and benzoylecgonine (BE), 25–5,000 pg/mg for cotinine, ecgonine methyl ester (EME) and 6AM, 50–5000 pg/mg for trans-3-hydroxycotinine (OH-cotinine) and codeine, and 250–5,000 pg/mg for nicotine. Potential endogenous and exogenous interferences were resolved. Intra- and inter-assay analytical recoveries were ≥92%, intra- and inter-day and total assay imprecision were ≤14% RSD and extraction efficiencies were ≥67.2% with ≤83% matrix effect. Method applicability was demonstrated with a postmortem fetal brain containing 40 pg/mg cotinine, 65 pg/mg OH-cotinine, 13 pg/mg cocaine, 34 pg/mg EME, and 525 pg/mg BE. This validated method is useful for determination of nicotine, opioid, and cocaine biomarkers in brain. PMID:19229524

  16. Quantification of greenhouse gas emissions from waste management processes for municipalities - A comparative review focusing on Africa

    SciTech Connect

    Friedrich, Elena; Trois, Cristina

    2011-07-15

    The amount of greenhouse gases (GHG) emitted due to waste management in the cities of developing countries is predicted to rise considerably in the near future; however, these countries have a series of problems in accounting and reporting these gases. Some of these problems are related to the status quo of waste management in the developing world and some to the lack of a coherent framework for accounting and reporting of greenhouse gases from waste at municipal level. This review summarizes and compares GHG emissions from individual waste management processes which make up a municipal waste management system, with an emphasis on developing countries and, in particular, Africa. It should be seen as a first step towards developing a more holistic GHG accounting model for municipalities. The comparison between these emissions from developed and developing countries at process level, reveals that there is agreement on the magnitude of the emissions expected from each process (generation of waste, collection and transport, disposal and recycling). The highest GHG savings are achieved through recycling, and these savings would be even higher in developing countries which rely on coal for energy production (e.g. South Africa, India and China) and where non-motorized collection and transport is used. The highest emissions are due to the methane released by dumpsites and landfills, and these emissions are predicted to increase significantly, unless more of the methane is captured and either flared or used for energy generation. The clean development mechanism (CDM) projects implemented in the developing world have made some progress in this field; however, African countries lag behind.

  17. Quantification of greenhouse gas emissions from waste management processes for municipalities--a comparative review focusing on Africa.

    PubMed

    Friedrich, Elena; Trois, Cristina

    2011-07-01

    The amount of greenhouse gases (GHG) emitted due to waste management in the cities of developing countries is predicted to rise considerably in the near future; however, these countries have a series of problems in accounting and reporting these gases. Some of these problems are related to the status quo of waste management in the developing world and some to the lack of a coherent framework for accounting and reporting of greenhouse gases from waste at municipal level. This review summarizes and compares GHG emissions from individual waste management processes which make up a municipal waste management system, with an emphasis on developing countries and, in particular, Africa. It should be seen as a first step towards developing a more holistic GHG accounting model for municipalities. The comparison between these emissions from developed and developing countries at process level, reveals that there is agreement on the magnitude of the emissions expected from each process (generation of waste, collection and transport, disposal and recycling). The highest GHG savings are achieved through recycling, and these savings would be even higher in developing countries which rely on coal for energy production (e.g. South Africa, India and China) and where non-motorized collection and transport is used. The highest emissions are due to the methane released by dumpsites and landfills, and these emissions are predicted to increase significantly, unless more of the methane is captured and either flared or used for energy generation. The clean development mechanism (CDM) projects implemented in the developing world have made some progress in this field; however, African countries lag behind. PMID:21450453

  18. Combustion of liquid paint wastes in fluidized bed boiler as element of waste management system in the paint factory

    SciTech Connect

    Soko, W.A.; Biaecka, B.

    1998-12-31

    In this paper the solution to waste problems in the paint industry is presented by describing their combustion in a fluidized bed boiler as a part of the waste management system in the paint factory. Based on the Cleaner Production idea and concept of integration of design process with a future exploitation of equipment, some modifications of the waste management scheme in the factory are discussed to reduce the quantity of toxic wastes. To verify this concept combustion tests of paint production wastes and cocombustion of paint wastes with coal in an adopted industrial boiler were done. Results of these tests are presented in the paper.

  19. Solidification/stabilisation of liquid oil waste in metakaolin-based geopolymer

    NASA Astrophysics Data System (ADS)

    Cantarel, V.; Nouaille, F.; Rooses, A.; Lambertin, D.; Poulesquen, A.; Frizon, F.

    2015-09-01

    The solidification/stabilisation of liquid oil waste in metakaolin based geopolymer was studied in the present work. The process consists of obtaining a stabilised emulsion of oil in a water-glass solution and then adding metakaolin to engage the setting of a geopolymer block with an oil emulsion stabilised in the material. Geopolymer/oil composites have been made with various oil fraction (7, 14 and 20 vol.%). The rigidity and the good mechanical properties have been demonstrated with compressive strength tests. Leaching tests evidenced the release of oil from the composite material is very limited whereas the constitutive components of the geopolymer (Na, Si and OH-) are involved into diffusion process.

  20. Laboratory development of methods for centralized treatment of liquid low-level waste at Oak Ridge National Laboratory

    SciTech Connect

    Arnold, W.D.; Bostick, D.T.; Burgess, M.W.; Taylor, P.A.; Perona, J.J.; Kent, T.E.

    1994-10-01

    Improved centralized treatment methods are needed in the management of liquid low-level waste (LLLW) at Oak Ridge National Laboratory (ORNL). LLLW, which usually contains radioactive contaminants at concentrations up to millicurie-per-liter levels, has accumulated in underground storage tanks for over 10 years and has reached a volume of over 350,000 gal. These wastes have been collected since 1984 and are a complex mixture of wastes from past nuclear energy research activities. The waste is a highly alkaline 4-5 M NaNO{sub 3} solution with smaller amounts of other salts. This type of waste will continue to be generated as a consequence of future ORNL research programs. Future LLLW (referred to as newly generated LLLW or NGLLLW) is expected to a highly alkaline solution of sodium carbonate and sodium hydroxide with a smaller concentration of sodium nitrate. New treatment facilities are needed to improve the manner in which these wastes are managed. These facilities must be capable of separating and reducing the volume of radioactive contaminants to small stable waste forms. Treated liquids must meet criteria for either discharge to the environment or solidification for onsite disposal. Laboratory testing was performed using simulated waste solutions prepared using the available characterization information as a basis. Testing was conducted to evaluate various methods for selective removal of the major contaminants. The major contaminants requiring removal from Melton Valley Storage Tank liquids are {sup 90}Sr and {sup 137}Cs. Principal contaminants in NGLLLW are {sup 9O}Sr, {sup 137}Cs, and {sup 106}Ru. Strontium removal testing began with literature studies and scoping tests with several ion-exchange materials and sorbents.

  1. Development of Advanced Electrochemical Emission Spectroscopy for Monitoring Corrosion in Simulated DOE Liquid Waste

    SciTech Connect

    Digby Macdonald; Brian Marx; Balaji Soundararajan; Morgan Smith

    2005-07-28

    The different tasks that have been carried out under the current program are as follows: (1) Theoretical and experimental assessment of general corrosion of iron/steel in borate buffer solutions by using electrochemical impedance spectroscopy (EIS), ellipsometry and XPS techniques; (2) Development of a damage function analysis (DFA), which would help in predicting the accumulation of damage due to pitting corrosion in an environment prototypical of DOE liquid waste systems; (3) Experimental measurement of crack growth rate, acoustic emission signals, and coupling currents for fracture in carbon and low alloy steels as functions of mechanical (stress intensity), chemical (conductivity), electrochemical (corrosion potential, ECP), and microstructural (grain size, precipitate size, etc) variables in a systematic manner, with particular attention being focused on the structure of the noise in the current and its correlation with the acoustic emissions; (4) Development of fracture mechanisms for carbon and low alloy steels that are consistent with the crack growth rate, coupling current data and acoustic emissions; (5) Inserting advanced crack growth rate models for SCC into existing deterministic codes for predicting the evolution of corrosion damage in DOE liquid waste storage tanks; (6) Computer simulation of the anodic and cathodic activity on the surface of the steel samples in order to exactly predict the corrosion mechanisms; (7) Wavelet analysis of EC noise data from steel samples undergoing corrosion in an environment similar to that of the high level waste storage containers, to extract data pertaining to general, pitting and stress corrosion processes, from the overall data. The work has yielded a number of important findings, including an unequivocal demonstration of the role of chloride ion in passivity breakdown on nickel in terms of cation vacancy generation within the passive film, the first detection and characterization of individual micro fracture

  2. Best available technology for the Los Alamos National Laboratory Radioactive Liquid Waste Treatment Facility

    SciTech Connect

    Midkiff, W.S.; Romero, R.L.; Suazo, I.L.; Garcia, R.; Parsons, R.M.

    1993-10-15

    The existing Los Alamos National Laboratory TA-50 liquid radioactive waste treatment plant RLWP has been in service for over thirty years, during this period many technical, regulatory, and processing changes have occurred. The existing facility can no longer comply with the demands and requirements for continued operation, and would not be able to comply with anticipated stringent future contaminant discharge limitations. Either a major upgrading or replacement of the existing facility is required. In order to assess the most appropriate means of providing an adequate facility to comply with predicted requirements for Ta-50, this Best Available Technology (BAT) Study was conducted to compare feasible technical and economic alternatives in order to define the most favorable technology configuration. This report consists of eleven sections. Section 1 provides a general introduction and background of the TA-50 operations and the basis for this study. Section 2 provides a technical discussion of the unit processes at TA-50 and several other comparable operations at other DOE sites. Section 3 addresses the evaluation and selection of appropriate treatment processes. Section 4 provides an analysis of environmental issues and concerns. Section 5 presents the rationale for the selection of preferred process configurations. Section 6 is the evaluation of operational issues. Section 7 addresses energy and resource use topics. Section 8 provides an economic analysis, and Section 9 summarizes the evaluation and the identification of the BAT. These sections are augmented by appendices. The report identifies the construction of a new radioactive liquid waste treatment facility as the BAT. Based on the information analyzed for this study, this option appears to provide the best combination of environmental compliance, operability, and economic value.

  3. 30 CFR 250.248 - What solid and liquid wastes and discharges information and cooling water intake information must...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... information and cooling water intake information must accompany the DPP or DOCD? 250.248 Section 250.248... and discharges information and cooling water intake information must accompany the DPP or DOCD? The following solid and liquid wastes and discharges information and cooling water intake information...

  4. 40 CFR 63.1217 - What are the standards for liquid fuel boilers that burn hazardous waste?

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 12 2012-07-01 2011-07-01 true What are the standards for liquid fuel boilers that burn hazardous waste? 63.1217 Section 63.1217 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS FOR SOURCE CATEGORIES National...

  5. 30 CFR 550.217 - What solid and liquid wastes and discharges information and cooling water intake information must...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 30 Mineral Resources 2 2013-07-01 2013-07-01 false What solid and liquid wastes and discharges information and cooling water intake information must accompany the EP? 550.217 Section 550.217 Mineral Resources BUREAU OF OCEAN ENERGY MANAGEMENT, DEPARTMENT OF THE INTERIOR OFFSHORE OIL AND GAS AND SULPHUR OPERATIONS IN THE OUTER CONTINENTAL...

  6. 30 CFR 550.248 - What solid and liquid wastes and discharges information and cooling water intake information must...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 30 Mineral Resources 2 2013-07-01 2013-07-01 false What solid and liquid wastes and discharges information and cooling water intake information must accompany the DPP or DOCD? 550.248 Section 550.248 Mineral Resources BUREAU OF OCEAN ENERGY MANAGEMENT, DEPARTMENT OF THE INTERIOR OFFSHORE OIL AND GAS AND SULPHUR OPERATIONS IN THE OUTER...

  7. 30 CFR 550.248 - What solid and liquid wastes and discharges information and cooling water intake information must...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 30 Mineral Resources 2 2014-07-01 2014-07-01 false What solid and liquid wastes and discharges information and cooling water intake information must accompany the DPP or DOCD? 550.248 Section 550.248 Mineral Resources BUREAU OF OCEAN ENERGY MANAGEMENT, DEPARTMENT OF THE INTERIOR OFFSHORE OIL AND GAS AND SULPHUR OPERATIONS IN THE OUTER...

  8. 30 CFR 550.217 - What solid and liquid wastes and discharges information and cooling water intake information must...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 30 Mineral Resources 2 2014-07-01 2014-07-01 false What solid and liquid wastes and discharges information and cooling water intake information must accompany the EP? 550.217 Section 550.217 Mineral Resources BUREAU OF OCEAN ENERGY MANAGEMENT, DEPARTMENT OF THE INTERIOR OFFSHORE OIL AND GAS AND SULPHUR OPERATIONS IN THE OUTER CONTINENTAL...

  9. Differential Isotope Labeling of 38 Dietary Polyphenols and Their Quantification in Urine by Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry.

    PubMed

    Achaintre, David; Buleté, Audrey; Cren-Olivé, Cécile; Li, Liang; Rinaldi, Sabina; Scalbert, Augustin

    2016-03-01

    A large number of polyphenols are consumed with the diet and may contribute to the prevention of chronic diseases such as cardiovascular diseases, diabetes, cancers, and neurodegenerative diseases. More comprehensive methods are needed to measure exposure to this complex family of bioactive plant compounds in epidemiological studies. We report here a novel method enabling the simultaneous measurement in urine of 38 polyphenols representative of the main classes and subclasses found in the diet. This method is based on differential (12)C-/(13)C-isotope labeling of polyphenols through derivatization with isotopic dansyl chloride reagents and on the analysis of the labeled polyphenols by tandem mass spectrometry. This derivatization approach overcomes the need for costly labeled standards. Different conditions for enzyme hydrolysis of polyphenol glucuronides and sulfate esters, extraction, and dansylation of unconjugated aglycones were tested and optimized. Limits of quantification varied from 0.01 to 1.1 μM depending on polyphenols. Intrabatch coefficients of variation varied between 3.9% and 9.6%. Interbatch variations were lower than 15% for 31 compounds and lower than 29% for 6 additional polyphenols out of the 38 tested. Thirty seven polyphenols were validated and then analyzed in 475, 24 h urine samples from the European Prospective Investigation on Cancer and Nutrition (EPIC) study. Thirty four polyphenols could be detected and successfully estimated and showed large interindividual variations of concentrations (2-3 orders of magnitude depending on the compound), with median concentrations spanning from 0.01 to over 1000 μM for all 34 compounds. PMID:26814424

  10. Mechanisms contributing to the thermal analysis of waste incineration bottom ash and quantification of different carbon species.

    PubMed

    Rocca, Stefania; van Zomeren, André; Costa, Giulia; Dijkstra, Joris J; Comans, Rob N J; Lombardi, Francesco

    2013-02-01

    The focus of this study was to identify the main compounds affecting the weight changes of bottom ash (BA) in conventional loss on ignition (LOI) tests and to obtain a better understanding of the individual processes in heterogeneous (waste) materials such as BA. Evaluations were performed on BA samples from a refuse derived fuel incineration (RDF-I) plant and a hospital waste incineration (HW-I) plant using thermogravimetric analysis and subsequent mass spectrometry (TG-MS) analysis of the gaseous thermal decomposition products. Results of TG-MS analysis on RDF-I BA indicated that the LOI measured at 550°C was due to moisture evaporation and dehydration of Ca(OH)(2) and hydrocalumite. Results for the HW-I BA showed that LOI at 550°C was predominantly related to the elemental carbon (EC) content of the sample. Decomposition of CaCO(3) around 700°C was identified in both materials. In addition, we have identified reaction mechanisms that underestimate the EC and overestimate the CaCO(3) contents of the HW-I BA during TG-MS analyses. These types of artefacts are expected to occur also when conventional LOI methods are adopted, in particular for materials that contain CaO/Ca(OH)(2) in combination with EC and/or organic carbon, such as e.g. municipal solid waste incineration (MSWI) bottom and fly ashes. We suggest that the same mechanisms that we have found (i.e. in situ carbonation) can also occur during combustion of the waste in the incinerator (between 450 and 650°C) demonstrating that the presence of carbonate in bottom ash is not necessarily indicative for weathering. These results may also give direction to further optimization of waste incineration technologies with regard to stimulating in situ carbonation during incineration and subsequent potential improvement of the leaching behavior of bottom ash. PMID:23246084

  11. Utilization of natural hematite as reactive barrier for immobilization of radionuclides from radioactive liquid waste.

    PubMed

    El Afifi, E M; Attallah, M F; Borai, E H

    2016-01-01

    Potential utilization of hematite as a natural material for immobilization of long-lived radionuclides from radioactive liquid waste was investigated. Hematite ore has been characterized by different analytical tools such as Fourier transformer infrared (FTIR), X-ray fluorescence (XRF), powder X-ray diffraction (XRD), thermogravimetry (TG) and differential thermal (DT) analysis, scanning electron microscopy (SEM) and BET-surface area. In this study, europium was used as REEs(III) and as a homolog of Am(III)-isotopes (such as (241)Am of 432.6 y, (242m)Am of 141 y and (243)Am of 7370 y). Micro particles of the hematite ore were used for treatment of radioactive waste containing (152+154)Eu(III). The results indicated that 96% (4.1 × 10(4) Bq) of (152+154)Eu(III) was efficiently retained onto hematite ore. Kinetic experiments indicated that the processes could be simulated by a pseudo-second-order model and suggested that the process may be chemisorption in nature. The applicability of Langmuir, Freundlich and Temkin models was investigated. It was found that Langmuir isotherm exhibited the best fit with the experimental results. It can be concluded that hematite is an economic and efficient reactive barrier for immobilization of long-lived radio isotopes of actinides and REEs(III). PMID:26465672

  12. Conditioning of Boron-Containing Low and Intermediate Level Liquid Radioactive Waste - 12041

    SciTech Connect

    Gorbunova, Olga A.; Kamaeva, Tatiana S.

    2012-07-01

    Improved cementation of low and intermediate level radioactive waste (ILW and LLW) aided by vortex electromagnetic treatment as well as silica addition was investigated. Positive effects including accelerated curing of boron-containing cement waste forms, improve end product quality, decreased product volume and reduced secondary LRW volume from equipment decontamination were established. These results established the possibility of boron-containing LRW cementation without the use of neutralizing alkaline additives that greatly increase the volume of the final product intended for long-term storage (burial). Physical (electromagnetic) treatment in a vortex mixer can change the state of LRW versus chemical treatment. By treating the liquid phase of cement solution only, instead of the whole solution, and using fine powder and nano-particles of ferric oxides instead of separable ferromagnetic cores for the activating agents the positive effect are obtained. VET for 1 to 3 minutes yields boron-containing LRW cemented products of satisfactory quality. Silica addition at 10 % by weight will accelerate curing and solidification and to decrease radionuclide leaching rates from boron-containing cement products. (authors)

  13. Pore solution chemistry of simulated low-level liquid waste incorporated in cement grouts

    SciTech Connect

    Kruger, A.A.

    1995-12-01

    Expressed pore solutions from simulated low level liquid waste cement grouts cured at room temperature, 50{degree}C and 90{degree}C for various duration were analyzed by standard chemical methods and ion chromatography. The solid portions of the grouts were formulated with portland cement, fly ash, slag, and attapulgite clay in the ratios of 3:3:3:1. Two different solutions simulating off-gas condensates expected from vitrification of Hanford low level tank wastes were made. One is highly alkaline and contains the species Na{sup {plus}}, P0{sub 4}{sup 3-}, N0{sub 2}{sup -}, NO{sub 3}{sup -} and OH{sup -}. The other is carbonated and contains the species, Na{sup {plus}}, PO{sub 4}{sup 3-}, NO{sub 2}{sup -}, NO{sub 3}{sup -}, and CO{sub 3}{sup 2-}. In both cases phosphate rapidly disappeared from the pore solution, leaving behind sodium in the form of hydroxide. The carbonates were also removed from the pore solution to form calcium carbonate and possibly calcium monocarboaluminate. These reactions resulted in the increase of hydroxide ion concentration in the early period. Subsequently there was a significant reduction OH{sup -} and Na{sup {plus}} ion concentrations. In contrast high concentration of N0{sub 2}{sup -} and N0{sub 3}{sup -} were retained in the pore solution indefinitely.

  14. Technoeconomic analysis for the destruction of toxic liquid wastes using induction plasma technology

    SciTech Connect

    Soucy, G.; Bergeron, E.; Boulos, M.I.

    1995-12-31

    During the past decade, thermal plasma technology has been pointed out as one of the most promising innovative technologies for the thermal destruction of hazardous wastes and for this role, it has been supported by the EPA. In this field, many process alternatives have been developed but insufficient attention have been given to the details of their economic viability. The objective of this paper is to carry out an economic analysis of a particular thermal induction plasma technology for toxic liquid waste destruction. This work is presented in three parts. The first part presents a description of the conceptual design for a process using high frequency (HF) induction plasma. The second part, based on an order-of-magnitude factored estimate, provides an analysis of the capital investment cost of this process. The third part presents an estimation of the operating costs and a discounted cash flow analysis of this conceptual project using a HF plasma generator. The analysis of the economic viability is discussed with reference to the net present worth and the internal rate of return. The discussion examines those variables that significantly affect the viability of such technology by exploring its advantages towards minimizing impacts on the global environment and economic situation. Finally, a comparison is drawn up between the induction plasma technology and other alternative competitive processes.

  15. Digital simulation of the regional effects of subsurface injection of liquid waste near Pensacola, Florida

    USGS Publications Warehouse

    Merritt, M.L.

    1984-01-01

    Industrial, organic, liquid waste has been injected into a part of the lower limestone of the Floridan aquifer at one site since 1963 and at another site since 1975, raising water levels in the injection zone throughout a large region. The hydrogeologic conceptual model of the injection zone is a layer tightly confined above by a thick layer of clay and in which lateral hydraulic conductivity decreases rapidly below the upper 60 feet. Recharge areas are to the north and east, where the confining layer pinches out. There appear to be permeability barriers to the northwest, west, and southwest due to facies changes, faults, or pinchouts. Measured and reconstructed preinjection water levels suggested that flow in the aquifer is from the northern recharge areas toward the southeast. A steady-state model simulation incorporating the cited boundary assumptions approximately simulated this pattern. A two-dimensional flow model and the subsurface waste injection program (SWIP) were calibrated to simulate the water level increases at various monitor wells since 1963. Sensitivity analyses showed the simulations to be quite sensitive to moderate errors in either transmissivity or storage parameter specifications. The predictive use of the hydraulic model is understood to be restricted to the geographical locations of data used for model calibration. (USGS)

  16. Characterization and monitoring of 300 Area facility liquid waste streams: 1994 Annual report

    SciTech Connect

    Riley, R.G.; Ballinger, M.Y.; Damberg, E.G.; Evans, J.C.; Julya, J.L.; Olsen, K.B.; Ozanich, R.M.; Thompson, C.J.; Vogel, H.R.

    1995-04-01

    This report summarizes the results of characterizing and monitoring the following sources during calendar year 1994: liquid waste streams from Buildings 306, 320, 324, 326, 331, and 3720 in the 300 Area of Hanford Site and managed by the Pacific Northwest Laboratory; treated and untreated Columbia River water (influent); and water at the confluence of the waste streams (that is, end-of-pipe). Data were collected from March to December before the sampling system installation was completed. Data from this initial part of the program are considered tentative. Samples collected were analyzed for chemicals, radioactivity, and general parameters. In general, the concentrations of chemical and radiological constituents and parameters in building wastewaters which were sampled and analyzed during CY 1994 were similar to historical data. Exceptions were the occasional observances of high concentrations of chloride, nitrate, and sodium that are believed to be associated with excursions that were occurring when the samples were collected. Occasional observances of high concentrations of a few solvents also appeared to be associated with infrequent building r eases. During calendar year 1994, nitrate, aluminum, copper, lead, zinc, bis(2-ethylhexyl) phthalate, and gross beta exceeded US Environmental Protection Agency maximum contaminant levels.

  17. Selective extraction and recovery of rare earth metals from phosphor powders in waste fluorescent lamps using an ionic liquid system.

    PubMed

    Yang, Fan; Kubota, Fukiko; Baba, Yuzo; Kamiya, Noriho; Goto, Masahiro

    2013-06-15

    The recycling of rare earth metals from phosphor powders in waste fluorescent lamps by solvent extraction using ionic liquids was studied. Acid leaching of rare earth metals from the waste phosphor powder was examined first. Yttrium (Y) and europium (Eu) dissolved readily in the acid solution; however, the leaching of other rare earth metals required substantial energy input. Ionization of target rare earth metals from the waste phosphor powders into the leach solution was critical for their successful recovery. As a high temperature was required for the complete leaching of all rare earth metals, ionic liquids, for which vapor pressure is negligible, were used as an alternative extracting phase to the conventional organic diluent. An extractant, N, N-dioctyldiglycol amic acid (DODGAA), which was recently developed, showed a high affinity for rare earth metal ions in liquid-liquid extraction although a conventional commercial phosphonic extractant did not. An effective recovery of the rare earth metals, Y, Eu, La and Ce, from the metal impurities, Fe, Al and Zn, was achieved from the acidic leach solution of phosphor powders using an ionic liquid containing DODGAA as novel extractant system. PMID:23587931

  18. Potential for land application of contaminated sewage sludge treated with fermented liquid from pineapple wastes.

    PubMed

    Del Mundo Dacera, Dominica; Babel, Sandhya; Parkpian, Preeda

    2009-08-15

    The suitability for land application of anaerobically digested sewage sludge treated with naturally fermented and Aspergillus niger (A. niger) fermented raw liquid from pineapple wastes, in terms of changes in the forms and amount of heavy metals and nutrient and pathogen content, were investigated in this study. Leaching studies for fermented liquid at optimum conditions (pH and contact time with best metal removal efficiencies) were carried out for the removal of Cd, Cr, Cu, Pb, Ni and Zn from sewage sludge, with citric acid as a reference. Using the same sludge before and after leaching, sequential fractionation studies were done to observe the effect of treatment on the forms of metals in sludge and their mobility and bioavailability. Results of laboratory scale studies revealed that leaching with all extractants at selected optimum conditions resulted in a decrease in heavy metals and pathogen content of the treated sludge, presence of sufficient amount of nutrients (nitrogen and phosphorous) and dominance of residual fractions in most metals, with sludge treated with A. niger, having the best quality. The results, therefore, indicate the high potential of the treated sludge for land application, with no harm from heavy metals released and no toxicity to the soil and groundwater. PMID:19232826

  19. The thermoelectrochemistry of lithium-glyme solvate ionic liquids: towards waste heat harvesting.

    PubMed

    Black, Jeffrey J; Murphy, Thomas; Atkin, Rob; Dolan, Andrew; Aldous, Leigh

    2016-07-27

    Thermoelectrochemistry offers a simple, scalable technique for direct conversion of waste heat into useful electricity. Here the thermoelectrochemical properties of lithium-glyme solvate ionic liquids, as well as their dilute electrolyte analogues, have been investigated using mixtures of tetraglyme (G4, tetraethylene glycol dimethyl ether) and lithium bis(trifluoromethylsulfonyl)imide (Li[NTf2]). The thermoelectrochemical process is entropically-driven by release of the glyme from the lithium-glyme complex cation, due to electrodeposition of lithium metal at the hotter lithium electrode with concomitant electrodissolution at the cooler lithium electrode. The optimum ratio for thermochemical electricity generation is not the solvate ionic liquid (equimolar mixture of Li[NTf2] and glyme), but rather one Li[NTf2] to four G4, due to the mixtures relatively high ionic conductivity and good apparent Seebeck coefficient (+1.4 mV K(-1)). Determination of the lithium-glyme mixture thermal conductivity enabled full assessment of the Figure of Merit (ZT), and the efficiency relative to the Carnot efficiency to be determined. As the lithium electrodeposits are porous, alternating the temperature gradient results in a system that actually improves with repeated use. PMID:27412130

  20. Comparative study on copper leaching from waste printed circuit boards by typical ionic liquid acids.

    PubMed

    Chen, Mengjun; Huang, Jinxiu; Ogunseitan, Oladele A; Zhu, Nengming; Wang, Yan-min

    2015-07-01

    Waste printed circuit boards (WPCBs) are attracting increasing concerns because the recovery of its content of valuable metallic resources is hampered by the presence of hazardous substances. In this study, we used ionic liquids (IL) to leach copper from WPCBs. [BSO3HPy]OTf, [BSO3HMIm]OTf, [BSO4HPy]HSO4, [BSO4HMim]HSO4 and [MIm]HSO4 were selected. Factors that affect copper leaching rate were investigated in detail and their leaching kinetics were also examined with the comparison of [Bmim]HSO4. The results showed that all six IL acids could successfully leach copper out, with near 100% recovery. WPCB particle size and leaching time had similar influences on copper leaching performance, while IL acid concentration, hydrogen peroxide addition, solid to liquid ratio, temperature, showed different influences. Moreover, IL acid with HSO4(-) was more efficient than IL acid with CF3SO3(-). These six IL acids indicate a similar behavior with common inorganic acids, except temperature since copper leaching rate of some IL acids decreases with its increase. The results of leaching kinetics studies showed that diffusion plays a more important role than surface reaction, whereas copper leaching by inorganic acids is usually controlled by surface reaction. This innovation provides a new option for recovering valuable materials such as copper from WPCBs. PMID:25869844

  1. Kinetic study of hydrolysis of xylan and agricultural wastes with hot liquid water.

    PubMed

    Zhuang, Xinshu; Yuan, Zhenhong; Ma, Longlong; Wu, Chuangzhi; Xu, Mingzhong; Xu, Jingliang; Zhu, Shunni; Qi, Wei

    2009-01-01

    We investigated the kinetics of hot liquid water (HLW) hydrolysis over a 60-min period using a self-designed setup. The reaction was performed within the range 160-220 degrees C, under reaction conditions of 4.0 MPa, a 1:20 solid:liquid ratio (g/mL), at 500 rpm stirring speed. Xylan was chosen as a model compound for hemicelluloses, and two kinds of agricultural wastes-rice straw and palm shell-were used as typical feedstocks representative of herbaceous and woody biomasses, respectively. The hydrolysis reactions for the three kinds of materials followed a first-order sequential kinetic model, and the hydrolysis activation energies were 65.58 kJ/mol for xylan, 68.76 kJ/mol for rice straw, and 95.19 kJ/mol for palm shell. The activation energies of sugar degradation were 147.21 kJ/mol for xylan, 47.08 kJ/mol for rice straw and 79.74 kJ/mol for palm shell. These differences may be due to differences in the composition and construction of the three kinds of materials. In order to reduce the decomposition of sugars, the hydrolysis time of biomasses such as rice straw and palm shell should be strictly controlled. PMID:19397989

  2. Pyrolysis mechanism for recycle renewable resource from polarizing film of waste liquid crystal display panels.

    PubMed

    Wang, Ruixue; Xu, Zhenming

    2014-08-15

    Liquid crystal display (LCD) panels mainly consist of polarizing film, liquid crystal and glass substrates. In this study, a novel pyrolysis model and a pyrolysis mechanism to recover the reusable resource from polarizing film of waste LCD panels was proposed. Polarizing film and its major components, such as cellulose triacetate (TAC) and polyvinyl alcohol (PVA) were pyrolyzed, respectively, to model the pyrolysis process. The pyrolysis process mainly generated a large ratio of oil, a few gases and a little residue. Acetic acid was the main oil product and could be easily recycled. The pyrolysis mechanism could be summarized as follows: (i) TAC, the main component of polarizing film, was heated and generated active TAC with a low polymerization, and then decomposed into triacetyl-d-glucose. (ii) Some triacetyl-d-glucose generated triacetyl-d-mannosan and its isomers through an intramolecular dehydration, while most triacetyl-d-glucose generated the main oil product, namely acetic acid, through a six-member cyclic transition state. (iii) Meanwhile, other products formed through a series of bond cleavage, dehydration, dehydrogenation, interesterification and Diels-Alder cycloaddition. This study could contribute significantly to understanding the polarizing film pyrolysis performance and serve as guidance for the future technological parameters control of the pyrolysis process. PMID:24992456

  3. Quantification of branched-chain keto acids in tissue by ultra fast liquid chromatography-mass spectrometry.

    PubMed

    Olson, Kristine C; Chen, Gang; Lynch, Christopher J

    2013-08-15

    Branched-chain keto acids (BCKAs) are associated with increased susceptibility to several degenerative diseases. However, BCKA concentrations in tissues or the amounts of tissue available are frequently at the limit of detection for standard plasma methods. To accurately and quickly determine tissue BCKAs, we have developed a sensitive ultra fast liquid chromatography-mass spectrometry (UFLC-MS) method. BCKAs from deproteinized tissue extractions were o-phenylenediamine (OPD) derivatized, ethyl acetate extracted, lyophilized in a vacuum centrifuge, and reconstituted in 200 mM ammonium acetate. Samples were injected onto a Shimadzu UFLC system coupled to an AB-Sciex 5600 Triple TOF mass spectrometer instrument that detected masses of the OPD BCKA products using a multiple reaction monitoring method. An OPD-derivatized (13)C-labeled keto acid was used as an internal standard. Application of the method for C57BL/6J (wild-type) and PP2Cm knockout mouse tissues, including kidney, adipose tissue, liver, gastrocnemius, and hypothalamus, is shown. The lowest tissue concentration measured by this method was 20 nM, with the standard curve covering a wide range (7.8-32,000 nM). Liquid chromatography-mass spectrometry run times for this assay were less than 5 min, facilitating high throughput, and the OPD derivatives were found to be stable over several days. PMID:23684523

  4. Cryogenic Coring and Magnetic Resonance Imaging for Quantification of Non-Aqueous Phase Liquids in Unconsolidated Soils

    NASA Astrophysics Data System (ADS)

    Kiaalhosseini, S.; Sale, T. C.; Watson, A. T.; Kohn, B. D.; Johnson, R. L.; Blotevogel, J.

    2014-12-01

    A novel approach of combining cryogenic coring of sediments with magnetic resonance imaging (MRI) of frozen soil cores is reported. Cryogenic coring has the potential to preserve critical properties of soil cores including the distribution of pore fluids. MRI can provide information on the qualitative and quantitative spatial distribution of non-aqueous phase liquid (NAPL) contaminants within the cores. Initial results of field-scale cryogenic coring indicated that injecting liquid nitrogen through a cooling coil around a soil core (6.3 cm diameter and 75 cm long) could freeze the core below the water table (water table at 7.2 m) in less than 15 minutes. MRI scanning of soil cores contaminated with trichloroethene (TCE) NAPL indicated that keeping the cores frozen at -20°C can suppress the competing MRI signals of water-bound hydrogen. Comparison of known and measured TCE NAPL saturation using MRI in spiked frozen soil samples showed close agreement. The results confirm the ability of cryogenic coring to prevent redistribution of pore fluids during sample withdrawal and storage. The results of MRI illustrate the ability of this method to discriminate between water and TCE in frozen cores, thus allowing for a sensitive spatial analysis of contaminant distribution. Overall, this novel combined approach has the potential to lower the cost of site investigation while providing an improved basis for site characterization and management.

  5. High-throughput wide dynamic range procedure for the simultaneous quantification of nicotine and cotinine in multiple biological matrices using hydrophilic interaction liquid chromatography-tandem mass spectrometry.

    PubMed

    Pérez-Ortuño, Raúl; Martínez-Sánchez, Jose M; Fernández, Esteve; Pascual, José A

    2015-11-01

    A straightforward, high-throughput method was developed and fully validated for the simultaneous determination of the specific tobacco biomarkers nicotine and its main metabolite cotinine in a wide dynamic range and supporting the most common human biological matrices (urine, oral fluid and hair). Sample preparation was performed inside the very HPLC injection vials by pipetting 0.5 mL of the liquid samples, deuterated internal standards in alkaline solution and dichloromethane as extraction solvent. Solid samples (i.e. around 10 mg hair) were first submitted to alkaline digestion in the HPLC vials and processed accordingly. The organic phase (reached through the upper aqueous layer) was directly injected without further treatment. Instrumental analysis was performed using hydrophilic interaction (HILIC) ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). Total chromatographic time was 2 min. The method covers a wide dynamic range making it fit-for-purpose for the analysis of samples covering entire populations, irrespective of the level of exposure or tobacco use. Calibration curves (r (2) > 0.995) covered the range 1-2000 ng/mL (or 0.05-100 ng/mg hair) for nicotine and 0.1-2000 ng/mL (or 0.005-100 ng/mg hair) for cotinine. Within-run and between-run precision and accuracy were typically below 10 %, and always below 20 % at the lower limit of quantification. The method was successfully applied to the analysis of samples from different projects involving multiple matrices. PMID:26342312

  6. Simultaneous extraction and quantification of albendazole and triclabendazole using vortex-assisted hollow-fiber liquid-phase microextraction combined with high-performance liquid chromatography.

    PubMed

    Asadi, Mohammad; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh

    2016-06-01

    A novel, simple, and rapid vortex-assisted hollow-fiber liquid-phase microextraction method was developed for the simultaneous extraction of albendazole and triclabendazole from various matrices before their determination by high-performance liquid chromatography with fluorescence detection. Several factors influencing the microextraction efficiency including sample pH, nature and volume of extraction solvent, ionic strength, vortex time, and sample volume were investigated and optimized. Under the optimal conditions, the limits of detection were 0.08 and 0.12 μg/L for albendazole and triclabendazole, respectively. The calibration curves were linear in the concentration ranges of 0.3-50.0 and 0.4-50.0 μg/L with the coefficients of determination of 0.9999 and 0.9995 for albendazole and triclabendazole, respectively. The interday and intraday relative standard deviations for albendazole and triclabendazole at three concentration levels (1.0, 10.0, and 30.0 μg/L) were in the range of 6.0-11.0 and 5.0-7.9%, respectively. The developed method was successfully applied to determine albendazole and triclabendazole in water, milk, honey, and urine samples. PMID:27079953

  7. A liquid chromatography tandem mass spectrometry method for the simultaneous quantification of 20 drugs of abuse and metabolites in human meconium

    PubMed Central

    Gray, Teresa R.; Shakleya, Diaa M.

    2011-01-01

    A method for the simultaneous quantification of 20 cocaine, amphetamine, opiate, and nicotine analytes in meconium, the first neonatal feces, by liquid chromatography tandem mass spectrometry was developed and validated. Specimen preparation included methanol homogenization and solid phase extraction. Two injections were required to achieve sufficient sensitivity and linear dynamic range. Linearity ranged from 0.5–25 up to 500 ng/g (250 ng/g p-hydroxymethamphetamine), and correlation coefficients were >0.996. Imprecision was <10.0% CV, analytical recovery 85.5–123.1%, and extraction efficiencies >46.7% at three concentrations across the linear range. Despite significant matrix effects of −305.7–40.7%, effects were similar for native and deuterated analytes. No carryover, endogenous or exogenous interferences were observed, with analyte stability at room temperature, 4 °C, and −20 °C and on the autosampler >70%, except for 6-acetylmorphine, hydrocodone, oxycodone, and morphine. Method applicability was demonstrated by analyzing meconium from drug-exposed neonates. PMID:19241063

  8. Absolute quantification of Pru av 2 in sweet cherry fruit by liquid chromatography/tandem mass spectrometry with the use of a stable isotope-labelled peptide.

    PubMed

    Ippoushi, Katsunari; Sasanuma, Motoe; Oike, Hideaki; Kobori, Masuko; Maeda-Yamamoto, Mari

    2016-08-01

    Pru av 2, a pathogenesis-related (PR) protein present in the sweet cherry (Prunus avium L.) fruit, is the principal allergen of cherry and one of the chief causes of pollen food syndrome (oral allergy syndrome). In this study, a quantitative assay for this protein was developed with the use of the protein absolute quantification (AQUA) method, which consists of liquid chromatography/tandem mass spectrometry (LC/MS/MS) employing TGC[CAM]STDASGK[(13)C6,(15)N2], a stable isotope-labelled internal standard (SIIS) peptide. This assay gave a linear relationship (r(2)>0.99) in a concentration range (2.3-600fmol/μL), and the overall coefficient of variation (CV) for multiple tests was 14.6%. Thus, the contents of this allergenic protein in sweet cherry products could be determined using this assay. This assay should be valuable for allergological investigations of Pru av 2 in sweet cherry and detection of protein contamination in foods. PMID:26988485

  9. Sensitive and rapid analytical method for the quantification of glucosamine in human plasma by ultra high performance liquid chromatography with tandem mass spectrometry.

    PubMed

    Yang, Wen; Zheng, Xiaohong; Simpemba, Ernest; Ma, Pengcheng; Ding, Li

    2015-06-01

    A highly sensitive and rapid ultra high performance liquid chromatography with tandem mass spectrometry method has been developed and validated for the determination of glucosamine in human plasma using miglitol as the internal standard. Special attention was paid to achieve the high throughput and sensitivity of the established method, and the absence of a matrix effect on the analytes. The sample preparation procedure involved a simple deproteinization step. The chromatographic separation was achieved on a Waters ACQUITY HSS Cyano column using a mixture of acetonitrile/2 mM ammonium acetate solution containing 0.03% formic acid (80:20, v/v) as the mobile phase with a very short run time of 1.5 min. This method was validated over the concentration range of 10-3000 ng/mL for glucosamine. The intra- and inter-batch precision was <13.9% for the low, medium, and high quality control samples. The established method is highly sensitive with a lower limit of quantification of 10 ng/mL, low enough to determine the circadian rhythm on endogenous glucosamine level in human plasma, which has not been reported in detail until now. The method was successfully applied to characterize the pharmacokinetic profile of glucosamine in healthy volunteers following a single oral administration of 750 or 1500 mg glucosamine hydrochloride. PMID:25802209

  10. A chemometric approach toward the detection and quantification of coffee adulteration by solid-phase microextraction using polymeric ionic liquid sorbent coatings.

    PubMed

    Toledo, Bruna R; Hantao, Leandro W; Ho, Tien D; Augusto, Fabio; Anderson, Jared L

    2014-06-13

    Solid-phase microextraction (SPME) using cross-linked polymeric ionic liquid (PIL)-based sorbent coatings was used to extract volatile aroma-related compounds from coffee samples. Several PIL-based coatings were screened alongside a commercial poly(acrylate) (PA) SPME coating. The best performing PIL-based SPME fiber, poly(1-vinyl-3-hexadecylimidazolium bis[(trifluoromethyl)sulfonylimide]) with 50% (w/w) 1,12-di(3-vinylbenzylimidazolium)dodecane dibis[(trifluoromethyl)sulfonyl]imide incorporated cross-linker, was used to isolate the volatile fraction of Arabica coffee. To illustrate the importance of trace analyte isolation, a method for the detection and quantification of coffee adulteration is described. Chromatographic profiles obtained by gas chromatography/mass spectrometry (GC/MS) were used to create the chemometric model. Partial least squares (PLS) regression was employed to correlate the aroma-related chemical fingerprint to the degree of adulteration. The proposed method successfully detected fraud down to 1% (w/w) of adulterant and accurately determined the degree of coffee adulteration (i.e, root mean square error of calibration and prediction of 0.54% and 0.83% (w/w), respectively). Finally, important aroma-related compounds including furans, methoxyphenols, pyrazines, and ketones were identified. PMID:24786655

  11. Liquid chromatography with high resolution mass spectrometry for identification of organic contaminants in fish fillet: screening and quantification assessment using two scan modes for data acquisition.

    PubMed

    Munaretto, Juliana S; May, Marília M; Saibt, Nathália; Zanella, Renato

    2016-07-22

    This study proposed a strategy to identify and quantify 182 organic contaminants from different chemical classes, as for instance pesticides, veterinary drug and personal care products, in fish fillet using liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (LC-QToF/MS). For this purpose, two different scan methods (full scan and all ions MS/MS) were evaluated to assess the best option for screening analysis in spiked fish fillet samples. In general, full scan acquisition was found to be more reliable (84%) in the automatic identification and quantification when compared to all ions MS/MS with 72% of the compounds detected. Additionally, a qualitative automatic search showed a mass accuracy error below 5ppm for 77% of the compounds in full scan mode compared to only 52% in all ions MS/MS scan. However, all ions MS/MS provides fragmentation information of the target compounds. Undoubtedly, structural information of a wide number of compounds can be obtained using high resolution mass spectrometry (HRMS), but it is necessary thoroughly assess it, in order to choose the best scan mode. PMID:27324622

  12. Characterization and quantification of histidine degradation in therapeutic protein formulations by size exclusion-hydrophilic interaction two dimensional-liquid chromatography with stable-isotope labeling mass spectrometry.

    PubMed

    Wang, Chunlei; Chen, Sike; Brailsford, John A; Yamniuk, Aaron P; Tymiak, Adrienne A; Zhang, Yingru

    2015-12-24

    Two dimensional liquid chromatography (2D-LC) coupling size exclusion (SEC) and hydrophilic interaction chromatography (HILIC) is demonstrated as a useful tool to study polar excipients, such as histidine and its degradant, in protein formulation samples. The SEC-HILIC setup successfully removed interferences from complex sample matrices and enabled accurate mass measurement of the histidine degradation product, which was then determined to be trans-urocanic acid. Because the SEC effluent is a strong solvent for the second dimension HILIC, experimental parameters needed to be carefully chosen, i.e., small transferring loop, fast gradient at high flow rates for the second dimension gradient, in order to mitigate the solvent mismatch and to ensure good peak shapes for HILIC separations. In addition, the generation of trans-urocanic acid was quantified by single heart-cutting SEC-HILIC 2D-LC combined with stable-isotope labeling mass spectrometry. Compared with existing 2D quantification methods, the proposed approach is fast, insensitive to solvent mismatch between dimensions, and tolerant of small retention time shifts in the first dimension. Finally, the first dimension diode array detector was found to be a potential degradation source for photolabile analytes such as trans-urocanic acid. PMID:26674608

  13. Identification and quantification of psychoactive drugs in whole blood using dried blood spot (DBS) by ultra-performance liquid chromatography tandem mass spectrometry.

    PubMed

    Kyriakou, Chrystalla; Marchei, Emilia; Scaravelli, Giulia; García-Algar, Oscar; Supervía, August; Graziano, Silvia

    2016-09-01

    A procedure based on ultra-high-pressure liquid chromatography tandem mass spectrometry has been developed for the determination of twenty three psychoactive drugs and metabolites in whole blood using dried blood spot (DBS). Chromatographic separation was achieved at ambient temperature using a reverse-phase column and a linear gradient elution with two solvents: 0.1% formic acid in acetonitrile and 5mM ammonium formate at pH 3. The mass spectrometer was operated in positive ion mode, using multiple reaction monitoring via positive electro-spray ionization. The method was linear from the limit of quantification (5ng/ml for all the analytes apart from 15ng/ml for Δ-9-tetrahydrocannabinol and metabolites) to 500ng/ml, and showed good correlation coefficients (r(2)=0.990) for all substances. Analytical recovery of analytes under investigation was always higher than 75% and intra-assay and inter-assay precision and accuracy always better than 15%. Using the validated method, ten DBS samples, collected at the hospital emergency department in cases of acute drug intoxication, were found positive to one or more psychoactive drugs. Our data support the potential of DBS sampling for non invasive monitoring of exposure/intoxication to psychoactive drugs. PMID:27232151

  14. Combination of precolumn nitro-reduction and ultraperformance liquid chromatography with fluorescence detection for the sensitive quantification of 1-nitronaphthalene, 2-nitrofluorene, and 1-nitropyrene in meat products.

    PubMed

    Deng, Kailin; Wong, Tin-Yan; Wang, Yinan; Leung, Elvis M K; Chan, Wan

    2015-04-01

    Carcinogenic nitropolycyclic aromatic hydrocarbons (nitro-PAHs) are ubiquitous in the ambient environment. They are emitted predominantly from internal combustion engines and by reacting polycyclic aromatic hydrocarbons with nitrogen oxide. The emerging evidence that nitro-PAHs are taken up by plants and bioaccumulatd in the food chain has aroused worldwide concerns for the potential of chronic poisoning through dietary intake. Therefore, analytical methods of high sensitivity are extremely important for assessing the risk of human exposure to nitro-PAHs. This paper describes the development of a simple and robust ultraperformance liquid chromatography coupled fluorescence detector (UPLC-FLD) method for the sensitive determination of nitro-PAHs in meat products. The method entails precolumn reduction of the otherwise nonfluorescent nitro-PAHs to amino-PAHs which strongly fluoresce for their determination by UPLC-FLD analysis. The developed method was validated for extraction efficiency, accuracy, precision, and detection limit and has been successfully applied in quantifying 1-nitronaphthalene (1-NN), 2-nitrofluorene (2-NF), and 1-nitropyrene (1-NP) in fresh and cured meat products. The results showed that the combination of Fe/H(+)-induced nitro-reduction and UPLC-FLD analysis allows sensitive quantification of 1-NN, 2-NF, and 1-NP at detection limits of 0.59, 0.51, and 0.31 μg/kg, respectively, which is at least 10 times lower than those of the existing analytical methods. PMID:25763600

  15. A green method for the quantification of plastics-derived endocrine disruptors in beverages by chemometrics-assisted liquid chromatography with simultaneous diode array and fluorescent detection.

    PubMed

    Vidal, Rocío B Pellegrino; Ibañez, Gabriela A; Escandar, Graciela M

    2016-10-01

    The aim of this study was to develop a novel analytical method for the determination of bisphenol A, nonylphenol, octylphenol, diethyl phthalate, dibutyl phthalate and diethylhexyl phthalate, compounds known for their endocrine-disruptor properties, based on liquid chromatography with simultaneous diode array and fluorescent detection. Following the principles of green analytical chemistry, solvent consumption and chromatographic run time were minimized. To deal with the resulting incomplete resolution in the chromatograms, a second-order calibration was proposed. Second-order data (elution time-absorbance wavelength and elution time-fluorescence emission wavelength matrices) were obtained and processed by multivariate curve resolution-alternating least-squares (MCR-ALS). Applying MCR-ALS allowed quantification of the analytes even in the presence of partially overlapped chromatographic and spectral bands among these compounds and the potential interferents. The obtained results from the analysis of beer, wine, soda, juice, water and distilled beverage samples were compared with gas chromatography-mass spectrometry (GC-MS). Limits of detection (LODs) in the range 0.04-0.38ngmL(-1) were estimated in real samples after a very simple solid-phase extraction. All the samples were found to contain at least three EDs, in concentrations as high as 334ngmL(-1). PMID:27474316

  16. Development of a liquid chromatographic method for the quantification of paromomycin. Application to in vitro release and ex vivo permeation studies

    NASA Astrophysics Data System (ADS)

    Pujol-Brugués, A.; Calpena-Campmany, A. C.; Riera-Lizandra, C.; Halbaut-Bellowa, L.; Clares-Naveros, B.

    2014-12-01

    We have developed a reversed phase high performance liquid chromatography pulsed amperometric detection (RPHPLC-PAD) method for the determination of paromomycin. It is sensitive, repeatable, and selective without the pretreatment step. Trifluoroacetic acid-water was utilized as the eluent and detected by PAD under NaOH alkaline conditions. The paromomycin detection limit (S/N = 3.3) was 2 μg mL-1 and the quantification limit (S/N = 10) was 6 μg mL-1. Coefficients of linear regression were higher than 0.99 for concentrations between 6.25 and 200 μg mL-1. The intra and inter-day precision (RSD) was less than 6.5%. The average recoveries were 97.53-102.01%. The proposed HPLC-PAD method presented advantageous performance characteristics and it can be considered suitable for the evaluation of paromomycin loaded nanogel formulation in ex vivo permeation and in vitro release studies.

  17. Quantification of bovine β-casein allergen in baked foodstuffs based on ultra-performance liquid chromatography with tandem mass spectrometry

    PubMed Central

    Chen, Qi; Zhang, Jingshun; Ke, Xing; Lai, Shiyun; Tao, Baohua; Yang, Jinchuan; Mo, Weimin; Ren, Yiping

    2015-01-01

    The quantification of allergens in food including baked food matrices is of great interest. The aim of the present study was to describe a non-immunologic method to quantify bovine β-casein using ultra-performance liquid chromatography tandem triple quadrupole mass spectrometry (UPLC-TQ-MS/MS) in multiple reaction monitoring (MRM) mode. Eight of 10 theoretical peptides from β-casein after tryptic digestion were compared and MRM methods were developed to determine five signature peptides. The peptide VLPVPQK was selected as the signature peptide for bovine β-casein because of the high sensitivity. A stable isotope-labelled internal standard was designed to adjust the instability of sample pre-treatment and ionisation caused by matrix effect. Using the present suspension digestion method, the native and denatured β-casein could be digested to release the signature peptide at the maximum extent. The UPLC-TQ-MS/MS method developed based on a tryptic signature peptide led to a reliable determination of bovine β-casein allergen in baked food matrices at a low quantitation level down to 500 μg kg–1 with a satisfactory accuracy (< 8.9%) and recovery (98.8% ± 2.6% to 106.7% ± 3.0%). PMID:25413212

  18. Simple and fast quantification of nitisone (NTBC) using liquid chromatography-tandem mass spectrometry method in plasma of tyrosinemia type 1 patients.

    PubMed

    Davit-Spraul, Anne; Romdhane, H