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Sample records for environmental samples analytical

  1. Development of analytical techniques for safeguards environmental samples at JAEA

    International Nuclear Information System (INIS)

    Sakurai, Satoshi; Magara, Masaaki; Usuda, Shigekazu; Watanabe, Kazuo; Esaka, Fumitaka; Hirayama, Fumio; Lee, Chi-Gyu; Yasuda, Kenichiro; Inagawa, Jun; Suzuki, Daisuke; Iguchi, Kazunari; Kokubu, Yoko S.; Miyamoto, Yutaka; Ohzu, Akira

    2007-01-01

    JAEA has been developing, under the auspices of the Ministry of Education, Culture, Sports, Science and Technology of Japan, analytical techniques for ultra-trace amounts of nuclear materials in environmental samples in order to contribute to the strengthened safeguards system. Development of essential techniques for bulk and particle analysis, as well as screening, of the environmental swipe samples has been established as ultra-trace analytical methods of uranium and plutonium. In January 2003, JAEA was qualified, including its quality control system, as a member of the JAEA network analytical laboratories for environmental samples. Since 2004, JAEA has conducted the analysis of domestic and the IAEA samples, through which JAEA's analytical capability has been verified and improved. In parallel, advanced techniques have been developed in order to expand the applicability to the samples of various elemental composition and impurities and to improve analytical accuracy and efficiency. This paper summarizes the trace of the technical development in environmental sample analysis at JAEA, and refers to recent trends of research and development in this field. (author)

  2. Analytical Methodology for the Determination of Radium Isotopes in Environmental Samples

    International Nuclear Information System (INIS)

    2010-01-01

    Reliable, comparable and 'fit for purpose' results are an essential requirement for any decision based on analytical measurements. For the analyst, the availability of tested and validated analytical procedures is an extremely important tool for production of such analytical measurements. For maximum utility, such procedures should be comprehensive, clearly formulated, and readily available to both the analyst and the customer for reference. Since 2004, the environment programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. Measurements of radium isotopes are important for radiological and environmental protection, geochemical and geochronological investigations, hydrology, etc. The suite of isotopes creates and stimulates continuing interest in the development of new methods for determination of radium in various media. In this publication, the four most routinely used analytical methods for radium determination in biological and environmental samples, i.e. alpha spectrometry, gamma spectrometry, liquid scintillation spectrometry and mass spectrometry, are reviewed

  3. Determination of 237Np in environmental and nuclear samples: A review of the analytical method

    International Nuclear Information System (INIS)

    Thakur, P.; Mulholland, G.P.

    2012-01-01

    A number of analytical methods has been developed and used for the determination of neptunium in environmental and nuclear fuel samples using alpha, ICP–MS spectrometry, and other analytical techniques. This review summarizes and discusses development of the radiochemical procedures for separation of neptunium (Np), since the beginning of the nuclear industry, followed by a more detailed discussion on recent trends in the separation of neptunium. This article also highlights the progress in analytical methods and issues associated with the determination of neptunium in environmental samples. - Highlights: ► Determination of Np in environmental and nuclear samples is reviewed. ► Various analytical methods used for the determination of Np are listed. ► Progress and issues associated with the determination of Np are discussed.

  4. Nuclear analytical techniques and their application to environmental samples

    International Nuclear Information System (INIS)

    Lieser, K.H.

    1986-01-01

    A survey is given on nuclear analytical techniques and their application to environmental samples. Measurement of the inherent radioactivity of elements or radionuclides allows determination of natural radioelements (e.g. Ra), man-made radioelements (e.g. Pu) and radionuclides in the environment. Activation analysis, in particular instrumental neutron activation analysis, is a very reliable and sensitive method for determination of a great number of trace elements in environmental samples, because the most abundant main constituents are not activated. Tracer techniques are very useful for studies of the behaviour and of chemical reactions of trace elements and compounds in the environment. Radioactive sources are mainly applied for excitation of characteristic X-rays (X-ray fluorescence analysis). (author)

  5. Analytical study on the determination of boron in environmental water samples

    International Nuclear Information System (INIS)

    Lopez, F.J.; Gimenez, E.; Hernandez, F.

    1993-01-01

    An analytical study on the determination of boron in environmental water samples was carried out. The curcumin and carmine standard methods were compared with the most recent Azomethine-H method in order to evaluate their analytical characteristics and feasibility for the analysis of boron in water samples. Analyses of synthetic water, ground water, sea water and waste water samples were carried out and a statistical evaluation of the results was made. The Azomethine-H method was found to be the most sensitive (detection limit 0.02 mg l -1 ) and selective (no interference of commonly occurring ions in water was observed), showing also the best precision (relative standard deviation lower than 4%). Moreover, it gave good results for all types of samples analyzed. The accuracy of this method was tested by the addition of known amounts of standard solutions to different types of water samples. The slopes of standard additions and direct calibration graphs were similar and recoveries of added boron ranged from 99 to 107%. (orig.)

  6. A review of analytical techniques for the determination of carbon-14 in environmental samples

    International Nuclear Information System (INIS)

    Milton, G.M.; Brown, R.M.

    1993-11-01

    This report contains a brief summary of analytical techniques commonly used for the determination of radiocarbon in a variety of environmental samples. Details of the applicable procedures developed and tested in the Environmental Research Branch at Chalk River Laboratories are appended

  7. Improved analytical sensitivity for uranium and plutonium in environmental samples: Cavity ion source thermal ionization mass spectrometry

    International Nuclear Information System (INIS)

    Ingeneri, Kristofer; Riciputi, L.

    2001-01-01

    Following successful field trials, environmental sampling has played a central role as a routine part of safeguards inspections since early 1996 to verify declared and to detect undeclared activity. The environmental sampling program has brought a new series of analytical challenges, and driven a need for advances in verification technology. Environmental swipe samples are often extremely low in concentration of analyte (ng level or lower), yet the need to analyze these samples accurately and precisely is vital, particularly for the detection of undeclared nuclear activities. Thermal ionization mass spectrometry (TIMS) is the standard method of determining isotope ratios of uranium and plutonium in the environmental sampling program. TIMS analysis typically employs 1-3 filaments to vaporize and ionize the sample, and the ions are mass separated and analyzed using magnetic sector instruments due to their high mass resolution and high ion transmission. However, the ionization efficiency (the ratio of material present to material actually detected) of uranium using a standard TIMS instrument is low (0.2%), even under the best conditions. Increasing ionization efficiency by even a small amount would have a dramatic impact for safeguards applications, allowing both improvements in analytical precision and a significant decrease in the amount of uranium and plutonium required for analysis, increasing the sensitivity of environmental sampling

  8. Characterization of carbon nanotubes and analytical methods for their determination in environmental and biological samples: A review

    Energy Technology Data Exchange (ETDEWEB)

    Herrero-Latorre, C., E-mail: carlos.herrero@usc.es; Álvarez-Méndez, J.; Barciela-García, J.; García-Martín, S.; Peña-Crecente, R.M.

    2015-01-01

    Highlights: • Analytical techniques for characterization of CNTs: classification, description and examples. • Determination methods for CNTs in biological and environmental samples. • Future trends and perspectives for characterization and determination of CNTs. - Abstract: In the present paper, a critical overview of the most commonly used techniques for the characterization and the determination of carbon nanotubes (CNTs) is given on the basis of 170 references (2000–2014). The analytical techniques used for CNT characterization (including microscopic and diffraction, spectroscopic, thermal and separation techniques) are classified, described, and illustrated with applied examples. Furthermore, the performance of sampling procedures as well as the available methods for the determination of CNTs in real biological and environmental samples are reviewed and discussed according to their analytical characteristics. In addition, future trends and perspectives in this field of work are critically presented.

  9. A review of electro analytical determinations of some important elements (Zn, Se, As) in environmental samples

    International Nuclear Information System (INIS)

    Lichiang; James, B.D.; Magee, R.J.

    1991-01-01

    This review covers electro analytical methods reported in the literature for the determination of zinc, cadmium, selenium and arsenic in environmental and biological samples. A comprehensive survey of electro analytical techniques used for the determination of four important elements, i.e. zinc, cadmium, selenium and arsenic is reported herein with 322 references up to 1990. (Orig./A.B.)

  10. Analytical Methodologies for the Determination of Endocrine Disrupting Compounds in Biological and Environmental Samples

    Directory of Open Access Journals (Sweden)

    Zoraida Sosa-Ferrera

    2013-01-01

    Full Text Available Endocrine-disruptor compounds (EDCs can mimic natural hormones and produce adverse effects in the endocrine functions by interacting with estrogen receptors. EDCs include both natural and synthetic chemicals, such as hormones, personal care products, surfactants, and flame retardants, among others. EDCs are characterised by their ubiquitous presence at trace-level concentrations and their wide diversity. Since the discovery of the adverse effects of these pollutants on wildlife and human health, analytical methods have been developed for their qualitative and quantitative determination. In particular, mass-based analytical methods show excellent sensitivity and precision for their quantification. This paper reviews recently published analytical methodologies for the sample preparation and for the determination of these compounds in different environmental and biological matrices by liquid chromatography coupled with mass spectrometry. The various sample preparation techniques are compared and discussed. In addition, recent developments and advances in this field are presented.

  11. Practical reporting times for environmental samples

    International Nuclear Information System (INIS)

    Bayne, C.K.; Schmoyer, D.D.; Jenkins, R.A.

    1993-02-01

    Preanalytical holding times for environmental samples are specified because chemical and physical characteristics may change between sampling and chemical analysis. For example, the Federal Register prescribes a preanalytical holding time of 14 days for volatile organic compounds in soil stored at 4 degrees C. The American Society for Testing Materials (ASTM) uses a more technical definition that the preanalytical holding time is the day when the analyte concentration for an environmental sample falls below the lower 99% confidence interval on the analyte concentration at day zero. This study reviews various holding time definitions and suggest a new preanalytical holding time approach using acceptable error rates for measuring an environmental analyte. This practical reporting time (PRT) approach has been applied to nineteen volatile organic compounds and four explosives in three environmental soil samples. A PRT nomograph of error rates has been developed to estimate the consequences of missing a preanalytical holding time. This nomograph can be applied to a large class of analytes with concentrations that decay linearly or exponentially with time regardless of sample matrices and storage conditions

  12. Practical reporting times for environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Bayne, C.K.; Schmoyer, D.D.; Jenkins, R.A.

    1993-02-01

    Preanalytical holding times for environmental samples are specified because chemical and physical characteristics may change between sampling and chemical analysis. For example, the Federal Register prescribes a preanalytical holding time of 14 days for volatile organic compounds in soil stored at 4{degrees}C. The American Society for Testing Materials (ASTM) uses a more technical definition that the preanalytical holding time is the day when the analyte concentration for an environmental sample falls below the lower 99% confidence interval on the analyte concentration at day zero. This study reviews various holding time definitions and suggest a new preanalytical holding time approach using acceptable error rates for measuring an environmental analyte. This practical reporting time (PRT) approach has been applied to nineteen volatile organic compounds and four explosives in three environmental soil samples. A PRT nomograph of error rates has been developed to estimate the consequences of missing a preanalytical holding time. This nomograph can be applied to a large class of analytes with concentrations that decay linearly or exponentially with time regardless of sample matrices and storage conditions.

  13. Current status of JAERI program on development of ultra-trace-analytical technology for safeguards environmental samples

    International Nuclear Information System (INIS)

    Adachi, T.; Usuda, S.; Watanabe, K.

    2001-01-01

    Full text: In order to contribute to the strengthened safeguards system based on the Program 93+2 of the IAEA, Japan Atomic Energy Research Institute (JAERI) is developing analytical technology for ultra-trace amounts of nuclear materials in environmental samples, and constructed the CLEAR facility (Clean Laboratory for Environmental Analysis and Research) for this purpose. The development of the technology is carried out, at existing laboratories for time being, in the following fields: screening, bulk analysis and particle analysis. The screening aims at estimating the amounts of nuclear materials in environmental samples to be introduced into the clean rooms, and is the first step to avoid cross-contamination among the samples and contamination of the clean rooms themselves. In addition to ordinary radiation spectrometry, Compton suppression technique was applied to low energy γ- and X-ray measurements, and sufficient reduction in background level has been demonstrated. Another technique in examination is imaging-plate method, which is a kind of autoradiography and suitable for determination of radioactive-particle distribution in the samples as well as for semiquantitative determination. As for the bulk analysis, the efforts are temporally made on uranium in swipe samples. Preliminary examination for optimization of sample pre-treatment conditions is in progress. At present, ashing by low-temperature-plasma method gives better results than high-temperature ashing or acid leaching. For the isotopic ratio measurement, instrumental performance of inductively-coupled plasma mass spectrometry (ICP-MS) are mainly examined because sample preparation for ICP-MS is simpler than that for thermal ionization mass spectrometry (TIMS). It was found by our measurement that the swipe material (TexWipe TX304, usually used by IAEA) contains un-negligible uranium blank with large deviation (2-6 ng/sheet). This would introduce significant uncertainty in the trace analysis. JAERI

  14. Analytical methodologies for aluminium speciation in environmental and biological samples--a review.

    Science.gov (United States)

    Bi, S P; Yang, X D; Zhang, F P; Wang, X L; Zou, G W

    2001-08-01

    It is recognized that aluminium (Al) is a potential environmental hazard. Acidic deposition has been linked to increased Al concentrations in natural waters. Elevated levels of Al might have serious consequences for biological communities. Of particular interest is the speciation of Al in aquatic environments, because Al toxicity depends on its forms and concentrations. In this paper, advances in analytical methodologies for Al speciation in environmental and biological samples during the past five years are reviewed. Concerns about the specific problems of Al speciation and highlights of some important methods are elucidated in sections devoted to hybrid techniques (HPLC or FPLC coupled with ET-AAS, ICP-AES, or ICP-MS), flow-injection analysis (FIA), nuclear magnetic resonance (27Al NMR), electrochemical analysis, and computer simulation. More than 130 references are cited.

  15. Paper-Based Analytical Device for Zinc Ion Quantification in Water Samples with Power-Free Analyte Concentration

    Directory of Open Access Journals (Sweden)

    Hiroko Kudo

    2017-04-01

    Full Text Available Insufficient sensitivity is a general issue of colorimetric paper-based analytical devices (PADs for trace analyte detection, such as metal ions, in environmental water. This paper demonstrates the colorimetric detection of zinc ions (Zn2+ on a paper-based analytical device with an integrated analyte concentration system. Concentration of Zn2+ ions from an enlarged sample volume (1 mL has been achieved with the aid of a colorimetric Zn2+ indicator (Zincon electrostatically immobilized onto a filter paper substrate in combination with highly water-absorbent materials. Analyte concentration as well as sample pretreatment, including pH adjustment and interferent masking, has been elaborated. The resulting device enables colorimetric quantification of Zn2+ in environmental water samples (tap water, river water from a single sample application. The achieved detection limit of 0.53 μM is a significant improvement over that of a commercial colorimetric Zn2+ test paper (9.7 μM, demonstrating the efficiency of the developed analyte concentration system not requiring any equipment.

  16. Voltammetric technique, a panacea for analytical examination of environmental samples

    International Nuclear Information System (INIS)

    Zahir, E.; Mohiuddin, S.; Naqvi, I.I.

    2012-01-01

    Voltammetric methods for trace metal analysis in environmental samples of marine origin like mangrove, sediments and shrimps are generally recommended. Three different electro-analytical techniques i.e. polarography, anodic stripping voltammetry (ASV) and adsorptive stripping voltammetry (ADSV) have been used. Cd/sub 2/+, Pb/sub 2/+, Cu/sub 2/+ and Mn/sub 2/+ were determined through ASV, Cr/sub 6/+ was analyzed by ADSV and Fe/sub 2/+, Zn/sub 2/+, Ni/sub 2/+ and Co/sub 2/+ were determined through polarography. Out of which pairs of Fe/sub 2/+Zn/sub 2/+ and Ni/sub 2/+Co/sub 2/+ were determined in two separate runs while Cd/sub 2/+, Pb/sub 2/+, Cu/sub 2/+ were analyzed in single run of ASV. Sensitivity and speciation capabilities of voltammetric methods have been employed. Analysis conditions were optimized that includes selection of supporting electrolyte, pH, working electrodes, sweep rate etc. Stripping voltammetry was adopted for analysis at ultra trace levels. Statistical parameters for analytical method development like selectivity factor, interference, repeatability (0.0065-0.130 macro g/g), reproducibility (0.08125-1.625 macro g/g), detection limits (0.032-5.06 macro g/g), limits of quantification (0.081-12.652 macro g/g), sensitivities (5.636-2.15 nA mL macro g-1) etc. were also determined. The percentage recoveries were found in between 95-105% using certified reference materials. Real samples of complex marine environment from Karachi coastline were also analyzed. The standard addition method was employed where any matrix effect was evidenced. (author)

  17. Hanford analytical sample projections FY 1998 - FY 2002

    International Nuclear Information System (INIS)

    Joyce, S.M.

    1998-01-01

    Analytical Services projections are compiled for the Hanford site based on inputs from the major programs for the years 1998 through 2002. Projections are categorized by radiation level, protocol, sample matrix and program. Analyses requirements are also presented. This document summarizes the Hanford sample projections for fiscal years 1998 to 2002. Sample projections are based on inputs submitted to Analytical Services covering Environmental Restoration, Tank Waste Remediation Systems (TWRS), Solid Waste, Liquid Effluents, Spent Nuclear Fuels, Transition Projects, Site Monitoring, Industrial Hygiene, Analytical Services and miscellaneous Hanford support activities. In addition, details on laboratory scale technology (development) work, Sample Management, and Data Management activities are included. This information will be used by Hanford Analytical Services (HAS) and the Sample Management Working Group (SMWG) to assure that laboratories and resources are available and effectively utilized to meet these documented needs

  18. Hanford analytical sample projections FY 1998--FY 2002

    Energy Technology Data Exchange (ETDEWEB)

    Joyce, S.M.

    1998-02-12

    Analytical Services projections are compiled for the Hanford site based on inputs from the major programs for the years 1998 through 2002. Projections are categorized by radiation level, protocol, sample matrix and program. Analyses requirements are also presented. This document summarizes the Hanford sample projections for fiscal years 1998 to 2002. Sample projections are based on inputs submitted to Analytical Services covering Environmental Restoration, Tank Waste Remediation Systems (TWRS), Solid Waste, Liquid Effluents, Spent Nuclear Fuels, Transition Projects, Site Monitoring, Industrial Hygiene, Analytical Services and miscellaneous Hanford support activities. In addition, details on laboratory scale technology (development) work, Sample Management, and Data Management activities are included. This information will be used by Hanford Analytical Services (HAS) and the Sample Management Working Group (SMWG) to assure that laboratories and resources are available and effectively utilized to meet these documented needs.

  19. Role of analytical chemistry in environmental monitoring

    International Nuclear Information System (INIS)

    Kayasth, S.; Swain, K.

    2004-01-01

    Basic aspects of pollution and the role of analytical chemistry in environmental monitoring are highlighted and exemplified, with emphasis on trace elements. Sources and pathways of natural and especially man-made polluting substances as well as physico-chemical characteristics are given. Attention is paid to adequate sampling in various compartments of the environment comprising both lithosphere and biosphere. Trace analysis is dealt with using a variety of analytical techniques, including criteria for choice of suited techniques, as well as aspects of analytical quality assurance and control. Finally, some data on trace elements levels in soil and water samples from India are presented. (author)

  20. Hanford analytical sample projections FY 1996 - FY 2001. Revision 4

    Energy Technology Data Exchange (ETDEWEB)

    Joyce, S.M.

    1997-07-02

    This document summarizes the biannual Hanford sample projections for fiscal year 1997-2001. Sample projections are based on inputs submitted to Analytical Services covering Environmental Restoration, Tank Wastes Remediation Systems, Solid Wastes, Liquid Effluents, Spent Nuclear Fuels, Transition Projects, Site Monitoring, Industrial Hygiene, Analytical Services and miscellaneous Hanford support activities. In addition to this revision, details on Laboratory scale technology (development), Sample management, and Data management activities were requested. This information will be used by the Hanford Analytical Services program and the Sample Management Working Group to assure that laboratories and resources are available and effectively utilized to meet these documented needs.

  1. 35th International Symposium on Environmental Analytical Chemistry - ISEAC 35. Book of Abstracts

    International Nuclear Information System (INIS)

    Namiestnik, J.; Gdaniec-Pietryka, M.; Klimaszewska, K.; Gorecka, A.; Sagajdakow, A.; Jakubowska, N.

    2008-01-01

    The ISEAC 35 is organized by the International Association of Environmental Analytical Chemistry (IAEAC), the Committee on Analytical Chemistry of the Polish Academy of Science (PAS), and the Chemical Faculty of Gdansk University of Technology (GUT). The Symposium includes a number of invited lectures treating frontier topics of environmental analytical chemistry, such as: (a) miniaturized spectroscopic tools for environmental survey analysis, (b) remote sensing in marine research, (c) xenobiotics in natural waters, (d) sampling and sample handling for environmental analysis. Book of Abstracts contains abstracts of 9 invited lectures, 62 oral presentations and 250 posters.

  2. [Progress in sample preparation and analytical methods for trace polar small molecules in complex samples].

    Science.gov (United States)

    Zhang, Qianchun; Luo, Xialin; Li, Gongke; Xiao, Xiaohua

    2015-09-01

    Small polar molecules such as nucleosides, amines, amino acids are important analytes in biological, food, environmental, and other fields. It is necessary to develop efficient sample preparation and sensitive analytical methods for rapid analysis of these polar small molecules in complex matrices. Some typical materials in sample preparation, including silica, polymer, carbon, boric acid and so on, are introduced in this paper. Meanwhile, the applications and developments of analytical methods of polar small molecules, such as reversed-phase liquid chromatography, hydrophilic interaction chromatography, etc., are also reviewed.

  3. Environmental sampling for trace analysis

    International Nuclear Information System (INIS)

    Markert, B.

    1994-01-01

    Often too little attention is given to the sampling before and after actual instrumental measurement. This leads to errors, despite increasingly sensitive analytical systems. This is one of the first books to pay proper attention to representative sampling. It offers an overview of the most common techniques used today for taking environmental samples. The techniques are clearly presented, yield accurate and reproducible results and can be used to sample -air - water - soil and sediments - plants and animals. A comprehensive handbook, this volume provides an excellent starting point for researchers in the rapidly expanding field of environmental analysis. (orig.)

  4. Studies on application of neutron activation analysis -Applied research on air pollution monitoring and development of analytical method of environmental samples

    International Nuclear Information System (INIS)

    Chung, Yong Sam; Moon, Jong Hwa; Chung, Young Ju; Jeong, Eui Sik; Lee, Sang Mi; Kang, Sang Hun; Cho, Seung Yeon; Kwon, Young Sik; Chung, Sang Wuk; Lee, Kyu Sung; Chun, Ki Hong; Kim, Nak Bae; Lee, Kil Yong; Yoon, Yoon Yeol; Chun, Sang Ki.

    1997-09-01

    This research report is written for results of applied research on air pollution monitoring using instrumental neutron activation analysis. For identification and standardization of analytical method, 24 environmental samples are analyzed quantitatively, and accuracy and precision of this method are measured. Using airborne particulate matter and biomonitor chosen as environmental indicators, trace elemental concentrations of sample collected at urban and rural site monthly are determined ant then the calculation of statistics and the factor analysis are carried out for investigation of emission source. Facilities for NAA are installed in a new HANARO reactor, functional test is performed for routine operation. In addition, unified software code for NAA is developed to improve accuracy, precision and abilities of analytical processes. (author). 103 refs., 61 tabs., 19 figs

  5. Development of analytical methods for the separation of plutonium, americium, curium and neptunium from environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Salminen, S.

    2009-07-01

    In this work, separation methods have been developed for the analysis of anthropogenic transuranium elements plutonium, americium, curium and neptunium from environmental samples contaminated by global nuclear weapons testing and the Chernobyl accident. The analytical methods utilized in this study are based on extraction chromatography. Highly varying atmospheric plutonium isotope concentrations and activity ratios were found at both Kurchatov (Kazakhstan), near the former Semipalatinsk test site, and Sodankylae (Finland). The origin of plutonium is almost impossible to identify at Kurchatov, since hundreds of nuclear tests were performed at the Semipalatinsk test site. In Sodankylae, plutonium in the surface air originated from nuclear weapons testing, conducted mostly by USSR and USA before the sampling year 1963. The variation in americium, curium and neptunium concentrations was great as well in peat samples collected in southern and central Finland in 1986 immediately after the Chernobyl accident. The main source of transuranium contamination in peats was from global nuclear test fallout, although there are wide regional differences in the fraction of Chernobyl-originated activity (of the total activity) for americium, curium and neptunium. The separation methods developed in this study yielded good chemical recovery for the elements investigated and adequately pure fractions for radiometric activity determination. The extraction chromatographic methods were faster compared to older methods based on ion exchange chromatography. In addition, extraction chromatography is a more environmentally friendly separation method than ion exchange, because less acidic waste solutions are produced during the analytical procedures. (orig.)

  6. Speciation of organotin compounds in environmental samples by GC-ICPMS

    International Nuclear Information System (INIS)

    Vahcic, M.; Milacic, R.; Scancar, J.

    2009-01-01

    Full text: Analytical procedure using 15 m GC column was applied for simultaneous speciation of OTCs in various environmental samples. Methyl-, butyl-, phenyl- and octyl- tin species were quantitatively determined. different extraction reagents and conditions were studied. OTCs species were derivatized by NaBEt 4 and extracted into isooctane or hexane. The applied analytical procedure considerably shortened analytical time and enabled simultaneous determination of 12 OTCs in environmental samples. (author)

  7. Soil sampling for environmental contaminants

    International Nuclear Information System (INIS)

    2004-10-01

    The Consultants Meeting on Sampling Strategies, Sampling and Storage of Soil for Environmental Monitoring of Contaminants was organized by the International Atomic Energy Agency to evaluate methods for soil sampling in radionuclide monitoring and heavy metal surveys for identification of punctual contamination (hot particles) in large area surveys and screening experiments. A group of experts was invited by the IAEA to discuss and recommend methods for representative soil sampling for different kinds of environmental issues. The ultimate sinks for all kinds of contaminants dispersed within the natural environment through human activities are sediment and soil. Soil is a particularly difficult matrix for environmental pollution studies as it is generally composed of a multitude of geological and biological materials resulting from weathering and degradation, including particles of different sizes with varying surface and chemical properties. There are so many different soil types categorized according to their content of biological matter, from sandy soils to loam and peat soils, which make analytical characterization even more complicated. Soil sampling for environmental monitoring of pollutants, therefore, is still a matter of debate in the community of soil, environmental and analytical sciences. The scope of the consultants meeting included evaluating existing techniques with regard to their practicability, reliability and applicability to different purposes, developing strategies of representative soil sampling for cases not yet considered by current techniques and recommending validated techniques applicable to laboratories in developing Member States. This TECDOC includes a critical survey of existing approaches and their feasibility to be applied in developing countries. The report is valuable for radioanalytical laboratories in Member States. It would assist them in quality control and accreditation process

  8. A sensitive analytical procedure for monitoring acrylamide in environmental water samples by offline SPE-UPLC/MS/MS.

    Science.gov (United States)

    Togola, Anne; Coureau, Charlotte; Guezennec, Anne-Gwenaëlle; Touzé, Solène

    2015-05-01

    The presence of acrylamide in natural systems is of concern from both environmental and health points of view. We developed an accurate and robust analytical procedure (offline solid phase extraction combined with UPLC/MS/MS) with a limit of quantification (20 ng L(-1)) compatible with toxicity threshold values. The optimized (considering the nature of extraction phases, sampling volumes, and solvent of elution) solid phase extraction (SPE) was validated according to ISO Standard ISO/IEC 17025 on groundwater, surface water, and industrial process water samples. Acrylamide is highly polar, which induces a high variability during the SPE step, therefore requiring the use of C(13)-labeled acrylamide as an internal standard to guarantee the accuracy and robustness of the method (uncertainty about 25 % (k = 2) at limit of quantification level). The specificity of the method and the stability of acrylamide were studied for these environmental media, and it was shown that the method is suitable for measuring acrylamide in environmental studies.

  9. Development of an analytical procedure for plutonium in the concentration range of femtogram/gram and its application to environmental samples

    International Nuclear Information System (INIS)

    Schuettelkopf, H.

    1981-09-01

    To study the behaviour of plutonium in the environment and to measure plutonium in the vicinity of nuclear facilities, a quick, sensitive analytical method is required which can be applied to all sample materials found in the environment. For a sediment contaminated with plutonium a boiling out method using first HNO 3 /HF and subsequently HNO 3 /Al(NO 3 ) 3 was found to be successful. The leaching solution was then extracted by TOPO and the plutonium backextracted by ascorbic acid/HCl. Some different purification steps and finally electroplating using ammonium oxalate led to an optimum sample for α- spectroscopic determination of plutonium. An analytical method was worked out for plutonium which can be applied to all materials found in the environment. The sample size is 100 g but it might also be much greater. The average chemical yield is 70 and 80%. The detection limit for soil samples is 0.1 fCi/g and for plant samples 0.5 fCi/g. One technician can perform eight analyses per working day. The analytical procedure was applied to a large number of environmental samples and the results of these analyses are indicated. (orig./RB) [de

  10. Development of analytical techniques for water and environmental samples (2)

    Energy Technology Data Exchange (ETDEWEB)

    Eum, Chul Hun; Jeon, Chi Wan; Jung, Kang Sup; Song, Kyung Sun; Kim, Sang Yeon [Korea Institute of Geology Mining and Materials, Taejon (Korea)

    1998-12-01

    The purpose of this study is to develop new analytical methods with good detection limit for toxic inorganic and organic compounds. The analyses of CN, organic acids, particulate materials in environmental samples have been done using several methods such as Ion Chromatography, SPE, SPME, GC/MS, GC/FID, SPLITT (split-flow thin cell fractionation) during the second year of this project. Advantage and disadvantage of several distillation method (by KS, JIS, EPA) for CN analysis in wastewater were investigated. As the results, we proposed new distillation apparatus for CN analysis, which was proved to be simpler, faster and to get better recovery than conventional apparatus. And ion chromatograph/pulsed amperometric detector (IC/PAD) system instead of colorimetry for CN detection was setup to solve matrix interference. And SPE(solid phase extraction) and SPME (solid phase micro extraction) as liquid-solid extraction technique were applied to the analysis of phenols in wastewater. Optimum experimental conditions and factors influencing analytical results were determined. From these results, It could be concluded that C{sub 18} cartridge and polystyrene-divinylbenzene disk in SPE method, polyacrylate fiber in SPME were proper solid phase adsorbent for phenol. Optimum conditions to analyze phenol derivatives simultaneously were established. Also, Continuous SPLITT (Split-flow thin cell) Fractionation (CSF) is a new preparative separation technique that is useful for fractionation of particulate and macromolecular materials. CSF is carried out in a thin ribbon-like channel equipped with two splitters at both inlet and outlet of the channel. In this work, we set up a new CSF system, and tested using polystyrene latex standard particles. And then we fractionated particles contained in air and underground water based on their sedimentation coefficients using CSF. (author). 27 refs., 13 tabs., 31 figs.

  11. Theoretical, analytical, and statistical interpretation of environmental data

    International Nuclear Information System (INIS)

    Lombard, S.M.

    1974-01-01

    The reliability of data from radiochemical analyses of environmental samples cannot be determined from nuclear counting statistics alone. The rigorous application of the principles of propagation of errors, an understanding of the physics and chemistry of the species of interest in the environment, and the application of information from research on the analytical procedure are all necessary for a valid estimation of the errors associated with analytical results. The specific case of the determination of plutonium in soil is considered in terms of analytical problems and data reliability. (U.S.)

  12. Determination of technetium-99 in environmental samples: A review

    International Nuclear Information System (INIS)

    Shi Keliang; Hou Xiaolin; Roos, Per; Wu Wangsuo

    2012-01-01

    Highlights: ► The source term, physicochemical properties, environmental distribution and behaviour of 99 Tc are presented. ► Various sample pre-treatment and pre-concentration techniques of technetium are discussed. ► Chemical separation and purification techniques for 99 Tc in environmental samples are reviewed. ► Measurement techniques for 99 Tc in environmental level and automated analytical methods are reviewed. ► The reported analytical methods of 99 Tc are critically compared to provide overall information. - Abstract: Due to the lack of a stable technetium isotope, and the high mobility and long half-life, 99 Tc is considered to be one of the most important radionuclides in safety assessment of environmental radioactivity as well as nuclear waste management. 99 Tc is also an important tracer for oceanographic research due to the high technetium solubility in seawater as TcO 4 − . A number of analytical methods, using chemical separation combined with radiometric and mass spectrometric measurement techniques, have been developed over the past decades for determination of 99 Tc in different environmental samples. This article summarizes and compares recently reported chemical separation procedures and measurement methods for determination of 99 Tc. Due to the extremely low concentration of 99 Tc in environmental samples, the sample preparation, pre-concentration, chemical separation and purification for removal of the interferences for detection of 99 Tc are the most important issues governing the accurate determination of 99 Tc. These aspects are discussed in detail in this article. Meanwhile, the different measurement techniques for 99 Tc are also compared with respect to advantages and drawbacks. Novel automated analytical methods for rapid determination of 99 Tc using solid extraction or ion exchange chromatography for separation of 99 Tc, employing flow injection or sequential injection approaches are also discussed.

  13. Evaluation of environmental samples containing heavy hydrocarbon components in environmental forensic investigations

    Energy Technology Data Exchange (ETDEWEB)

    Raia, J.C.; Blakley, C.R.; Fuex, A.N.; Villalanti, D.C.; Fahrenthold, P.D. [Triton Anal Corp, Houston, TX (United States)

    2004-03-01

    This article presents a procedure to evaluate and characterize environmental samples containing mixtures of hydrocarbons over a wide boiling range of materials that include fuels and other products used in commerce. The range of the method extends to the higher boiling and heavier molecular weight hydrocarbon products in the range of motor oil, bunker fuel, and heavier residue materials. The procedure uses the analytical laboratory technique of high-temperature simulated distillation along with mathematical regression of the analytical data to estimate the relative contribution of individual products in mixtures of hydrocarbons present in environmental samples. An analytical technique to determine hydrocarbon-type distributions by gas chromatography-mass spectrometry with nitric oxide ionization spectrometry evaluation is also presented. This type of analysis allows complex hydrocarbon mixtures to be classified by their chemical composition, or types of hydrocarbons that include paraffins, cycloparaffins, monoaromatics, and polycyclic aromatic hydrocarbons. Characteristic hydrocarbon patterns for example, in the relative distribution of polycyclic aromatic hydrocarbons are valuable for determining the potential origin of materials present in environmental samples. These methods provide quantitative data for hydrocarbon components in mixtures as a function of boiling range and 'hydrocarbon fingerprints' of the types of materials present. This information is valuable in assessing environmental impacts of hydrocarbons at contaminated sites and establishing the liabilities and cost allocations for responsible parties.

  14. Sampling and measurement of long-lived radionuclides in environmental samples

    International Nuclear Information System (INIS)

    Brauer, F.P.; Goles, R.W.; Kaye, J.H.; Rieck, H.G. Jr.

    1977-01-01

    The volatile and semivolatile long-lived man-made radionuclides 3 H, 14 C, 79 Se, 85 Kr, 99 Tc, 129 I, 135 Cs, and 137 Cs are of concern in operation of nuclear facilities because they are difficult and expensive to contain and once emitted to the environment they become permanent ecological constituents with both local and global distributions. Species-selective sampling and analytical methods (radiochemical, neutron activation, and mass spectrometric) have been developed for many of these nuclides with sensitivities well below those required for radiation protection. These sampling and analytical methods have been applied to the measurement of current environmental levels of some of the more ecologically important radionuclides. The detection and tracing of long-lived radionuclides is being conducted in order to establish base-line values and to study environmental behavior. This paper describes detection and measurement techniques and summarizes current measurement results

  15. Nuclear and nuclear related analytical methods applied in environmental research

    International Nuclear Information System (INIS)

    Popescu, Ion V.; Gheboianu, Anca; Bancuta, Iulian; Cimpoca, G. V; Stihi, Claudia; Radulescu, Cristiana; Oros Calin; Frontasyeva, Marina; Petre, Marian; Dulama, Ioana; Vlaicu, G.

    2010-01-01

    Nuclear Analytical Methods can be used for research activities on environmental studies like water quality assessment, pesticide residues, global climatic change (transboundary), pollution and remediation. Heavy metal pollution is a problem associated with areas of intensive industrial activity. In this work the moss bio monitoring technique was employed to study the atmospheric deposition in Dambovita County Romania. Also, there were used complementary nuclear and atomic analytical methods: Neutron Activation Analysis (NAA), Atomic Absorption Spectrometry (AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). These high sensitivity analysis methods were used to determine the chemical composition of some samples of mosses placed in different areas with different pollution industrial sources. The concentrations of Cr, Fe, Mn, Ni and Zn were determined. The concentration of Fe from the same samples was determined using all these methods and we obtained a very good agreement, in statistical limits, which demonstrate the capability of these analytical methods to be applied on a large spectrum of environmental samples with the same results. (authors)

  16. Isotope dilution and sampling factors of the quality assurance and TQM of environmental analysis

    International Nuclear Information System (INIS)

    Macasek, F.

    1999-01-01

    Sampling and preparatory treatment of environmental objects is discussed from the view of their information content, functional speciation of the pollutant, statistical distribution treatment and uncertainty assessment. During homogenization of large samples, a substantial information may be lost and validity of environmental information becomes vague. Isotope dilution analysis is discussed as the most valuable tool for both validity of analysis and evaluation of samples variance. Data collection for a non-parametric statistical treatment of series of 'non-representative' sub-samples, and physico-chemical speciation of analyte may actually better fulfill criteria of similarity and representativeness. Large samples are often required due to detection limits of analysis, but the representativeness of environmental samples should by understood not only by the mean analyte concentration, but also by its spatial and time variance. Hence, heuristic analytical scenarios and interpretation of results must be designed by cooperation of environmentalists and analytical chemists. (author)

  17. DOE methods for evaluating environmental and waste management samples

    International Nuclear Information System (INIS)

    Goheen, S.C.; McCulloch, M.; Thomas, B.L.; Riley, R.G.; Sklarew, D.S.; Mong, G.M.; Fadeff, S.K.

    1993-03-01

    DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) provides applicable methods in use by. the US Department of Energy (DOE) laboratories for sampling and analyzing constituents of waste and environmental samples. The development of DOE Methods is supported by the Laboratory Management Division (LMD) of the DOE. This document contains chapters and methods that are proposed for use in evaluating components of DOE environmental and waste management samples. DOE Methods is a resource intended to support sampling and analytical activities that will aid in defining the type and breadth of contamination and thus determine the extent of environmental restoration or waste management actions needed, as defined by the DOE, the US Environmental Protection Agency (EPA), or others

  18. DOE methods for evaluating environmental and waste management samples.

    Energy Technology Data Exchange (ETDEWEB)

    Goheen, S C; McCulloch, M; Thomas, B L; Riley, R G; Sklarew, D S; Mong, G M; Fadeff, S K [eds.; Pacific Northwest Lab., Richland, WA (United States)

    1994-04-01

    DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) provides applicable methods in use by. the US Department of Energy (DOE) laboratories for sampling and analyzing constituents of waste and environmental samples. The development of DOE Methods is supported by the Laboratory Management Division (LMD) of the DOE. This document contains chapters and methods that are proposed for use in evaluating components of DOE environmental and waste management samples. DOE Methods is a resource intended to support sampling and analytical activities that will aid in defining the type and breadth of contamination and thus determine the extent of environmental restoration or waste management actions needed, as defined by the DOE, the US Environmental Protection Agency (EPA), or others.

  19. Report on DOE analytical laboratory capacity available to meet EM environmental sampling and analysis needs for FY 93-99

    International Nuclear Information System (INIS)

    1994-01-01

    The DOE Analytical Laboratory Capacity Study was conducted to give EM-263 current information about existing and future analytical capacities and capabilities of site laboratories within the DOE Complex. Each DOE site may have one or more analytical laboratories in operation. These facilities were established to support site missions such as production, research and development, and personnel and environmental monitoring. With changing site missions and the DOE directives for environmental monitoring and cleanup, these laboratories are either devoting or planning to devote resources to support EM activities. The DOE site laboratories represent a considerable amount of capital investment and analytical capability, capacity, and expertise that can be applied to support the EM mission. They not only provide cost-effective high-volume analytical laboratory services, but are also highly recognized analytical research and development centers. Several sites have already transferred their analytical capability from traditional production support to environmental monitoring and waste management support. A model was developed to determine the analytical capacity of all laboratories in the DOE Complex. The model was applied at nearly all the major laboratories and the results collected from these studies are summarized in this report

  20. Sampling, storage and sample preparation procedures for X ray fluorescence analysis of environmental materials

    International Nuclear Information System (INIS)

    1997-06-01

    X ray fluorescence (XRF) method is one of the most commonly used nuclear analytical technique because of its multielement and non-destructive character, speed, economy and ease of operation. From the point of view of quality assurance practices, sampling and sample preparation procedures are the most crucial steps in all analytical techniques, (including X ray fluorescence) applied for the analysis of heterogeneous materials. This technical document covers recent modes of the X ray fluorescence method and recent developments in sample preparation techniques for the analysis of environmental materials. Refs, figs, tabs

  1. Empirical insights and considerations for the OBT inter-laboratory comparison of environmental samples

    International Nuclear Information System (INIS)

    Kim, Sang-Bog; Roche, Jennifer

    2013-01-01

    Organically bound tritium (OBT) is an important tritium species that can be measured in most environmental samples, but has only recently been recognized as a species of tritium in these samples. Currently, OBT is not routinely measured by environmental monitoring laboratories around the world. There are no certified reference materials (CRMs) for environmental samples. Thus, quality assurance (QA), or verification of the accuracy of the OBT measurement, is not possible. Alternatively, quality control (QC), or verification of the precision of the OBT measurement, can be achieved. In the past, there have been differences in OBT analysis results between environmental laboratories. A possible reason for the discrepancies may be differences in analytical methods. Therefore, inter-laboratory OBT comparisons among the environmental laboratories are important and would provide a good opportunity for adopting a reference OBT analytical procedure. Due to the analytical issues, only limited information is available on OBT measurement. Previously conducted OBT inter-laboratory practices are reviewed and the findings are described. Based on our experiences, a few considerations were suggested for the international OBT inter-laboratory comparison exercise to be completed in the near future. -- Highlights: ► Inter-laboratory OBT comparisons would provide a good opportunity for developing reference OBT analytical procedures. ► The measurement of environmental OBT concentrations has a higher associated uncertainty. ► Certified reference materials for OBT in environmental samples are required

  2. Intercalibration of analytical methods on marine environmental samples

    International Nuclear Information System (INIS)

    1988-06-01

    The pollution of the seas by various chemical substances constitutes nowadays one of the principal concerns of mankind. The International Atomic Energy Agency has organized in past years several intercomparison exercises in the framework of its Analytical Quality Control Service. The present intercomparison had a double aim: first, to give laboratories participating in this intercomparison an opportunity for checking their analytical performance. Secondly, to produce on the basis of the results of this intercomparison a reference material made of fish tissue which would be accurately certified with respect to many trace elements. Such a material could be used by analytical chemists to check the validity of new analytical procedures. In total, 53 laboratories from 29 countries reported results (585 laboratory means for 48 elements). 5 refs, 52 tabs

  3. Evaluating the reproducibility of environmental radioactivity monitoring data through replicate sample analysis

    International Nuclear Information System (INIS)

    Lindeken, C.L.; White, J.H.; Silver, W.J.

    1978-01-01

    At the Lawrence Livermore Laboratory, about 10% of the sampling effort in the environmental monitoring program represents replicate sample collection. Replication of field samples was initiated as part of the quality assurance program for environmental monitoring to determine the reproducibility of environmental measurements. In the laboratory these replicates are processed along with routine samples. As all components of variance are included in analysis of such field samples, comparison of the analytical data from replicate analyses provides a basis for estimating the overall reproducibility of the measurements. The replication study indicates that the reproducibility of environmental radioactivity monitoring data is subject to considerably more variability than is indicated by the accompanying counting errors. The data are also compared with analyses of duplicate aliquots from a well mixed sample or with duplicate aliquots of samples with known radionuclide content. These comparisons show that most of the variability is associated with the collection and preparation of the sample rather than with the analytical procedures

  4. Comparison of the analytical methods used to determine natural and artificial radionuclides from environmental samples by gamma, alpha and beta spectrometry

    DEFF Research Database (Denmark)

    Pöllänen, Roy; Virtanen, Sinikka; Kämäräinen, Meerit

    In CAMNAR, an extensive interlaboratory exercise on the analytical methods used to determine several radionuclides present in the environmental samples was organized. Activity concentration of different natural radionuclides, such as Rn-222, Pb-210, Po-210, K-40, Ra-226, Ra-228 and isotopes...... of uranium, in addition to artificial Cs-137 and Am-241 were analysed from lake sediment samples and drinking water. The measurement techniques were gamma-ray spectrometry, alpha spectrometry, liquid scintillation counting and inductively coupled plasma mass spectrometry. Twenty six laboratories from nine...

  5. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    Directory of Open Access Journals (Sweden)

    Helena Prosen

    2014-05-01

    Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  6. Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

    Science.gov (United States)

    Prosen, Helena

    2014-05-23

    Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

  7. Analytical quality control in environmental analysis - Recent results and future trends of the IAEA's analytical quality control programme

    Energy Technology Data Exchange (ETDEWEB)

    Suschny, O; Heinonen, J

    1973-12-01

    The significance of analytical results depends critically on the degree of their reliability, an assessment of this reliability is indispensable if the results are to have any meaning at all. Environmental radionuclide analysis is a relatively new analytical field in which new methods are continuously being developed and into which many new laboratories have entered during the last ten to fifteen years. The scarcity of routine methods and the lack of experience of the new laboratories have made the need for the assessment of the reliability of results particularly urgent in this field. The IAEA, since 1962, has provided assistance to its member states by making available to their laboratories analytical quality control services in the form of standard samples, reference materials and the organization of analytical intercomparisons. The scope of this programme has increased over the years and now includes, in addition to environmental radionuclides, non-radioactive environmental contaminants which may be analysed by nuclear methods, materials for forensic neutron activation analysis, bioassay materials and nuclear fuel. The results obtained in recent intercomparisons demonstrate the continued need for these services. (author)

  8. DOE methods for evaluating environmental and waste management samples

    Energy Technology Data Exchange (ETDEWEB)

    Goheen, S.C.; McCulloch, M.; Thomas, B.L.; Riley, R.G.; Sklarew, D.S.; Mong, G.M.; Fadeff, S.K. [eds.

    1994-10-01

    DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) is a resource intended to support sampling and analytical activities for the evaluation of environmental and waste management samples from U.S. Department of Energy (DOE) sites. DOE Methods is the result of extensive cooperation from all DOE analytical laboratories. All of these laboratories have contributed key information and provided technical reviews as well as significant moral support leading to the success of this document. DOE Methods is designed to encompass methods for collecting representative samples and for determining the radioisotope activity and organic and inorganic composition of a sample. These determinations will aid in defining the type and breadth of contamination and thus determine the extent of environmental restoration or waste management actions needed, as defined by the DOE, the U.S. Environmental Protection Agency, or others. The development of DOE Methods is supported by the Analytical Services Division of DOE. Unique methods or methods consolidated from similar procedures in the DOE Procedures Database are selected for potential inclusion in this document. Initial selection is based largely on DOE needs and procedure applicability and completeness. Methods appearing in this document are one of two types, {open_quotes}Draft{close_quotes} or {open_quotes}Verified{close_quotes}. {open_quotes}Draft{close_quotes} methods that have been reviewed internally and show potential for eventual verification are included in this document, but they have not been reviewed externally, and their precision and bias may not be known. {open_quotes}Verified{close_quotes} methods in DOE Methods have been reviewed by volunteers from various DOE sites and private corporations. These methods have delineated measures of precision and accuracy.

  9. DOE methods for evaluating environmental and waste management samples

    International Nuclear Information System (INIS)

    Goheen, S.C.; McCulloch, M.; Thomas, B.L.; Riley, R.G.; Sklarew, D.S.; Mong, G.M.; Fadeff, S.K.

    1994-10-01

    DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) is a resource intended to support sampling and analytical activities for the evaluation of environmental and waste management samples from U.S. Department of Energy (DOE) sites. DOE Methods is the result of extensive cooperation from all DOE analytical laboratories. All of these laboratories have contributed key information and provided technical reviews as well as significant moral support leading to the success of this document. DOE Methods is designed to encompass methods for collecting representative samples and for determining the radioisotope activity and organic and inorganic composition of a sample. These determinations will aid in defining the type and breadth of contamination and thus determine the extent of environmental restoration or waste management actions needed, as defined by the DOE, the U.S. Environmental Protection Agency, or others. The development of DOE Methods is supported by the Analytical Services Division of DOE. Unique methods or methods consolidated from similar procedures in the DOE Procedures Database are selected for potential inclusion in this document. Initial selection is based largely on DOE needs and procedure applicability and completeness. Methods appearing in this document are one of two types, open-quotes Draftclose quotes or open-quotes Verifiedclose quotes. open-quotes Draftclose quotes methods that have been reviewed internally and show potential for eventual verification are included in this document, but they have not been reviewed externally, and their precision and bias may not be known. open-quotes Verifiedclose quotes methods in DOE Methods have been reviewed by volunteers from various DOE sites and private corporations. These methods have delineated measures of precision and accuracy

  10. DOE methods for evaluating environmental and waste management samples

    International Nuclear Information System (INIS)

    Goheen, S.C.; McCulloch, M.; Thomas, B.L.; Riley, R.G.; Sklarew, D.S.; Mong, G.M.; Fadeff, S.K.

    1994-04-01

    DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) is a resource intended to support sampling and analytical activities for the evaluation of environmental and waste management samples from U.S. Department of Energy (DOE) sites. DOE Methods is the result of extensive cooperation from all DOE analytical laboratories. All of these laboratories have contributed key information and provided technical reviews as well as significant moral support leading to the success of this document. DOE Methods is designed to encompass methods for collecting representative samples and for determining the radioisotope activity and organic and inorganic composition of a sample. These determinations will aid in defining the type and breadth of contamination and thus determine the extent of environmental restoration or waste management actions needed, as defined by the DOE, the U.S. Environmental Protection Agency, or others. The development of DOE Methods is supported by the Laboratory Management Division of the DOE. Methods are prepared for entry into DOE Methods as chapter editors, together with DOE and other participants in this program, identify analytical and sampling method needs. Unique methods or methods consolidated from similar procedures in the DOE Procedures Database are selected for potential inclusion in this document. Initial selection is based largely on DOE needs and procedure applicability and completeness. Methods appearing in this document are one of two types. open-quotes Draftclose quotes or open-quotes Verified.close quotes. open-quotes Draftclose quotes methods that have been reviewed internally and show potential for eventual verification are included in this document, but they have not been reviewed externally, and their precision and bias may not be known. open-quotes Verifiedclose quotes methods in DOE Methods have been reviewed by volunteers from various DOE sites and private corporations

  11. Analytical techniques for measurement of 99Tc in environmental samples

    International Nuclear Information System (INIS)

    Anon.

    1979-01-01

    Three new methods have been developed for measuring 99 Tc in environmental samples. The most sensitive method is isotope dilution mass spectrometry, which allows measurement of about 1 x 10 -12 grams of 99 Tc. Results on analysis of five samples by this method compare very well with values obtained by a second independent method, which involves counting of beta particles from 99 Tc and internal conversion electrons from /sup 97m/Tc. A third method involving electrothermal atomic absorption has also been developed. Although this method is not as sensitive as the first two techniques, the cost per analysis is expected to be considerably less for certain types of samples

  12. Temperature-controlled micro-TLC: a versatile green chemistry and fast analytical tool for separation and preliminary screening of steroids fraction from biological and environmental samples.

    Science.gov (United States)

    Zarzycki, Paweł K; Slączka, Magdalena M; Zarzycka, Magdalena B; Bartoszuk, Małgorzata A; Włodarczyk, Elżbieta; Baran, Michał J

    2011-11-01

    This paper is a continuation of our previous research focusing on development of micro-TLC methodology under temperature-controlled conditions. The main goal of present paper is to demonstrate separation and detection capability of micro-TLC technique involving simple analytical protocols without multi-steps sample pre-purification. One of the advantages of planar chromatography over its column counterpart is that each TLC run can be performed using non-previously used stationary phase. Therefore, it is possible to fractionate or separate complex samples characterized by heavy biological matrix loading. In present studies components of interest, mainly steroids, were isolated from biological samples like fish bile using single pre-treatment steps involving direct organic liquid extraction and/or deproteinization by freeze-drying method. Low-molecular mass compounds with polarity ranging from estetrol to progesterone derived from the environmental samples (lake water, untreated and treated sewage waters) were concentrated using optimized solid-phase extraction (SPE). Specific bands patterns for samples derived from surface water of the Middle Pomerania in northern part of Poland can be easily observed on obtained micro-TLC chromatograms. This approach can be useful as simple and non-expensive complementary method for fast control and screening of treated sewage water discharged by the municipal wastewater treatment plants. Moreover, our experimental results show the potential of micro-TLC as an efficient tool for retention measurements of a wide range of steroids under reversed-phase (RP) chromatographic conditions. These data can be used for further optimalization of SPE or HPLC systems working under RP conditions. Furthermore, we also demonstrated that micro-TLC based analytical approach can be applied as an effective method for the internal standard (IS) substance search. Generally, described methodology can be applied for fast fractionation or screening of the

  13. State of the art of environmentally friendly sample preparation approaches for determination of PBDEs and metabolites in environmental and biological samples: A critical review.

    Science.gov (United States)

    Berton, Paula; Lana, Nerina B; Ríos, Juan M; García-Reyes, Juan F; Altamirano, Jorgelina C

    2016-01-28

    Green chemistry principles for developing methodologies have gained attention in analytical chemistry in recent decades. A growing number of analytical techniques have been proposed for determination of organic persistent pollutants in environmental and biological samples. In this light, the current review aims to present state-of-the-art sample preparation approaches based on green analytical principles proposed for the determination of polybrominated diphenyl ethers (PBDEs) and metabolites (OH-PBDEs and MeO-PBDEs) in environmental and biological samples. Approaches to lower the solvent consumption and accelerate the extraction, such as pressurized liquid extraction, microwave-assisted extraction, and ultrasound-assisted extraction, are discussed in this review. Special attention is paid to miniaturized sample preparation methodologies and strategies proposed to reduce organic solvent consumption. Additionally, extraction techniques based on alternative solvents (surfactants, supercritical fluids, or ionic liquids) are also commented in this work, even though these are scarcely used for determination of PBDEs. In addition to liquid-based extraction techniques, solid-based analytical techniques are also addressed. The development of greener, faster and simpler sample preparation approaches has increased in recent years (2003-2013). Among green extraction techniques, those based on the liquid phase predominate over those based on the solid phase (71% vs. 29%, respectively). For solid samples, solvent assisted extraction techniques are preferred for leaching of PBDEs, and liquid phase microextraction techniques are mostly used for liquid samples. Likewise, green characteristics of the instrumental analysis used after the extraction and clean-up steps are briefly discussed. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Environmental analytical laboratory setup operation and QA/QC

    International Nuclear Information System (INIS)

    Hsu, J.P.; Boyd, J.A.; DeViney, S.

    1991-01-01

    Environmental analysis requires precise and timely measurements. The required precise measurement is ensured with quality control and timeliness through an efficient operation. The efficiency of the operation also ensures cost-competitiveness. Environmental analysis plays a very important role in the environmental protection program. Due to the possible litigation involvement, most environmental analyses follow stringent criteria, such as the U.S. EPA Contract Laboratory Program procedures with analytical results documented in an orderly manner. The documentation demonstrates that all quality control steps are followed and facilitates data evaluation to determine the quality and usefulness of the data. Furthermore, the tedious documents concerning sample checking, chain-of-custody, standard or surrogate preparation, daily refrigerator and oven temperature monitoring, analytical and extraction logbooks, standard operation procedures, etc., also are an important part of the laboratory documentation. Quality control for environmental analysis is becoming more stringent, required documentation is becoming more detailed and turnaround time is shorter. However, the business is becoming more cost-competitive and it appears that this trend will continue. In this paper, we discuss what should be done to deal this high quality, fast-paced and tedious environmental analysis process at a competitive cost. The success of environmental analysis is people. The knowledge and experience of the staff are the key to a successful environmental analysis program. In order to be successful in this new area, the ability to develop new methods is crucial. In addition, the laboratory information system, laboratory automation and quality assurance/quality control (QA/QC) are major factors for laboratory success. This paper concentrates on these areas

  15. Determination of radium isotopes in environmental samples by gamma spectrometry, liquid scintillation counting and alpha spectrometry: a review of analytical methodology

    International Nuclear Information System (INIS)

    Jia, Guogang; Jia, Jing

    2012-01-01

    Radium (Ra) isotopes are important from the viewpoints of radiation protection and environmental protection. Their high toxicity has stimulated the continuing interest in methodology research for determination of Ra isotopes in various media. In this paper, the three most routinely used analytical techniques for Ra isotope determination in biological and environmental samples, i.e. low-background γ-spectrometry, liquid scintillation counting and α-spectrometry, were reviewed, with emphasis on new methodological developments in sample preparation, preconcentration, separation, purification, source preparation and measurement techniques. The accuracy, selectivity, traceability, applicability and minimum detectable activity (MDA) of the three techniques were discussed. It was concluded that the MDA (0.1 mBq L −1 ) of the α-spectrometry technique coupled with chemical separation is about two orders of magnitude lower than that of low-background HPGe γ-spectrometry and LSC techniques. Therefore, when maximum sensitivity is required, the α-spectrometry technique remains the first choice. - Highlights: ► A review is made for determination of Ra isotopes in environmental samples. ► Gamma spectrometry, LSC and a-spectrometry are the main concerned radiometric approach. ► Sample preparation, preconcentration, separation and source preparation are discussed. ► The methods can analyse air, water, seawater, soil, sediment and foodstuffs samples. ► Some new data obtained recently from our laboratory for Ra method study are included.

  16. New trends in sample preparation techniques for environmental analysis.

    Science.gov (United States)

    Ribeiro, Cláudia; Ribeiro, Ana Rita; Maia, Alexandra S; Gonçalves, Virgínia M F; Tiritan, Maria Elizabeth

    2014-01-01

    Environmental samples include a wide variety of complex matrices, with low concentrations of analytes and presence of several interferences. Sample preparation is a critical step and the main source of uncertainties in the analysis of environmental samples, and it is usually laborious, high cost, time consuming, and polluting. In this context, there is increasing interest in developing faster, cost-effective, and environmentally friendly sample preparation techniques. Recently, new methods have been developed and optimized in order to miniaturize extraction steps, to reduce solvent consumption or become solventless, and to automate systems. This review attempts to present an overview of the fundamentals, procedure, and application of the most recently developed sample preparation techniques for the extraction, cleanup, and concentration of organic pollutants from environmental samples. These techniques include: solid phase microextraction, on-line solid phase extraction, microextraction by packed sorbent, dispersive liquid-liquid microextraction, and QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe).

  17. Appendices to report on DOE analytical laboratory capacity available to meet EM environmental sampling and analysis needs for FY 93-99

    International Nuclear Information System (INIS)

    1994-01-01

    The DOE Analytical Laboratory Capacity Study was conducted to give EM-263 current information about existing and future analytical capacities and capabilities of site laboratories within the DOE Complex. Each DOE site may have one or more analytical laboratories in operation. These facilities were established to support site missions such as production, research and development, and personnel and environmental monitoring. With changing site missions and the DOE directives for environmental monitoring and cleanup, these laboratories are either devoting or planning to devote resources to support EM activities. The DOE site laboratories represent a considerable amount of capital investment and analytical capability, capacity, and expertise that can be applied to support the EM mission. They not only provide cost-effective high-volume analytical laboratory services, but are also highly recognized analytical research and development centers. Several sites have already transferred their analytical capability from traditional production support to environmental monitoring and waste management support. A model was developed to determine the analytical capacity of all laboratories in the DOE Complex. The model was applied at nearly all the major laboratories and the results collected from these studies are summarized in this report

  18. Empirical insights and considerations for the OBT inter-laboratory comparison of environmental samples.

    Science.gov (United States)

    Kim, Sang-Bog; Roche, Jennifer

    2013-08-01

    Organically bound tritium (OBT) is an important tritium species that can be measured in most environmental samples, but has only recently been recognized as a species of tritium in these samples. Currently, OBT is not routinely measured by environmental monitoring laboratories around the world. There are no certified reference materials (CRMs) for environmental samples. Thus, quality assurance (QA), or verification of the accuracy of the OBT measurement, is not possible. Alternatively, quality control (QC), or verification of the precision of the OBT measurement, can be achieved. In the past, there have been differences in OBT analysis results between environmental laboratories. A possible reason for the discrepancies may be differences in analytical methods. Therefore, inter-laboratory OBT comparisons among the environmental laboratories are important and would provide a good opportunity for adopting a reference OBT analytical procedure. Due to the analytical issues, only limited information is available on OBT measurement. Previously conducted OBT inter-laboratory practices are reviewed and the findings are described. Based on our experiences, a few considerations were suggested for the international OBT inter-laboratory comparison exercise to be completed in the near future. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

  19. Ash contents of foodstuff samples in environmental radioactivity analysis

    International Nuclear Information System (INIS)

    Oikawa, Shinji; Ohta, Hiroshi; Hayano, Kazuhiko; Nonaka, Nobuhiro

    2004-01-01

    Statistical data of the ash content in various environmental samples obtained from an environmental radioactivity survey project commissioned by the Japanese government of Science and Technology Agency (at present Ministry of Education, Culture, Sports, Sciences and Technology) during the past 10 years are expressed for establishing a standard of ash content in environmental samples based on radioactivity analysis. The ash content for some kinds of environmental samples such as dietary food, milk, Japanese radish, spinach, fish, green tea and potato was reviewed in the light of statistical and stochastic viewpoints. For all of the samples reviewed in this paper, the coefficient of variation varied from 4.7% for milk to 36.3% for cabbage. Dietary food and milk samples were reviewed more than 1900 and 1400 samples, respectively. Especially, ash content of dietary food depended mainly on the dietary culture reflected on the period. However it showed an almost invariant distribution within 18.7% of coefficient of variation during the past 10 years. Pretreatment of environmental samples especially ashing processes are important from the viewpoint on environmental radioactivity analysis, which is one of the especial fields in analytical chemistry. Statistical reviewed data obtained in this paper may be useful for sample preparation. (author)

  20. Waste minimization in analytical chemistry through innovative sample preparation techniques

    International Nuclear Information System (INIS)

    Smith, L. L.

    1998-01-01

    Because toxic solvents and other hazardous materials are commonly used in analytical methods, characterization procedures result in significant and costly amount of waste. We are developing alternative analytical methods in the radiological and organic areas to reduce the volume or form of the hazardous waste produced during sample analysis. For the radiological area, we have examined high-pressure, closed-vessel microwave digestion as a way to minimize waste from sample preparation operations. Heated solutions of strong mineral acids can be avoided for sample digestion by using the microwave approach. Because reactivity increases with pressure, we examined the use of less hazardous solvents to leach selected contaminants from soil for subsequent analysis. We demonstrated the feasibility of this approach by extracting plutonium from a NET reference material using citric and tartaric acids with microwave digestion. Analytical results were comparable to traditional digestion methods, while hazardous waste was reduced by a factor often. We also evaluated the suitability of other natural acids, determined the extraction performance on a wider variety of soil types, and examined the extraction efficiency of other contaminants. For the organic area, we examined ways to minimize the wastes associated with the determination of polychlorinated biphenyls (PCBs) in environmental samples. Conventional methods for analyzing semivolatile organic compounds are labor intensive and require copious amounts of hazardous solvents. For soil and sediment samples, we have a method to analyze PCBs that is based on microscale extraction using benign solvents (e.g., water or hexane). The extraction is performed at elevated temperatures in stainless steel cells containing the sample and solvent. Gas chromatography-mass spectrometry (GC/MS) was used to quantitate the analytes in the isolated extract. More recently, we developed a method utilizing solid-phase microextraction (SPME) for natural

  1. Computer system for environmental sample analysis and data storage and analysis

    International Nuclear Information System (INIS)

    Brauer, F.P.; Fager, J.E.

    1976-01-01

    A mini-computer based environmental sample analysis and data storage system has been developed. The system is used for analytical data acquisition, computation, storage of analytical results, and tabulation of selected or derived results for data analysis, interpretation and reporting. This paper discussed the structure, performance and applications of the system

  2. Recent Trends in Microextraction Techniques Employed in Analytical and Bioanalytical Sample Preparation

    Directory of Open Access Journals (Sweden)

    Abuzar Kabir

    2017-12-01

    Full Text Available Sample preparation has been recognized as a major step in the chemical analysis workflow. As such, substantial efforts have been made in recent years to simplify the overall sample preparation process. Major focusses of these efforts have included miniaturization of the extraction device; minimizing/eliminating toxic and hazardous organic solvent consumption; eliminating sample pre-treatment and post-treatment steps; reducing the sample volume requirement; reducing extraction equilibrium time, maximizing extraction efficiency etc. All these improved attributes are congruent with the Green Analytical Chemistry (GAC principles. Classical sample preparation techniques such as solid phase extraction (SPE and liquid-liquid extraction (LLE are being rapidly replaced with emerging miniaturized and environmentally friendly techniques such as Solid Phase Micro Extraction (SPME, Stir bar Sorptive Extraction (SBSE, Micro Extraction by Packed Sorbent (MEPS, Fabric Phase Sorptive Extraction (FPSE, and Dispersive Liquid-Liquid Micro Extraction (DLLME. In addition to the development of many new generic extraction sorbents in recent years, a large number of molecularly imprinted polymers (MIPs created using different template molecules have also enriched the large cache of microextraction sorbents. Application of nanoparticles as high-performance extraction sorbents has undoubtedly elevated the extraction efficiency and method sensitivity of modern chromatographic analyses to a new level. Combining magnetic nanoparticles with many microextraction sorbents has opened up new possibilities to extract target analytes from sample matrices containing high volumes of matrix interferents. The aim of the current review is to critically audit the progress of microextraction techniques in recent years, which has indisputably transformed the analytical chemistry practices, from biological and therapeutic drug monitoring to the environmental field; from foods to phyto

  3. Environmental Safety and Health Analytical Laboratory, Pantex Plant, Amarillo, Texas. Final Environmental Assessment

    International Nuclear Information System (INIS)

    1995-06-01

    The US Department of Energy (DOE) has prepared an Environmental Assessment (EA) of the construction and operation of an Environmental Safety and Health (ES ampersand H) Analytical Laboratory and subsequent demolition of the existing Analytical Chemistry Laboratory building at Pantex Plant near Amarillo, Texas. In accordance with the Council on Environmental Quality requirements contained in 40 CFR 1500--1508.9, the Environmental Assessment examined the environmental impacts of the Proposed Action and discussed potential alternatives. Based on the analysis of impacts in the EA, conducting the proposed action, construction of an analytical laboratory and demolition of the existing facility, would not significantly effect the quality of the human environment within the meaning of the National Environmental Policy Act of 1969 (NEPA) and the Council on Environmental Quality regulations in 40 CFR 1508.18 and 1508.27

  4. Application of advanced nuclear and instrumental analytical techniques for characterisation of environmental materials

    International Nuclear Information System (INIS)

    Sudersanan, M.; Pawaskar, P.B.; Kayasth, S.R.; Kumar, S.C.

    2002-01-01

    Full text: Increasing realisation about the toxic effects of metal ions in environmental materials has given an impetus to research on analytical techniques for their characterization. The large number of analytes present at very low levels has necessitated the use of sensitive, selective and element specific techniques for their characterization. The concern about precision and accuracy on such analysis, which have socio-economic bearing, has emphasized the use of Certified Reference Materials and the use of multi-technique approach for the unambiguous characterization of analytes. The recent work carried out at Analytical Chemistry Division, BARC on these aspects is presented in this paper. Increasing use of fossil fuels has led to the generation of large quantities of fly ash which pose problems of safe disposal. The utilization of these materials for land filling is an attractive option but the presence of trace amounts of toxic metals like mercury, arsenic, lead etc may cause environmental problems. In view of the inhomogeneous nature of the material, efficient sample processing is an important factor, in addition to the validation of the results by the use of proper standards. Analysis was carried out on flyash samples received as reference materials and also as samples from commercial sources using a combination of both nuclear techniques like INAA and RNAA as well as other techniques like AAS, ICPAES, cold vapour AAS for mercury and hydride generation technique for arsenic. Similar analysis using nuclear techniques was employed for the characterization of air particulates. Biological materials often serve as sensitive indicator materials for pollution measurements. They are also employed for studies on the uptake of toxic metals like U, Th, Cd, Pb, Hg etc. The presence of large amounts of organic materials in them necessitate an appropriate sample dissolution procedure. In view of the possibility of loss of certain analytes like Cd, Hg, As, by high

  5. The Use and Abuse of Limits of Detection in Environmental Analytical Chemistry

    Directory of Open Access Journals (Sweden)

    Richard J. C. Brown

    2008-01-01

    Full Text Available The limit of detection (LoD serves as an important method performance measure that is useful for the comparison of measurement techniques and the assessment of likely signal to noise performance, especially in environmental analytical chemistry. However, the LoD is only truly related to the precision characteristics of the analytical instrument employed for the analysis and the content of analyte in the blank sample. This article discusses how other criteria, such as sampling volume, can serve to distort the quoted LoD artificially and make comparison between various analytical methods inequitable. In order to compare LoDs between methods properly, it is necessary to state clearly all of the input parameters relating to the measurements that have been used in the calculation of the LoD. Additionally, the article discusses that the use of LoDs in contexts other than the comparison of the attributes of analytical methods, in particular when reporting analytical results, may be confusing, less informative than quoting the actual result with an accompanying statement of uncertainty, and may act to bias descriptive statistics.

  6. Post-analytical stability of 23 common chemistry and immunochemistry analytes in incurred samples

    DEFF Research Database (Denmark)

    Nielsen, Betina Klint; Frederiksen, Tina; Friis-Hansen, Lennart

    2017-01-01

    BACKGROUND: Storage of blood samples after centrifugation, decapping and initial sampling allows ordering of additional blood tests. The pre-analytic stability of biochemistry and immunochemistry analytes has been studied in detail, but little is known about the post-analytical stability...... in incurred samples. METHODS: We examined the stability of 23 routine analytes on the Dimension Vista® (Siemens Healthineers, Denmark): 42-60 routine samples in lithium-heparin gel tubes (Vacutainer, BD, USA) were centrifuged at 3000×g for 10min. Immediately after centrifugation, initial concentration...... of analytes were measured in duplicate (t=0). The tubes were stored decapped at room temperature and re-analyzed after 2, 4, 6, 8 and 10h in singletons. The concentration from reanalysis were normalized to initial concentration (t=0). Internal acceptance criteria for bias and total error were used...

  7. PIXE - Analysis for environmental and biological samples

    International Nuclear Information System (INIS)

    Baptista, G.B.

    1980-04-01

    The usefulness and accuracy of PIXE as an analytical tool in the study of trace elements in environmental samples of the Brazilian Cerrado are discussed. The report lists actual and forthcoming publications resulting from the study. The mechanism of exchange of elements in solution in water to aerosols has been investigated. For details of the procedure the reader is referred to an earlier report

  8. Abstracts book of 4. Poznan Analytical Seminar on Modern Methods of Sample Preparation and Trace Amounts Determination of Elements

    International Nuclear Information System (INIS)

    1995-01-01

    The 4. Poznan Analytical Seminar on Modern Methods of Sample Preparation and Trace Amounts Determination of Elements has been held in Poznan 27-28 April 1995. The new versions of analytical methods have been presented for quantitative determination of trace elements in biological, environmental and geological materials. Also the number of special techniques for sample preparation enables achievement the best precision of analytical results have been shown and discussed

  9. Determination of technetium-99 in environmental samples: A review

    DEFF Research Database (Denmark)

    Shi, Keliang; Hou, Xiaolin; Roos, Per

    2012-01-01

    Due to the lack of a stable technetium isotope, and the high mobility and long half-life, 99Tc is considered to be one of the most important radionuclides in safety assessment of environmental radioactivity as well as nuclear waste management. 99Tc is also an important tracer for oceanographic...... research due to the high technetium solubility in seawater as TcO4−. A number of analytical methods, using chemical separation combined with radiometric and mass spectrometric measurement techniques, have been developed over the past decades for determination of 99Tc in different environmental samples....... This article summarizes and compares recently reported chemical separation procedures and measurement methods for determination of 99Tc. Due to the extremely low concentration of 99Tc in environmental samples, the sample preparation, pre-concentration, chemical separation and purification for removal...

  10. Bias Assessment of General Chemistry Analytes using Commutable Samples.

    Science.gov (United States)

    Koerbin, Gus; Tate, Jillian R; Ryan, Julie; Jones, Graham Rd; Sikaris, Ken A; Kanowski, David; Reed, Maxine; Gill, Janice; Koumantakis, George; Yen, Tina; St John, Andrew; Hickman, Peter E; Simpson, Aaron; Graham, Peter

    2014-11-01

    Harmonisation of reference intervals for routine general chemistry analytes has been a goal for many years. Analytical bias may prevent this harmonisation. To determine if analytical bias is present when comparing methods, the use of commutable samples, or samples that have the same properties as the clinical samples routinely analysed, should be used as reference samples to eliminate the possibility of matrix effect. The use of commutable samples has improved the identification of unacceptable analytical performance in the Netherlands and Spain. The International Federation of Clinical Chemistry and Laboratory Medicine (IFCC) has undertaken a pilot study using commutable samples in an attempt to determine not only country specific reference intervals but to make them comparable between countries. Australia and New Zealand, through the Australasian Association of Clinical Biochemists (AACB), have also undertaken an assessment of analytical bias using commutable samples and determined that of the 27 general chemistry analytes studied, 19 showed sufficiently small between method biases as to not prevent harmonisation of reference intervals. Application of evidence based approaches including the determination of analytical bias using commutable material is necessary when seeking to harmonise reference intervals.

  11. Some analytical aspects about determination of Sr89 and Sr90 in environmental samples

    International Nuclear Information System (INIS)

    Gasco, C.; Alvarez Garcia, A.

    1988-01-01

    Some problems about determination of Sr 89 and Sr 90 in environmental samples have been studied. The main difficulties are due to the wide range in the concentration of their components and the contents of chemical and radiochemical interferent elements. The behaviour of strontium on ion exchange resin has been described by some experiments in various media: aqueous media, calcium concentration and matrix variable. The differences of alkaline-earth nitrate and carbonate solubilities have been analyzed in nitric acid. The chemical recovery in environmental samples has been determined. (Author)

  12. Analytical and environmental aspects of the flame retardant tetrabromobisphenol-A and its derivatives.

    Science.gov (United States)

    Covaci, Adrian; Voorspoels, Stefan; Abdallah, Mohamed Abou-Elwafa; Geens, Tinne; Harrad, Stuart; Law, Robin J

    2009-01-16

    The present article reviews the available literature on the analytical and environmental aspects of tetrabromobisphenol-A (TBBP-A), a currently intensively used brominated flame retardant (BFR). Analytical methods, including sample preparation, chromatographic separation, detection techniques, and quality control are discussed. An important recent development in the analysis of TBBP-A is the growing tendency for liquid chromatographic techniques. At the detection stage, mass-spectrometry is a well-established and reliable technology in the identification and quantification of TBBP-A. Although interlaboratory exercises for BFRs have grown in popularity in the last 10 years, only a few participating laboratories report concentrations for TBBP-A. Environmental levels of TBBP-A in abiotic and biotic matrices are low, probably due to the major use of TBBP-A as reactive FR. As a consequence, the expected human exposure is low. This is in agreement with the EU risk assessment that concluded that there is no risk for humans concerning TBBP-A exposure. Much less analytical and environmental information exists for the various groups of TBBP-A derivatives which are largely used as additive flame retardants.

  13. Transuranium analysis methodologies for biological and environmental samples

    International Nuclear Information System (INIS)

    Wessman, R.A.; Lee, K.D.; Curry, B.; Leventhal, L.

    1978-01-01

    Analytical procedures for the most abundant transuranium nuclides in the environment (i.e., plutonium and, to a lesser extent, americium) are available. There is a lack of procedures for doing sequential analysis for Np, Pu, Am, and Cm in environmental samples, primarily because of current emphasis on Pu and Am. Reprocessing requirements and waste disposal connected with the fuel cycle indicate that neptunium and curium must be considered in environmental radioactive assessments. Therefore it was necessary to develop procedures that determine all four of these radionuclides in the environment. The state of the art of transuranium analysis methodology as applied to environmental samples is discussed relative to different sample sources, such as soil, vegetation, air, water, and animals. Isotope-dilution analysis with 243 Am ( 239 Np) and 236 Pu or 242 Pu radionuclide tracers is used. Americium and curium are analyzed as a group, with 243 Am as the tracer. Sequential extraction procedures employing bis(2-ethyl-hexyl)orthophosphoric acid (HDEHP) were found to result in lower yields and higher Am--Cm fractionation than ion-exchange methods

  14. Rapid and Automated Determination of Plutonium and Neptunium in Environmental Samples

    DEFF Research Database (Denmark)

    Qiao, Jixin

    This thesis presents improved analytical methods for rapid and automated determination of plutonium and neptunium in environmental samples using sequential injection (SI) based chromatography and inductively coupled plasma mass spectrometry (ICP-MS). The progress of methodology development...... and optimization for rapid determination of plutonium in environmental samples using SIextraction chromatography prior to inductively coupled plasma mass spectrometry (Paper III); (3) Development of an SI-chromatographic method for simultaneous determination of plutonium and neptunium in environmental samples...... for rapid and simultaneous determination of plutonium and neptunium within an SI system (Paper VI). The results demonstrate that the developed methods in this study are reliable and efficient for accurate assays of trace levels of plutonium and neptunium as demanded in different situations including...

  15. Recovery of environmental analytes from clays and soils by supercritical fluid extracting/gas chromatography

    International Nuclear Information System (INIS)

    Emery, A.P.; Chesler, S.N.; MacCrehan, W.A.

    1992-01-01

    This paper reports on Supercritical Fluid Extraction (SFE) which promises to provide rapid extractions of organic analytes from environmental sample types without the use of hazardous solvents. In addition, SFE protocols using commercial instrumentation can be automated lowering analysis costs. Because of these benefits, we are investigating SFE as an alternative to the solvent extraction (eg. Soxhlet and sonication) techniques required in many EPA test procedures. SFE, using non-polar carbon dioxide as well as more polar supercritical fluids, was used to determine n-alkane hydrocarbons and polynuclear aromatic hydrocarbons (PAHs) in solid samples. The extraction behavior of these analyte classes from environmentally-contaminated soil matrices and model soil and clay matrices was investigated using a SFE apparatus in which the extracted analytes were collected on a solid phase trap and then selectively eluted with a solvent. The SFE conditions for quantitative recovery of n-alkane hydrocarbons in diesel fuel from a series of clays and soils were determined using materials prepared at the 0.02% level with diesel fuel oil in order to simplify analyte collection and analysis after extraction. The effect of extraction parameters including temperature, fluid flow rate and modifier addition were investigated by monitoring the amount of diesel fuel extracted as a function of time

  16. Design of a Clean Room for Quality Control of an Environmental Sampling in KINAC

    International Nuclear Information System (INIS)

    Yoon, Jongho; Ahn, Gil Hoon; Seo, Hana; Han, Kitek; Park, Il Jin

    2014-01-01

    The objective of environmental sampling and analysis for safeguards is to characterize the nuclear materials handled and the activities conducted at the specific locations. The KINAC is responsible for the conclusions drawn from the analytical results provided by the analytical laboratories. To assure the KINAC of the continuity of the quality of the analytical results provided by the laboratories, the KINAC will implement a quality control(QC) programme. One of the QC programme is to prepare QC samples. The establishment of a clean room is needed to handle QC samples due to stringent control of contamination. The KINAC designed a clean facility with cleanliness of ISO Class 6, the Clean Room for Estimation and Assay of trace Nuclear materials(CREAN) to meet conflicting requirements of a clean room and for handling of nuclear materials according to Korean laws. The clean room will be expected to acquire of a radiation safety license under these conditions in this year and continue to improve it. The construction of the CREAN facility will be completed by the middle of 2015. In terms of QC programme, the establishment of a clean room is essential and will be not only very helpful for setting of quality control system for the national environmental sampling programme but also be applied for the environmental sample analysis techniques to the nuclear forensics

  17. Fluoroquinolone antibiotics in environmental waters: sample preparation and determination.

    Science.gov (United States)

    Speltini, Andrea; Sturini, Michela; Maraschi, Federica; Profumo, Antonella

    2010-04-01

    The aim of this review is to provide a general overview on the analytical methods proposed in the last decade for trace fluoroquinolone (FQ) determination in environmental waters. A large number of studies have been developed on this topic in reason of the importance of their monitoring in the studies of environmental mobility and potential degradation pathways. Every step of the analysis has been carefully considered, with a particular attention to sample preparation, in relationship with the problems involved in the analysis of real matrices. The different strategies to minimise interference from organic matter and to achieve optimal sensitivity, especially important in those samples with lower FQ concentrations, were also highlighted. Results and progress in this field have been described and critically commented. Moreover, a worldwide overview on the presence of FQs in the environmental waters has been reported.

  18. Neutron activation analysis as analytical tool of environmental issue

    International Nuclear Information System (INIS)

    Otoshi, Tsunehiko

    2004-01-01

    Neutron activation analysis (NAA) ia applicable to the sample of wide range of research fields, such as material science, biology, geochemistry and so on. However, respecting the advantages of NAA, a sample with small amounts or a precious sample is the most suitable samples for NAA, because NAA is capable of trace analysis and non-destructive determination. In this paper, among these fields, NAA of atmospheric particulate matter (PM) sample is discussed emphasizing on the use of obtained data as an analytical tool of environmental issue. Concentration of PM in air is usually very low, and it is not easy to get vast amount of sample even using a high volume air sampling devise. Therefore, high sensitive NAA is suitable to determine elements in PM samples. Main components of PM is crust oriented silicate, and so on in rural/remote area, and carbonic materials and heavy metals are concentrated in PM in urban area, because of automobile exhaust and other anthropogenic emission source. Elemental pattern of PM reflects a condition of air around the monitoring site. Trends of air pollution can be traced by periodical monitoring of PM by NAA method. Elemental concentrations in air change by season. For example, crustal elements increase in dry season, and sea salts components increase their concentration when wind direction from sea is dominant. Elements that emitted from anthropogenic sources are mainly contained in fine portion of PM, and increase their concentration during winter season, when emission from heating system is high and air is stable. For further analysis and understanding of environmental issues, indicator elements for various emission sources, and elemental concentration ratios of some environmental samples and source portion assignment techniques are useful. (author)

  19. Ensuring comparability of data generated by multiple analytical laboratories for environmental decision making at the Fernald Environmental Management Project

    International Nuclear Information System (INIS)

    Sutton, C.; Campbell, B.A.; Danahy, R.J.; Dugan, T.A.; Tomlinson, F.K.

    1994-01-01

    The Fernald Environmental Management Project is a US Department of Energy (DOE)-owned facility located 17 miles northwest of Cincinnati, Ohio. From 1952 until 1989, the Fernald site provided high-purity uranium metal products to support US defense programs. In 1989 the mission of Fernald changed from one of uranium production to one of environmental restoration. At Fernald, multiple functional programs require analytical data. Inorganic and organic data for these programs are currently generated by seven laboratories, while radiochemical data are being obtained from six laboratories. Quality Assurance (QA) and Quality Control (QC) programs have been established to help ensure comparability of data generated by multiple laboratories at different times. The quality assurance program for organic and inorganic measurements specifies which analytical methodologies and sample preparation procedures are to be used based on analyte class, sample matrix, and data quality requirements. In contrast, performance specifications have been established for radiochemical analyses. A blind performance evaluation program for all laboratories, both on-site and subcontracted commercial laboratories, provides continuous feedback on data quality. The necessity for subcontractor laboratories to participate in the performance evaluation program is a contractual requirement. Similarly, subcontract laboratories are contractually required to generate data which meet radiochemical performance specifications. The Fernald on-site laboratory must also fulfill these requirements

  20. Review of Analytes of Concern and Sample Methods for Closure of DOE High Level Waste Storage Tanks

    International Nuclear Information System (INIS)

    Thomas, T.R.

    2002-01-01

    Sampling residual waste after tank cleaning and analysis for analytes of concern to support closure and cleaning targets of large underground tanks used for storage of legacy high level radioactive waste (HLW) at Department of Energy (DOE) sites has been underway since about 1995. The DOE Tanks Focus Area (TFA) has been working with DOE tank sites to develop new sampling plans, and sampling methods for assessment of residual waste inventories. This paper discusses regulatory analytes of concern, sampling plans, and sampling methods that support closure and cleaning target activities for large storage tanks at the Hanford Site, the Savannah River Site (SRS), the Idaho National Engineering and Environmental Laboratory (INEEL), and the West Valley Demonstration Project (WVDP)

  1. Quantifying the measurement uncertainty of results from environmental analytical methods.

    Science.gov (United States)

    Moser, J; Wegscheider, W; Sperka-Gottlieb, C

    2001-07-01

    The Eurachem-CITAC Guide Quantifying Uncertainty in Analytical Measurement was put into practice in a public laboratory devoted to environmental analytical measurements. In doing so due regard was given to the provisions of ISO 17025 and an attempt was made to base the entire estimation of measurement uncertainty on available data from the literature or from previously performed validation studies. Most environmental analytical procedures laid down in national or international standards are the result of cooperative efforts and put into effect as part of a compromise between all parties involved, public and private, that also encompasses environmental standards and statutory limits. Central to many procedures is the focus on the measurement of environmental effects rather than on individual chemical species. In this situation it is particularly important to understand the measurement process well enough to produce a realistic uncertainty statement. Environmental analytical methods will be examined as far as necessary, but reference will also be made to analytical methods in general and to physical measurement methods where appropriate. This paper describes ways and means of quantifying uncertainty for frequently practised methods of environmental analysis. It will be shown that operationally defined measurands are no obstacle to the estimation process as described in the Eurachem/CITAC Guide if it is accepted that the dominating component of uncertainty comes from the actual practice of the method as a reproducibility standard deviation.

  2. Sampling Large Graphs for Anticipatory Analytics

    Science.gov (United States)

    2015-05-15

    low. C. Random Area Sampling Random area sampling [8] is a “ snowball ” sampling method in which a set of random seed vertices are selected and areas... Sampling Large Graphs for Anticipatory Analytics Lauren Edwards, Luke Johnson, Maja Milosavljevic, Vijay Gadepally, Benjamin A. Miller Lincoln...systems, greater human-in-the-loop involvement, or through complex algorithms. We are investigating the use of sampling to mitigate these challenges

  3. Analytical Chemistry Division's sample transaction system

    International Nuclear Information System (INIS)

    Stanton, J.S.; Tilson, P.A.

    1980-10-01

    The Analytical Chemistry Division uses the DECsystem-10 computer for a wide range of tasks: sample management, timekeeping, quality assurance, and data calculation. This document describes the features and operating characteristics of many of the computer programs used by the Division. The descriptions are divided into chapters which cover all of the information about one aspect of the Analytical Chemistry Division's computer processing

  4. Radioactive kryptonates in the analysis of environmental samples

    International Nuclear Information System (INIS)

    Tolgyessy, J.

    1986-01-01

    The term ''radioactive Kryptonates'' is used for substances into which atoms or ions of the radioactive nuclide 85 Kr are incorporated. The basis of the use of radioactive Kryptonates in analytical chemistry is that during a chemical reaction the crystalline lattice of the kryptonated carrier is destroyed, the carrier consumed, and the radioactive krypton released (radio-release method). Analysis can be made with a calibration curve or by comparison with a standard. Radio-release methods with the aid of radioactive Kryptonates as analytical reagents are very useful for the analysis of environmental samples, e.g. for the determination of air pollutants (ozone, sulphur dioxide, fluorine, hydrogen fluoride, mercury); and water pollutants (oxygen, dichromate, vanadium, hydrochloric acid, sulphur dioxide). (author)

  5. Eco-analytical Methodology in Environmental Problems Monitoring

    Science.gov (United States)

    Agienko, M. I.; Bondareva, E. P.; Chistyakova, G. V.; Zhironkina, O. V.; Kalinina, O. I.

    2017-01-01

    Among the problems common to all mankind, which solutions influence the prospects of civilization, the problem of ecological situation monitoring takes very important place. Solution of this problem requires specific methodology based on eco-analytical comprehension of global issues. Eco-analytical methodology should help searching for the optimum balance between environmental problems and accelerating scientific and technical progress. The fact that Governments, corporations, scientists and nations focus on the production and consumption of material goods cause great damage to environment. As a result, the activity of environmentalists is developing quite spontaneously, as a complement to productive activities. Therefore, the challenge posed by the environmental problems for the science is the formation of geo-analytical reasoning and the monitoring of global problems common for the whole humanity. So it is expected to find the optimal trajectory of industrial development to prevent irreversible problems in the biosphere that could stop progress of civilization.

  6. Three-phase double-arc plasma for spectrochemical analysis of environmental samples.

    Science.gov (United States)

    Mohamed, M M; Ghatass, Z F; Shalaby, E A; Kotb, M M; El-Raey, M

    2000-12-01

    A new instrument, which uses a three-phase current to support a double-arc argon plasma torch for evaporation, atomization and excitation of solid or powder samples, is described. The sampling arc is ignited between the first and second electrode while the excitation arc is ignited between the second and third electrode. Aerosol generated from the sample (first electrode) is swept by argon gas, through a hole in the second electrode (carbon tubing electrode), into the excitation plasma. A tangential stream of argon gas is introduced through an inlet orifice as a coolant gas for the second electrode. This gas stream forces the excitation arc discharge to rotate reproducibly around the electrode surface. Discharge rotation increases the stability of the excitation plasma. Spectroscopic measurements are made directly in the current-carrying region of the excitation arc. An evaluation of each parameter influencing the device performance was performed. Analytical calibration curves were obtained for Fe, Al, K, and Pb. Finally, the present technique was applied for the analysis of environmental samples. The present method appears to have significant, low cost analytical utility for environmental measurements.

  7. Analytical laboratory quality assurance guidance in support of EM environmental sampling and analysis activities

    International Nuclear Information System (INIS)

    1994-05-01

    This document introduces QA guidance pertaining to design and implementation of laboratory procedures and processes for collecting DOE Environmental Restoration and Waste Management (EM) ESAA (environmental sampling and analysis activities) data. It addresses several goals: identifying key laboratory issues and program elements to EM HQ and field office managers; providing non-prescriptive guidance; and introducing environmental data collection program elements for EM-263 assessment documents and programs. The guidance describes the implementation of laboratory QA elements within a functional QA program (development of the QA program and data quality objectives are not covered here)

  8. Green Aspects of Techniques for the Determination of Currently Used Pesticides in Environmental Samples

    OpenAIRE

    Maciej Tankiewicz; Jacek Namieśnik; Jolanta Stocka; Marek Biziuk

    2011-01-01

    Pesticides are among the most dangerous environmental pollutants because of their stability, mobility and long-term effects on living organisms. Their presence in the environment is a particular danger. It is therefore crucial to monitor pesticide residues using all available analytical methods. The analysis of environmental samples for the presence of pesticides is very difficult: the processes involved in sample preparation are labor-intensive and time-consuming. To date, it has been standa...

  9. Determination of Glucocorticoids in UPLC-MS in Environmental Samples from an Occupational Setting

    Directory of Open Access Journals (Sweden)

    Enrico Oddone

    2015-01-01

    Full Text Available Occupational exposures to glucocorticoids are still a neglected issue in some work environments, including pharmaceutical plants. We developed an analytical method to quantify simultaneously 21 glucocorticoids using UPLC coupled with mass spectrometry to provide a basis to carry out environmental monitoring. Samples were taken from air, hand-washing tests, pad-tests and wipe-tests. This paper reports the contents of the analytical methodology, along with the results of this extensive environmental and personal monitoring of glucocorticoids. The method in UPLC-MS turned out to be suitable and effective for the aim of the study. Wipe-test and pad-test desorption was carried out using 50 mL syringes, a simple technique that saves time without adversely affecting analyte recovery. Results showed a widespread environmental pollution due to glucocorticoids. This is of particular concern. Evaluation of the dose absorbed by each worker and identification of a biomarker for occupational exposure will contribute to assessment and prevention of occupational exposure.

  10. Performance evaluation of the food and environmental monitoring radio-analytical laboratory in Ghana

    International Nuclear Information System (INIS)

    Agyeman, Lilian Ataa

    2016-06-01

    Since the establishment of the Radiation Protection Institute’s Food and Environmental Laboratory in 1988, there has never been any thorough evaluation of the activities of the facility to provide assurance of the quality of analytical results produced by the laboratory. The objective of this study, therefore, was to assess the performance level of the Food and Environmental monitoring laboratory with respect to the requirements for a standard analytical laboratory (IAEA, 1989) and ISO 17025. The study focused on the performance of the Gamma Spectrometry laboratory of the Radiation Protection Institute, Ghana Atomic Energy Commission which has been involved in monitoring of radionuclides in food and environmental samples. In doing that, data from 1988 to 2015 was reviewed to ascertain whether the Laboratory has being performing as required in providing quality results on food and environmental samples measured. Besides this data (records kept), the evaluation also covered some Technical Quality Control measures, such as Energy and Efficiency Calibration, that need to be put in place for such laboratories. The laboratory meets almost all conditions and equipment requirements of IAEA (1989), however the laboratory falls short of the management requirements of ISO 17025. Based on the results it was recommended, among others, that management of the laboratory should ensure there are procedures for how calibration and testing is performed for different types of equipment and also the competence of all who operate specific equipment, perform tests, evaluate results and sign test reports ensured. (au)

  11. Environmental Stewardship: A Conceptual Review and Analytical Framework

    Science.gov (United States)

    Bennett, Nathan J.; Whitty, Tara S.; Finkbeiner, Elena; Pittman, Jeremy; Bassett, Hannah; Gelcich, Stefan; Allison, Edward H.

    2018-04-01

    There has been increasing attention to and investment in local environmental stewardship in conservation and environmental management policies and programs globally. Yet environmental stewardship has not received adequate conceptual attention. Establishing a clear definition and comprehensive analytical framework could strengthen our ability to understand the factors that lead to the success or failure of environmental stewardship in different contexts and how to most effectively support and enable local efforts. Here we propose such a definition and framework. First, we define local environmental stewardship as the actions taken by individuals, groups or networks of actors, with various motivations and levels of capacity, to protect, care for or responsibly use the environment in pursuit of environmental and/or social outcomes in diverse social-ecological contexts. Next, drawing from a review of the environmental stewardship, management and governance literatures, we unpack the elements of this definition to develop an analytical framework that can facilitate research on local environmental stewardship. Finally, we discuss potential interventions and leverage points for promoting or supporting local stewardship and future applications of the framework to guide descriptive, evaluative, prescriptive or systematic analysis of environmental stewardship. Further application of this framework in diverse environmental and social contexts is recommended to refine the elements and develop insights that will guide and improve the outcomes of environmental stewardship initiatives and investments. Ultimately, our aim is to raise the profile of environmental stewardship as a valuable and holistic concept for guiding productive and sustained relationships with the environment.

  12. Environmental Stewardship: A Conceptual Review and Analytical Framework.

    Science.gov (United States)

    Bennett, Nathan J; Whitty, Tara S; Finkbeiner, Elena; Pittman, Jeremy; Bassett, Hannah; Gelcich, Stefan; Allison, Edward H

    2018-04-01

    There has been increasing attention to and investment in local environmental stewardship in conservation and environmental management policies and programs globally. Yet environmental stewardship has not received adequate conceptual attention. Establishing a clear definition and comprehensive analytical framework could strengthen our ability to understand the factors that lead to the success or failure of environmental stewardship in different contexts and how to most effectively support and enable local efforts. Here we propose such a definition and framework. First, we define local environmental stewardship as the actions taken by individuals, groups or networks of actors, with various motivations and levels of capacity, to protect, care for or responsibly use the environment in pursuit of environmental and/or social outcomes in diverse social-ecological contexts. Next, drawing from a review of the environmental stewardship, management and governance literatures, we unpack the elements of this definition to develop an analytical framework that can facilitate research on local environmental stewardship. Finally, we discuss potential interventions and leverage points for promoting or supporting local stewardship and future applications of the framework to guide descriptive, evaluative, prescriptive or systematic analysis of environmental stewardship. Further application of this framework in diverse environmental and social contexts is recommended to refine the elements and develop insights that will guide and improve the outcomes of environmental stewardship initiatives and investments. Ultimately, our aim is to raise the profile of environmental stewardship as a valuable and holistic concept for guiding productive and sustained relationships with the environment.

  13. Intercalibration of analytical methods on marine environmental samples. Results of MEDPOL-II exercise for the intercalibration of chlorinated hydrocarbon measurements on mussel homogenate (MA-M-2/OC)

    International Nuclear Information System (INIS)

    1986-10-01

    Mussels have been considered as good indicators of chlorinated hydrocarbon pollution of the marine environment and this led to the development of mussel watch programmes in many countries in the late seventies. These intercalibration exercises were arranged in order to increase the quality of analytical capabilities of environmental laboratories. The samples MA-M-2/0C of Mediterranean mussels with chlorinated hydrocarbon content were checked by 27 laboratories. It was judged highly suitable for these laboratories to have at their disposal a reference material made of mussel tissue with robust estimations of the true values with respect to several chlorinated hydrocarbons. Such a material would allow chemists to check the validity of new analytical procedures

  14. Environmental sample banking-research and methodology

    International Nuclear Information System (INIS)

    Becker, D.A.

    1976-01-01

    The National Bureau of Standards (NBS), in cooperation with the Environment Protection Agency and the National Science Foundation, is engaged in a research program establishing methodology for environmental sample banking. This program is aimed toward evaluating the feasibility of a National Environment Specimen Bank (NESB). The capability for retrospective chemical analyses to evaluate changes in our environment would provide useful information. Much of this information could not be obtained using data from previously analyzed samples. However, to assure validity for these stored samples, they must be sampled, processed and stored under rigorously evaluated, controlled and documented conditions. The program currently under way in the NBS Analytical Chemistry Division has 3 main components. The first is an extension survey of available literature concerning problems of contamination, losses and storage. The components of interest include trace elements, pesticides, other trace organics (PCBs, plasticizers, etc.), radionuclides and microbiological species. The second component is an experimental evaluation of contamination and losses during sampling and sample handling. Of particular interest here is research into container cleaning methodology for trace elements, with respect to adsorption, desorption, leaching and partial dissolution by various sample matrices. The third component of this program is an evaluation of existing methodology for long-term sample storage

  15. 40 CFR 141.22 - Turbidity sampling and analytical requirements.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Turbidity sampling and analytical... § 141.22 Turbidity sampling and analytical requirements. The requirements in this section apply to... the water distribution system at least once per day, for the purposes of making turbidity measurements...

  16. Screening of IAEA environmental samples for fissile material content

    International Nuclear Information System (INIS)

    Hembree, Doyle M. Jr.; Carter, Joel A.; Devault, Gerald L.; Whitaker, J. Michael; Glasgow, David

    2001-01-01

    Full text: Analysis of environmental samples for the International Atomic Energy Agency (IAEA) Strengthened Safeguards Systems program requires that stringent measures be taken to control contamination. To facilitate contamination control, it is extremely useful to have some estimate of the fissile content of a given sample prior to beginning sample preparation and analysis. This is particularly true for laboratories that employ clean rooms during sample preparation. A review of the analytical results for samples submitted between January 1, 1999 and September 1, 2000 revealed that the total uranium content values ranged from 0.2 to greater than 500,000 ng/sample. Poor estimates of the uranium or plutonium content in the samples have caused some of the laboratories in the IAEA Network of Analytical Laboratories (NWAL) to experience clean laboratory contamination, sample cross contamination, and non-ideal uranium spike additions. This has led to significant increases in analysis costs (e.g., recertification of clean rooms after removing contamination, and rerunning samples) and degradation in data quality. A number of methods have been proposed for screening environmental samples for fissile material content, including gamma spectrometry, x-ray fluorescence, kinetic phosphorimetry (KPA), and inductively coupled plasma-mass spectrometry (ICP-MS). Gamma spectrometry and x-ray fluorescence are suitable for screening samples with microgram or greater quantities of uranium. ICP-MS and KPA are used successfully in some DOE NWAL laboratories to screen environmental samples. A neutron activation analysis (NAA) method that offers numerous advantages over other screening techniques for environmental samples has recently been proposed. Fissile materials such as 239 Pu and 235 U can be made to undergo fission in the intense neutron field to which they are exposed during neutron activation analysis (NAA). Some of the fission products emit neutrons referred to as 'delayed

  17. Simple analytical technique for liquid scintillation counting of environmental carbon-14 using gel suspension method

    International Nuclear Information System (INIS)

    Okai, Tomio; Wakabayashi, Genichiro; Nagao, Kenjiro; Matoba, Masaru; Ohura, Hirotaka; Momoshima, Noriyuki; Kawamura, Hidehisa

    2000-01-01

    A simple analytical technique for liquid scintillation counting of environmental 14 C was developed. Commercially available gelling agent, N-lauroyl-L -glutamic -α,γ-dibutylamide, was used for the gel-formation of the samples (gel suspension method) and for the subsequent liquid scintillation counting of 14 C in the form of CaCO 3 . Our procedure for sample preparation is much simpler than that of the conventional methods and requires no special equipment. Self absorption, stability and reproducibility of gel suspension samples were investigated in order to evaluate the characteristics of the gel suspension method for 14 C activity measurement. The self absorption factor is about 70% and slightly decrease as CaCO 3 weight increase. This is considered to be mainly due to the absorption of β-rays and scintillation light by the CaCO 3 sample itself. No change of the counting rate for the gel suspension sample was observed for more than 2 years after the sample preparation. Four samples were used for checking the reproducibility of the sample preparation method. The same values were obtained for the counting rate of 24 C activity within the counting error. No change of the counting rate was observed for the 're-gelated' sample. These results show that the gel suspension method is appropriate for the 14 C activity measurement by the liquid scintillation counting method and useful for a long-term preservation of the sample for repeated measurement. The above analytical technique was applied to actual environmental samples in Fukuoka prefecture, Japan. Results obtained were comparable with those by other researchers and appear to be reasonable. Therefore, the newly developed technique is useful for the routine monitoring of environmental 14 C. (author)

  18. Determination and interpretation of environmental water samples contaminated by uranium mining activities

    International Nuclear Information System (INIS)

    Meinrath, G.; Volke, P.; Helling, C.; Merkel, B.J.; Dudel, E.G.

    1999-01-01

    Interpretation of environmental behavior of uranium is based on several steps of data analysis and statistical inference. First step is sampling and analyzing of uranium in field samples by routine laboratory methods. Such methods have to fulfill multiple requirements like robustness, efficiency, low detection limit and precision. A comparison of different approaches in assigning uncertainty to experimentally obtained analytical data shows that classical error estimation is not significantly inferior to more sophisticated modern techniques like inverse regression or orthogonal regression. A second step is the correlation of analytical data with current state of insight into environmental behavior of uranium. Such a correlation furthers the choice of adequate geochemical models and quality of geochemical data base for subsequent detailed analysis, e.g. by geochemical modeling. An appraisal of the individual steps in this complex analysis is given on the basis of statistical procedures for calibration and an E H -pH diagram of uranium for atmospheric conditions. (orig.)

  19. Self-attenuation of gamma rays during radioactivity concentration analysis of environmental samples

    International Nuclear Information System (INIS)

    Watson, D.; Dharmasiri, J.; Akber, R.

    2001-01-01

    Gamma spectroscopy using HPGe detector systems is a readily used technique for routine analysis of radioactivity in environmental samples. The systems are generally calibrated using standards of known radioactivity and composition. Radioactivity in environmental samples is generally distributed in the bulk of the material. When a sample of finite thickness is analysed through gamma spectroscopy, a proportion of the gamma rays emitted from the sample is either stopped or scattered from the sample material itself. These processes of self-absorption and self-attenuation depend upon the physical and elemental composition of the sample and the energy of the gamma radiation. Since environmental samples vary in composition, instrument calibration using a fixed matrix composition may not be valid for a diversity of samples. We selected and analysed five sample matrices to investigate the influence of self-absorption and self-attenuation in environmental samples. Our selection consisted of bentonite and kaolin representing clay, quartz representing silica, ash representing prepared biota, and analytical grade MnO 2 representing a co-precipitant used for extractive radioactivity from aqueous samples. Our findings show that within 5% of uncertainty the silica based standards can be used to cover the environmental samples of varying clay (silica content). The detection efficiency for ash and MnO 2 could be different particularly in the 30 - 100 keV energy range. The differences in sample behaviour can be explained on the basis of atomic number, mass number and density

  20. Moving your laboratories to the field – Advantages and limitations of the use of field portable instruments in environmental sample analysis

    Energy Technology Data Exchange (ETDEWEB)

    Gałuszka, Agnieszka, E-mail: Agnieszka.Galuszka@ujk.edu.pl [Geochemistry and the Environment Division, Institute of Chemistry, Jan Kochanowski University, 15G Świętokrzyska St., 25-406 Kielce (Poland); Migaszewski, Zdzisław M. [Geochemistry and the Environment Division, Institute of Chemistry, Jan Kochanowski University, 15G Świętokrzyska St., 25-406 Kielce (Poland); Namieśnik, Jacek [Department of Analytical Chemistry, Chemical Faculty, Gdańsk University of Technology (GUT), 11/12 G. Narutowicz St., 80-233 Gdańsk (Poland)

    2015-07-15

    The recent rapid progress in technology of field portable instruments has increased their applications in environmental sample analysis. These instruments offer a possibility of cost-effective, non-destructive, real-time, direct, on-site measurements of a wide range of both inorganic and organic analytes in gaseous, liquid and solid samples. Some of them do not require the use of reagents and do not produce any analytical waste. All these features contribute to the greenness of field portable techniques. Several stationary analytical instruments have their portable versions. The most popular ones include: gas chromatographs with different detectors (mass spectrometer (MS), flame ionization detector, photoionization detector), ultraviolet–visible and near-infrared spectrophotometers, X-ray fluorescence spectrometers, ion mobility spectrometers, electronic noses and electronic tongues. The use of portable instruments in environmental sample analysis gives a possibility of on-site screening and a subsequent selection of samples for routine laboratory analyses. They are also very useful in situations that require an emergency response and for process monitoring applications. However, quantification of results is still problematic in many cases. The other disadvantages include: higher detection limits and lower sensitivity than these obtained in laboratory conditions, a strong influence of environmental factors on the instrument performance and a high possibility of sample contamination in the field. This paper reviews recent applications of field portable instruments in environmental sample analysis and discusses their analytical capabilities. - Highlights: • Field portable instruments are widely used in environmental sample analysis. • Field portable instruments are indispensable for analysis in emergency response. • Miniaturization of field portable instruments reduces resource consumption. • In situ analysis is in agreement with green analytical chemistry

  1. Moving your laboratories to the field – Advantages and limitations of the use of field portable instruments in environmental sample analysis

    International Nuclear Information System (INIS)

    Gałuszka, Agnieszka; Migaszewski, Zdzisław M.; Namieśnik, Jacek

    2015-01-01

    The recent rapid progress in technology of field portable instruments has increased their applications in environmental sample analysis. These instruments offer a possibility of cost-effective, non-destructive, real-time, direct, on-site measurements of a wide range of both inorganic and organic analytes in gaseous, liquid and solid samples. Some of them do not require the use of reagents and do not produce any analytical waste. All these features contribute to the greenness of field portable techniques. Several stationary analytical instruments have their portable versions. The most popular ones include: gas chromatographs with different detectors (mass spectrometer (MS), flame ionization detector, photoionization detector), ultraviolet–visible and near-infrared spectrophotometers, X-ray fluorescence spectrometers, ion mobility spectrometers, electronic noses and electronic tongues. The use of portable instruments in environmental sample analysis gives a possibility of on-site screening and a subsequent selection of samples for routine laboratory analyses. They are also very useful in situations that require an emergency response and for process monitoring applications. However, quantification of results is still problematic in many cases. The other disadvantages include: higher detection limits and lower sensitivity than these obtained in laboratory conditions, a strong influence of environmental factors on the instrument performance and a high possibility of sample contamination in the field. This paper reviews recent applications of field portable instruments in environmental sample analysis and discusses their analytical capabilities. - Highlights: • Field portable instruments are widely used in environmental sample analysis. • Field portable instruments are indispensable for analysis in emergency response. • Miniaturization of field portable instruments reduces resource consumption. • In situ analysis is in agreement with green analytical chemistry

  2. Method validation and uncertainty evaluation of organically bound tritium analysis in environmental sample.

    Science.gov (United States)

    Huang, Yan-Jun; Zeng, Fan; Zhang, Bing; Chen, Chao-Feng; Qin, Hong-Juan; Wu, Lian-Sheng; Guo, Gui-Yin; Yang, Li-Tao; Shang-Guan, Zhi-Hong

    2014-08-01

    The analytical method for organically bound tritium (OBT) was developed in our laboratory. The optimized operating conditions and parameters were established for sample drying, special combustion, distillation, and measurement on a liquid scintillation spectrometer (LSC). Selected types of OBT samples such as rice, corn, rapeseed, fresh lettuce and pork were analyzed for method validation of recovery rate reproducibility, the minimum detection concentration, and the uncertainty for typical low level environmental sample was evaluated. The combustion water recovery rate of different dried environmental sample was kept at about 80%, the minimum detection concentration of OBT ranged from 0.61 to 0.89 Bq/kg (dry weight), depending on the hydrogen content. It showed that this method is suitable for OBT analysis of environmental sample with stable recovery rate, and the combustion water yield of a sample with weight about 40 g would provide sufficient quantity for measurement on LSC. Copyright © 2014 Elsevier Ltd. All rights reserved.

  3. Quality assurance programs developed and implemented by the US Department of Energy's Analytical Services Program for environmental restoration and waste management activities

    International Nuclear Information System (INIS)

    Lillian, D.; Bottrell, D.

    1993-01-01

    The U.S. Department of Energy's (DOE's) Office of Environmental Restoration and Waste Management (EM) has been tasked with addressing environmental contamination and waste problems facing the Department. A key element of any environmental restoration or waste management program is environmental data. An effective and efficient sampling and analysis program is required to generate credible environmental data. The bases for DOE's EM Analytical Services Program (ASP) are contained in the charter and commitments in Secretary of Energy Notice SEN-13-89, EM program policies and requirements, and commitments to Congress and the Office of Inspector General (IG). The Congressional commitment by DOE to develop and implement an ASP was in response to concerns raised by the Chairman of the Congressional Environment, Energy, and Natural Resources Subcommittee, and the Chairman of the Congressional Oversight and Investigations Subcommittee of the Committee on Energy and Commerce, regarding the production of analytical data. The development and implementation of an ASP also satisfies the IG's audit report recommendations on environmental analytical support, including development and implementation of a national strategy for acquisition of quality sampling and analytical services. These recommendations were endorsed in Departmental positions, which further emphasize the importance of the ASP to EM's programs. In September 1990, EM formed the Laboratory Management Division (LMD) in the Office of Technology Development to provide the programmatic direction needed to establish and operate an EM-wide ASP program. In January 1992, LMD issued the open-quotes Analytical Services Program Five-Year Plan.close quotes This document described LMD's strategy to ensure the production of timely, cost-effective, and credible environmental data. This presentation describes the overall LMD Analytical Services Program and, specifically, the various QA programs

  4. Analysis of environmental contamination resulting from catastrophic incidents: part 2. Building laboratory capability by selecting and developing analytical methodologies.

    Science.gov (United States)

    Magnuson, Matthew; Campisano, Romy; Griggs, John; Fitz-James, Schatzi; Hall, Kathy; Mapp, Latisha; Mullins, Marissa; Nichols, Tonya; Shah, Sanjiv; Silvestri, Erin; Smith, Terry; Willison, Stuart; Ernst, Hiba

    2014-11-01

    Catastrophic incidents can generate a large number of samples of analytically diverse types, including forensic, clinical, environmental, food, and others. Environmental samples include water, wastewater, soil, air, urban building and infrastructure materials, and surface residue. Such samples may arise not only from contamination from the incident but also from the multitude of activities surrounding the response to the incident, including decontamination. This document summarizes a range of activities to help build laboratory capability in preparation for sample analysis following a catastrophic incident, including selection and development of fit-for-purpose analytical methods for chemical, biological, and radiological contaminants. Fit-for-purpose methods are those which have been selected to meet project specific data quality objectives. For example, methods could be fit for screening contamination in the early phases of investigation of contamination incidents because they are rapid and easily implemented, but those same methods may not be fit for the purpose of remediating the environment to acceptable levels when a more sensitive method is required. While the exact data quality objectives defining fitness-for-purpose can vary with each incident, a governing principle of the method selection and development process for environmental remediation and recovery is based on achieving high throughput while maintaining high quality analytical results. This paper illustrates the result of applying this principle, in the form of a compendium of analytical methods for contaminants of interest. The compendium is based on experience with actual incidents, where appropriate and available. This paper also discusses efforts aimed at adaptation of existing methods to increase fitness-for-purpose and development of innovative methods when necessary. The contaminants of interest are primarily those potentially released through catastrophes resulting from malicious activity

  5. A review of analytical procedures for the simultaneous determination of medically important veterinary antibiotics in environmental water: Sample preparation, liquid chromatography, and mass spectrometry.

    Science.gov (United States)

    Kim, Chansik; Ryu, Hong-Duck; Chung, Eu Gene; Kim, Yongseok; Lee, Jae-Kwan

    2018-07-01

    Medically important (MI) antibiotics are defined by the United States Food and Drug Administration as drugs containing certain active antimicrobial ingredients that are used for the treatment of human diseases or enteric pathogens causing food-borne diseases. The presence of MI antibiotic residues in environmental water is a major concern for both aquatic ecosystems and public health, particularly because of their potential to contribute to the development of antimicrobial-resistant microorganisms. In this article, we present a review of global trends in the sales of veterinary MI antibiotics and the analytical methodologies used for the simultaneous determination of antibiotic residues in environmental water. According to recently published government reports, sales volumes have increased steadily, despite many countries having adopted strategies for reducing the consumption of antibiotics. Global attention needs to be directed urgently at establishing new management strategies for reducing the use of MI antimicrobial products in the livestock industry. The development of standardized analytical methods for the detection of multiple residues is required to monitor and understand the fate of antibiotics in the environment. Simultaneous analyses of antibiotics have mostly been conducted using high-performance liquid chromatography-tandem mass spectrometry with a solid-phase extraction (SPE) pretreatment step. Currently, on-line SPE protocols are used for the rapid and sensitive detection of antibiotics in water samples. On-line detection protocols must be established for the monitoring and screening of unknown metabolites and transformation products of antibiotics in environmental water. Copyright © 2018 Elsevier Ltd. All rights reserved.

  6. Graphene-based solid-phase extraction disk for fast separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples.

    Science.gov (United States)

    Wang, Zonghua; Han, Qiang; Xia, Jianfei; Xia, Linhua; Ding, Mingyu; Tang, Jie

    2013-06-01

    Graphene has great potentials for the use in sample preparation due to its ultra high specific surface area, superior chemical stability, and excellent thermal stability. In our work, a novel graphene-based SPE disk was developed for separation and preconcentration of trace polycyclic aromatic hydrocarbons from environmental water samples. Based on the strong π-π stacking interaction between the analytes and graphene, the analytes extracted by graphene were eluted by cyclohexane and then determined by GC-MS. Under the optimized conditions, high flow rate (30 mL/min) and sensitivity (0.84-13 ng/L) were achieved. The proposed method was successfully applied to the analysis of real environmental water samples with recoveries ranging from 72.8 to 106.2%. Furthermore, the property of anticlogging and reusability was also improved. This work reveals great potentials of graphene-based SPE disk in environmental analytical. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Historical review of long-term soil sampling for environmental surveillance at the Hanford Site and vicinity

    Energy Technology Data Exchange (ETDEWEB)

    Price, K.R.; Rickard, W.H.

    1997-08-01

    Soil samples have been collected routinely from the environs of the Hanford Site and analyzed since 1971. Correct interpretation of results depends on samples being collected from the same locations, the locations remaining relatively undisturbed, and collection and analytical procedures remaining the same or being equivalent. Historical files, documents, and annual environmental reports were reviewed to evaluate these factors. It was determined that 20 soil sampling locations, 11 onsite and 9 offsite, were established between 1971 and 1977 and represent long-term sampling locations. Sample collection and analytical procedures have remained essentially the same since 1971. The physical ecological attributes of each long-term soil sampling location were evaluated. During the review of historical records, a few results for 1970, 1971, and 1972 were noted as previously unreported in annual or special reports. These results are included in Appendix A. To complete the record, results previously reported in annual environmental reports are given in Appendix B. Global Positioning System (GPS) reading for 20 long-term soil sampling locations are provided in Appendix C.

  8. Historical review of long-term soil sampling for environmental surveillance at the Hanford Site and vicinity

    International Nuclear Information System (INIS)

    Price, K.R.; Rickard, W.H.

    1997-08-01

    Soil samples have been collected routinely from the environs of the Hanford Site and analyzed since 1971. Correct interpretation of results depends on samples being collected from the same locations, the locations remaining relatively undisturbed, and collection and analytical procedures remaining the same or being equivalent. Historical files, documents, and annual environmental reports were reviewed to evaluate these factors. It was determined that 20 soil sampling locations, 11 onsite and 9 offsite, were established between 1971 and 1977 and represent long-term sampling locations. Sample collection and analytical procedures have remained essentially the same since 1971. The physical ecological attributes of each long-term soil sampling location were evaluated. During the review of historical records, a few results for 1970, 1971, and 1972 were noted as previously unreported in annual or special reports. These results are included in Appendix A. To complete the record, results previously reported in annual environmental reports are given in Appendix B. Global Positioning System (GPS) reading for 20 long-term soil sampling locations are provided in Appendix C

  9. Environmental vulnerability assessment using Grey Analytic Hierarchy Process based model

    International Nuclear Information System (INIS)

    Sahoo, Satiprasad; Dhar, Anirban; Kar, Amlanjyoti

    2016-01-01

    Environmental management of an area describes a policy for its systematic and sustainable environmental protection. In the present study, regional environmental vulnerability assessment in Hirakud command area of Odisha, India is envisaged based on Grey Analytic Hierarchy Process method (Grey–AHP) using integrated remote sensing (RS) and geographic information system (GIS) techniques. Grey–AHP combines the advantages of classical analytic hierarchy process (AHP) and grey clustering method for accurate estimation of weight coefficients. It is a new method for environmental vulnerability assessment. Environmental vulnerability index (EVI) uses natural, environmental and human impact related factors, e.g., soil, geology, elevation, slope, rainfall, temperature, wind speed, normalized difference vegetation index, drainage density, crop intensity, agricultural DRASTIC value, population density and road density. EVI map has been classified into four environmental vulnerability zones (EVZs) namely: ‘low’, ‘moderate’ ‘high’, and ‘extreme’ encompassing 17.87%, 44.44%, 27.81% and 9.88% of the study area, respectively. EVI map indicates that the northern part of the study area is more vulnerable from an environmental point of view. EVI map shows close correlation with elevation. Effectiveness of the zone classification is evaluated by using grey clustering method. General effectiveness is in between “better” and “common classes”. This analysis demonstrates the potential applicability of the methodology. - Highlights: • Environmental vulnerability zone identification based on Grey Analytic Hierarchy Process (AHP) • The effectiveness evaluation by means of a grey clustering method with support from AHP • Use of grey approach eliminates the excessive dependency on the experience of experts.

  10. Environmental vulnerability assessment using Grey Analytic Hierarchy Process based model

    Energy Technology Data Exchange (ETDEWEB)

    Sahoo, Satiprasad [School of Water Resources, Indian Institute of Technology Kharagpur (India); Dhar, Anirban, E-mail: anirban.dhar@gmail.com [Department of Civil Engineering, Indian Institute of Technology Kharagpur (India); Kar, Amlanjyoti [Central Ground Water Board, Bhujal Bhawan, Faridabad, Haryana (India)

    2016-01-15

    Environmental management of an area describes a policy for its systematic and sustainable environmental protection. In the present study, regional environmental vulnerability assessment in Hirakud command area of Odisha, India is envisaged based on Grey Analytic Hierarchy Process method (Grey–AHP) using integrated remote sensing (RS) and geographic information system (GIS) techniques. Grey–AHP combines the advantages of classical analytic hierarchy process (AHP) and grey clustering method for accurate estimation of weight coefficients. It is a new method for environmental vulnerability assessment. Environmental vulnerability index (EVI) uses natural, environmental and human impact related factors, e.g., soil, geology, elevation, slope, rainfall, temperature, wind speed, normalized difference vegetation index, drainage density, crop intensity, agricultural DRASTIC value, population density and road density. EVI map has been classified into four environmental vulnerability zones (EVZs) namely: ‘low’, ‘moderate’ ‘high’, and ‘extreme’ encompassing 17.87%, 44.44%, 27.81% and 9.88% of the study area, respectively. EVI map indicates that the northern part of the study area is more vulnerable from an environmental point of view. EVI map shows close correlation with elevation. Effectiveness of the zone classification is evaluated by using grey clustering method. General effectiveness is in between “better” and “common classes”. This analysis demonstrates the potential applicability of the methodology. - Highlights: • Environmental vulnerability zone identification based on Grey Analytic Hierarchy Process (AHP) • The effectiveness evaluation by means of a grey clustering method with support from AHP • Use of grey approach eliminates the excessive dependency on the experience of experts.

  11. Rapid and automated determination of plutonium and neptunium in environmental samples

    International Nuclear Information System (INIS)

    Qiao, J.

    2011-03-01

    This thesis presents improved analytical methods for rapid and automated determination of plutonium and neptunium in environmental samples using sequential injection (SI) based chromatography and inductively coupled plasma mass spectrometry (ICP-MS). The progress of methodology development in this work consists of 5 subjects stated as follows: 1) Development and optimization of an SI-anion exchange chromatographic method for rapid determination of plutonium in environmental samples in combination of inductively coupled plasma mass spectrometry detection (Paper II); (2) Methodology development and optimization for rapid determination of plutonium in environmental samples using SI-extraction chromatography prior to inductively coupled plasma mass spectrometry (Paper III); (3) Development of an SI-chromatographic method for simultaneous determination of plutonium and neptunium in environmental samples (Paper IV); (4) Investigation of the suitability and applicability of 242 Pu as a tracer for rapid neptunium determination using anion exchange chromatography in an SI-network coupled with inductively coupled plasma mass spectrometry (Paper V); (5) Exploration of macro-porous anion exchange chromatography for rapid and simultaneous determination of plutonium and neptunium within an SI system (Paper VI). The results demonstrate that the developed methods in this study are reliable and efficient for accurate assays of trace levels of plutonium and neptunium as demanded in different situations including environmental risk monitoring and assessment, emergency preparedness and surveillance of contaminated areas. (Author)

  12. Rapid and automated determination of plutonium and neptunium in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Qiao, J.

    2011-03-15

    This thesis presents improved analytical methods for rapid and automated determination of plutonium and neptunium in environmental samples using sequential injection (SI) based chromatography and inductively coupled plasma mass spectrometry (ICP-MS). The progress of methodology development in this work consists of 5 subjects stated as follows: 1) Development and optimization of an SI-anion exchange chromatographic method for rapid determination of plutonium in environmental samples in combination of inductively coupled plasma mass spectrometry detection (Paper II); (2) Methodology development and optimization for rapid determination of plutonium in environmental samples using SI-extraction chromatography prior to inductively coupled plasma mass spectrometry (Paper III); (3) Development of an SI-chromatographic method for simultaneous determination of plutonium and neptunium in environmental samples (Paper IV); (4) Investigation of the suitability and applicability of 242Pu as a tracer for rapid neptunium determination using anion exchange chromatography in an SI-network coupled with inductively coupled plasma mass spectrometry (Paper V); (5) Exploration of macro-porous anion exchange chromatography for rapid and simultaneous determination of plutonium and neptunium within an SI system (Paper VI). The results demonstrate that the developed methods in this study are reliable and efficient for accurate assays of trace levels of plutonium and neptunium as demanded in different situations including environmental risk monitoring and assessment, emergency preparedness and surveillance of contaminated areas. (Author)

  13. A new tool for the evaluation of the analytical procedure: Green Analytical Procedure Index.

    Science.gov (United States)

    Płotka-Wasylka, J

    2018-05-01

    A new means for assessing analytical protocols relating to green analytical chemistry attributes has been developed. The new tool, called GAPI (Green Analytical Procedure Index), evaluates the green character of an entire analytical methodology, from sample collection to final determination, and was created using such tools as the National Environmental Methods Index (NEMI) or Analytical Eco-Scale to provide not only general but also qualitative information. In GAPI, a specific symbol with five pentagrams can be used to evaluate and quantify the environmental impact involved in each step of an analytical methodology, mainly from green through yellow to red depicting low, medium to high impact, respectively. The proposed tool was used to evaluate analytical procedures applied in the determination of biogenic amines in wine samples, and polycyclic aromatic hydrocarbon determination by EPA methods. GAPI tool not only provides an immediately perceptible perspective to the user/reader but also offers exhaustive information on evaluated procedures. Copyright © 2018 Elsevier B.V. All rights reserved.

  14. Sampling and chemical analysis in environmental samples around Nuclear Power Plants and some environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Yong Woo; Han, Man Jung; Cho, Seong Won; Cho, Hong Jun; Oh, Hyeon Kyun; Lee, Jeong Min; Chang, Jae Sook [KORTIC, Taejon (Korea, Republic of)

    2002-12-15

    Twelve kinds of environmental samples such as soil, seawater, underground water, etc. around Nuclear Power Plants(NPPs) were collected. Tritium chemical analysis was tried for the samples of rain water, pine-needle, air, seawater, underground water, chinese cabbage, a grain of rice and milk sampled around NPPs, and surface seawater and rain water sampled over the country. Strontium in the soil that sere sampled at 60 point of district in Korea were analyzed. Tritium were sampled at 60 point of district in Korea were analyzed. Tritium were analyzed in 21 samples of surface seawater around the Korea peninsular that were supplied from KFRDI(National Fisheries Research and Development Institute). Sampling and chemical analysis environmental samples around Kori, Woolsung, Youngkwang, Wooljin Npps and Taeduk science town for tritium and strontium analysis was managed according to plans. Succeed to KINS after all samples were tried.

  15. Contemporary sample stacking in analytical electrophoresis

    Czech Academy of Sciences Publication Activity Database

    Šlampová, Andrea; Malá, Zdeňka; Pantůčková, Pavla; Gebauer, Petr; Boček, Petr

    2013-01-01

    Roč. 34, č. 1 (2013), s. 3-18 ISSN 0173-0835 R&D Projects: GA ČR GAP206/10/1219 Institutional support: RVO:68081715 Keywords : biological samples * stacking * trace analysis * zone electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.161, year: 2013

  16. Contemporary sample stacking in analytical electrophoresis

    Czech Academy of Sciences Publication Activity Database

    Malá, Zdeňka; Šlampová, Andrea; Křivánková, Ludmila; Gebauer, Petr; Boček, Petr

    2015-01-01

    Roč. 36, č. 1 (2015), s. 15-35 ISSN 0173-0835 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : biological samples * stacking * trace analysis * zone electrophoresis Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.482, year: 2015

  17. Quality assurance programs developed and implemented by the US Department of Energy`s Analytical Services Program for environmental restoration and waste management activities

    Energy Technology Data Exchange (ETDEWEB)

    Lillian, D.; Bottrell, D. [Dept. of Energy, Germntown, MD (United States)

    1993-12-31

    The U.S. Department of Energy`s (DOE`s) Office of Environmental Restoration and Waste Management (EM) has been tasked with addressing environmental contamination and waste problems facing the Department. A key element of any environmental restoration or waste management program is environmental data. An effective and efficient sampling and analysis program is required to generate credible environmental data. The bases for DOE`s EM Analytical Services Program (ASP) are contained in the charter and commitments in Secretary of Energy Notice SEN-13-89, EM program policies and requirements, and commitments to Congress and the Office of Inspector General (IG). The Congressional commitment by DOE to develop and implement an ASP was in response to concerns raised by the Chairman of the Congressional Environment, Energy, and Natural Resources Subcommittee, and the Chairman of the Congressional Oversight and Investigations Subcommittee of the Committee on Energy and Commerce, regarding the production of analytical data. The development and implementation of an ASP also satisfies the IG`s audit report recommendations on environmental analytical support, including development and implementation of a national strategy for acquisition of quality sampling and analytical services. These recommendations were endorsed in Departmental positions, which further emphasize the importance of the ASP to EM`s programs. In September 1990, EM formed the Laboratory Management Division (LMD) in the Office of Technology Development to provide the programmatic direction needed to establish and operate an EM-wide ASP program. In January 1992, LMD issued the {open_quotes}Analytical Services Program Five-Year Plan.{close_quotes} This document described LMD`s strategy to ensure the production of timely, cost-effective, and credible environmental data. This presentation describes the overall LMD Analytical Services Program and, specifically, the various QA programs.

  18. An intercomparison on radionuclides in environmental samples, Baltic-Danish co-operation project on radiation protection 2001-2003

    DEFF Research Database (Denmark)

    Nielsen, S.P.

    2004-01-01

    Sixteen laboratories participated in an intercomparison exercise carried out in 2003 on laboratory analyses of radionuclides in environmental samples. The sample types included seawater, lake water, soil, dry milk and seaweed and the exercise involved theradionuclides 137Cs, 90Sr, 60Co, 239, 240Pu...... laboratories passed the evaluation tests. The results indicate that for several of the laboratories there isroom to improve the analytical quality on radionuclides in environmental samples to match an uncertainty corresponding to a relative standard deviation of 10%....

  19. Possibilities for decreasing detection limits of analytical methods for determination of transformation products of unsymmetrical dimethylhydrazine in environmental samples

    Directory of Open Access Journals (Sweden)

    Bulat Kenessov

    2015-12-01

    Full Text Available Most rockets of middle and heavy class launched from Kazakhstan, Russia, China and other countries still use highly toxic unsymmetrical dimethylhydrazine (UDMH as a liquid propellant. Study of migration, distribution and accumulation of UDMH transformation products in environment and human health impact assessment of space rocket activity are currently complicated due to the absence of analytical methods allowing detection of trace concentrations of these compounds in analyzed samples. This paper reviews methods and approaches, which can be applied for development of such methods. Detection limits at a part-per-trillion (ppt level may be achieved using most selective and sensitive methods based on gas or liquid chromatography in combination of tandem or high-resolution mass spectrometry. In addition, 1000-fold concentration of samples or integrated sample preparation methods, e.g., dynamic headspace extraction, are required. Special attention during development and application of such methods must be paid to purity of laboratory air, reagents, glassware and analytical instruments.

  20. Improvements to sample processing and measurement to enable more widespread environmental application of tritium

    Energy Technology Data Exchange (ETDEWEB)

    Moran, James; Alexander, Thomas; Aalseth, Craig; Back, Henning; Mace, Emily; Overman, Cory; Seifert, Allen; Freeburg, Wilcox

    2017-08-01

    Previous measurements have demonstrated the wealth of information that tritium (T) can provide on environmentally relevant processes. We present modifications to sample preparation approaches that enable T measurement by proportional counting on small sample sizes equivalent to 120 mg of water and demonstrate the accuracy of these methods on a suite of standardized water samples. This enhanced method should provide the analytical flexibility needed to address persistent knowledge gaps in our understanding of T behavior in the environment.

  1. New trends in the analytical determination of emerging contaminants and their transformation products in environmental waters.

    Science.gov (United States)

    Agüera, Ana; Martínez Bueno, María Jesús; Fernández-Alba, Amadeo R

    2013-06-01

    Since the so-called emerging contaminants were established as a new group of pollutants of environmental concern, a great effort has been devoted to the knowledge of their distribution, fate and effects in the environment. After more than 20 years of work, a significant improvement in knowledge about these contaminants has been achieved, but there is still a large gap of information on the growing number of new potential contaminants that are appearing and especially of their unpredictable transformation products. Although the environmental problem arising from emerging contaminants must be addressed from an interdisciplinary point of view, it is obvious that analytical chemistry plays an important role as the first step of the study, as it allows establishing the presence of chemicals in the environment, estimate their concentration levels, identify sources and determine their degradation pathways. These tasks involve serious difficulties requiring different analytical solutions adjusted to purpose. Thus, the complexity of the matrices requires highly selective analytical methods; the large number and variety of compounds potentially present in the samples demands the application of wide scope methods; the low concentrations at which these contaminants are present in the samples require a high detection sensitivity, and high demands on the confirmation and high structural information are needed for the characterisation of unknowns. New developments on analytical instrumentation have been applied to solve these difficulties. Furthermore and not less important has been the development of new specific software packages intended for data acquisition and, in particular, for post-run analysis. Thus, the use of sophisticated software tools has allowed successful screening analysis, determining several hundreds of analytes, and assisted in the structural elucidation of unknown compounds in a timely manner.

  2. Analytical laboratory and mobile sampling platform

    International Nuclear Information System (INIS)

    Stetzenbach, K.; Smiecinski, A.

    1996-01-01

    This is the final report for the Analytical Laboratory and Mobile Sampling Platform project. This report contains only major findings and conclusions resulting from this project. Detailed reports of all activities performed for this project were provided to the Project Office every quarter since the beginning of the project. This report contains water chemistry data for samples collected in the Nevada section of Death Valley National Park (Triangle Area Springs), Nevada Test Site springs, Pahranagat Valley springs, Nevada Test Site wells, Spring Mountain springs and Crater Flat and Amargosa Valley wells

  3. A rapid and sensitive analytical method for the determination of 14 pyrethroids in water samples.

    Science.gov (United States)

    Feo, M L; Eljarrat, E; Barceló, D

    2010-04-09

    A simple, efficient and environmentally friendly analytical methodology is proposed for extracting and preconcentrating pyrethroids from water samples prior to gas chromatography-negative ion chemical ionization mass spectrometry (GC-NCI-MS) analysis. Fourteen pyrethroids were selected for this work: bifenthrin, cyfluthrin, lambda-cyhalothrin, cypermethrin, deltamethrin, esfenvalerate, fenvalerate, fenpropathrin, tau-fluvalinate, permethrin, phenothrin, resmethrin, tetramethrin and tralomethrin. The method is based on ultrasound-assisted emulsification-extraction (UAEE) of a water-immiscible solvent in an aqueous medium. Chloroform was used as extraction solvent in the UAEE technique. Target analytes were quantitatively extracted achieving an enrichment factor of 200 when 20 mL aliquot of pure water spiked with pyrethroid standards was extracted. The method was also evaluated with tap water and river water samples. Method detection limits (MDLs) ranged from 0.03 to 35.8 ng L(-1) with RSDs values or =0.998. Recovery values were in the range of 45-106%, showing satisfactory robustness of the method for analyzing pyrethroids in water samples. The proposed methodology was applied for the analysis of river water samples. Cypermethrin was detected at concentration levels ranging from 4.94 to 30.5 ng L(-1). Copyright 2010 Elsevier B.V. All rights reserved.

  4. Stability of volatile organics in environmental soil samples

    Energy Technology Data Exchange (ETDEWEB)

    Maskarinec, M.P.; Bayne, C.K.; Jenkins, R.A.; Johnson, L.H.; Holladay, S.K.

    1992-11-01

    This report focuses on data generated for the purpose of establishing the stability of 19 volatile organic compounds in environmental soil samples. The study was carried out over a 56 day (for two soils) and a 111 day (for one reference soil) time frame and took into account as many variables as possible within the constraints of budget and time. The objectives of the study were: 1) to provide a data base which could be used to provide guidance on pre-analytical holding times for regulatory purposes; and 2) to provide a basis for the evaluation of data which is generated outside of the currently allowable holding times.

  5. Metal-organic framework based in-syringe solid-phase extraction for the on-site sampling of polycyclic aromatic hydrocarbons from environmental water samples.

    Science.gov (United States)

    Zhang, Xiaoqiong; Wang, Peiyi; Han, Qiang; Li, Hengzhen; Wang, Tong; Ding, Mingyu

    2018-04-01

    In-syringe solid-phase extraction is a promising sample pretreatment method for the on-site sampling of water samples because of its outstanding advantages of portability, simple operation, short extraction time, and low cost. In this work, a novel in-syringe solid-phase extraction device using metal-organic frameworks as the adsorbent was fabricated for the on-site sampling of polycyclic aromatic hydrocarbons from environmental waters. Trace polycyclic aromatic hydrocarbons were effectively extracted through the self-made device followed by gas chromatography with mass spectrometry analysis. Owing to the excellent adsorption performance of metal-organic frameworks, the analytes could be completely adsorbed during one adsorption cycle, thus effectively shortening the extraction time. Moreover, the adsorbed analytes could remain stable on the device for at least 7 days, revealing the potential of the self-made device for on-site sampling of degradable compounds in remote regions. The limit of detection ranged from 0.20 to 1.9 ng/L under the optimum conditions. Satisfactory recoveries varying from 84.4 to 104.5% and relative standard deviations below 9.7% were obtained in real samples analysis. The results of this study promote the application of metal-organic frameworks in sample preparation and demonstrate the great potential of in-syringe solid-phase extraction for the on-site sampling of trace contaminants in environmental waters. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Radionuclide determination in environmental samples by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Lariviere, Dominic; Taylor, Vivien F.; Evans, R. Douglas; Cornett, R. Jack

    2006-01-01

    The determination of naturally occurring and anthropogenic radionuclides in the environment by inductively coupled plasma mass spectrometry has gained recognition over the last fifteen years, relative to radiometric techniques, as the result of improvement in instrumental performance, sample introduction equipment, and sample preparation. With the increase in instrumental sensitivity, it is now possible to measure ultratrace levels (fg range) of many radioisotopes, including those with half-lives between 1 and 1000 years, without requiring very complex sample pre-concentration schemes. However, the identification and quantification of radioisotopes in environmental matrices is still hampered by a variety of analytical issues such as spectral (both atomic and molecular ions) and non-spectral (matrix effect) interferences and instrumental limitations (e.g., abundance sensitivity). The scope of this review is to highlight recent analytical progress and issues associated with the determination of radionuclides by inductively coupled plasma mass spectrometry. The impact of interferences, instrumental limitations (e.g., degree of ionization, abundance sensitivity, detection limits) and low sample-to-plasma transfer efficiency on the measurement of radionuclides by inductively coupled plasma mass spectrometry will be described. Solutions that overcome these issues will be discussed, highlighting their pros and cons and assessing their impact on the measurement of environmental radioactivity. Among the solutions proposed, mass and chemical resolution through the use of sector-field instruments and chemical reactions/collisions in a pressurized cell, respectively, will be described. Other methods, such as unique sample introduction equipment (e.g., laser ablation, electrothermal vaporisation, high efficiency nebulization) and instrumental modifications/optimizations (e.g., instrumental vacuum, radiofrequency power, guard electrode) that improve sensitivity and performance

  7. Use of nuclear and related analytical techniques in environmental research as exemplified by selected air pollution studies

    International Nuclear Information System (INIS)

    Smodis, B.; Jacimovic, R.; Jeran, Z.; Stropnik, B.; Svetina, M.

    2000-01-01

    Among nuclear and nuclear related analytical techniques, neutron activation analysis and X-ray fluorescence spectrometry proved to be particularly useful for environmental studies owing to their nondestructive character and multi element capability. This paper emphasizes their importance among other multielement analytical methods by discussing their specific role due to specific physics basis, quite different to other destructive non-nuclear methods, and by summarizing results obtained in several studies related to air pollution research, including analyses of airborne particulate matter, water samples, lichens and mosses. (author)

  8. Industrial and environmental applications of nuclear analytical techniques. Report of a workshop

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1999-11-01

    The IAEA has programme the utilisation of nuclear analytical techniques (NATs), in particular for industrial and environmental applications. A major purpose is to help the developing Member States apply their analytical capabilities optimally for socio-economic progress and development. A large number of institutions in Europe, Africa, Latin America and Asia have established X ray fluorescence (XRF) and gamma ray measurement techniques and facilities for neutron activation analysis (NAA) have been initiated in institutions in these regions. Moreover, there is a growing interest among many institutes in applying more advanced analytical techniques, such as particle induced X ray emission (PIXE) and microanalytical techniques based on X ray emission induced by conventional sources or synchrotron radiation to the analysis of environmental and biological materials and industrial products. In order to define new areas of application of NATs and to extend the range of these techniques, a number of initiatives have recently been taken. It includes a workshop on industrial and environmental applications of nuclear analytical techniques, organized by the IAEA in Vienna, 7-11 September 1998. The main objectives of the workshop were as follows: (1) to review recent applications of NATs in industrial and environmental studies; (2) to identify emerging trends in methodologies and applications of NATs; (3) to demonstrate analytical capabilities of selected NATs. The following topics were reviewed during the workshop: (1) XRF and accelerator based analytical techniques; (2) portable XRF systems and their applications in industry, mineral prospecting and processing, (3) portable gamma ray spectrometers; and (4) NAA and its applications in industry and environmental studies. Micro-XRF and micro-PIXE methods and their applications in the above fields were also discussed, including aspects of synchrotron radiation induced X ray emission.

  9. Industrial and environmental applications of nuclear analytical techniques. Report of a workshop

    International Nuclear Information System (INIS)

    1999-11-01

    The IAEA has programme the utilisation of nuclear analytical techniques (NATs), in particular for industrial and environmental applications. A major purpose is to help the developing Member States apply their analytical capabilities optimally for socio-economic progress and development. A large number of institutions in Europe, Africa, Latin America and Asia have established X ray fluorescence (XRF) and gamma ray measurement techniques and facilities for neutron activation analysis (NAA) have been initiated in institutions in these regions. Moreover, there is a growing interest among many institutes in applying more advanced analytical techniques, such as particle induced X ray emission (PIXE) and microanalytical techniques based on X ray emission induced by conventional sources or synchrotron radiation to the analysis of environmental and biological materials and industrial products. In order to define new areas of application of NATs and to extend the range of these techniques, a number of initiatives have recently been taken. It includes a workshop on industrial and environmental applications of nuclear analytical techniques, organized by the IAEA in Vienna, 7-11 September 1998. The main objectives of the workshop were as follows: (1) to review recent applications of NATs in industrial and environmental studies; (2) to identify emerging trends in methodologies and applications of NATs; (3) to demonstrate analytical capabilities of selected NATs. The following topics were reviewed during the workshop: (1) XRF and accelerator based analytical techniques; (2) portable XRF systems and their applications in industry, mineral prospecting and processing, (3) portable gamma ray spectrometers; and (4) NAA and its applications in industry and environmental studies. Micro-XRF and micro-PIXE methods and their applications in the above fields were also discussed, including aspects of synchrotron radiation induced X ray emission

  10. Environmental surveillance master sampling schedule

    International Nuclear Information System (INIS)

    Bisping, L.E.

    1995-02-01

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest Laboratory (PNL) for the U.S. Department of Energy (DOE). This document contains the planned 1994 schedules for routine collection of samples for the Surface Environmental Surveillance Project (SESP), Drinking Water Project, and Ground-Water Surveillance Project. Samples are routinely collected for the SESP and analyzed to determine the quality of air, surface water, soil, sediment, wildlife, vegetation, foodstuffs, and farm products at Hanford Site and surrounding communities. The responsibility for monitoring onsite drinking water falls outside the scope of the SESP. PNL conducts the drinking water monitoring project concurrent with the SESP to promote efficiency and consistency, utilize expertise developed over the years, and reduce costs associated with management, procedure development, data management, quality control, and reporting. The ground-water sampling schedule identifies ground-water sampling .events used by PNL for environmental surveillance of the Hanford Site. Sampling is indicated as annual, semi-annual, quarterly, or monthly in the sampling schedule. Some samples are collected and analyzed as part of ground-water monitoring and characterization programs at Hanford (e.g. Resources Conservation and Recovery Act (RCRA), Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA), or Operational). The number of samples planned by other programs are identified in the sampling schedule by a number in the analysis column and a project designation in the Cosample column. Well sampling events may be merged to avoid redundancy in cases where sampling is planned by both-environmental surveillance and another program

  11. Environmental surveillance master sampling schedule

    Energy Technology Data Exchange (ETDEWEB)

    Bisping, L.E.

    1995-02-01

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest Laboratory (PNL) for the U.S. Department of Energy (DOE). This document contains the planned 1994 schedules for routine collection of samples for the Surface Environmental Surveillance Project (SESP), Drinking Water Project, and Ground-Water Surveillance Project. Samples are routinely collected for the SESP and analyzed to determine the quality of air, surface water, soil, sediment, wildlife, vegetation, foodstuffs, and farm products at Hanford Site and surrounding communities. The responsibility for monitoring onsite drinking water falls outside the scope of the SESP. PNL conducts the drinking water monitoring project concurrent with the SESP to promote efficiency and consistency, utilize expertise developed over the years, and reduce costs associated with management, procedure development, data management, quality control, and reporting. The ground-water sampling schedule identifies ground-water sampling .events used by PNL for environmental surveillance of the Hanford Site. Sampling is indicated as annual, semi-annual, quarterly, or monthly in the sampling schedule. Some samples are collected and analyzed as part of ground-water monitoring and characterization programs at Hanford (e.g. Resources Conservation and Recovery Act (RCRA), Comprehensive Environmental Response, Compensation, and Liability Act (CERCLA), or Operational). The number of samples planned by other programs are identified in the sampling schedule by a number in the analysis column and a project designation in the Cosample column. Well sampling events may be merged to avoid redundancy in cases where sampling is planned by both-environmental surveillance and another program.

  12. Environmental sampling

    International Nuclear Information System (INIS)

    Puckett, J.M.

    1998-01-01

    Environmental Sampling (ES) is a technology option that can have application in transparency in nuclear nonproliferation. The basic process is to take a sample from the environment, e.g., soil, water, vegetation, or dust and debris from a surface, and through very careful sample preparation and analysis, determine the types, elemental concentration, and isotopic composition of actinides in the sample. The sample is prepared and the analysis performed in a clean chemistry laboratory (CCL). This ES capability is part of the IAEA Strengthened Safeguards System. Such a Laboratory is planned to be built by JAERI at Tokai and will give Japan an intrinsic ES capability. This paper presents options for the use of ES as a transparency measure for nuclear nonproliferation

  13. Nonactivation interaction techniques in the analysis of environmental samples

    International Nuclear Information System (INIS)

    Tolgyessy, J.

    1986-01-01

    Nonactivation interaction analytical methods are based on the interaction processes of nuclear and X-ray radiation with a sample, leading to their absorption and backscattering, to the ionization of gases or excitation of fluorescent X-ray by radiation, but not to the activation of determined elements. From the point of view of environmental analysis, the most useful nonactivation interaction techniques are X-ray fluorescence by photon or charged particle excitation, ionization of gases by nuclear radiation, elastic scattering of charged particles and backscattering of beta radiation. The significant advantage of these methods is that they are nondestructive. (author)

  14. The measure of radiocarbon in the drating of environmental samples

    International Nuclear Information System (INIS)

    Ruiz Pessenda, L.C.; Camargo, P.B. de

    1990-01-01

    An analytical system for radiocarbon dating of environmental samples (charcoal, shell, wood, etc.) using low level liquid scintillation spectrometry has been developed and optimized at Center for Nuclear Energy in Agriculture of the University of Sao Paulo. Physical and chemical pretreatment of samples to remove oils, resins, carbonates and fulvic and humic acids; the benzene synthesis of NBS oxalic acid standard, calcium carbonate P.A. and marble and the results of benzene yield; the optimization of radiocarbon counting window; the effect of scintillators PPO-POPOP and butyl PBD on the efficiency of detection and background of radiocarbon, are described. Samples of charcoal, shell and wood, previously dated at the radiocarbon laboratories of Centre des Faibles Radioactives, France, and Instituto de Geociencias of USP, are analysed for preliminary laboratory intercomparison. (author) [pt

  15. Analytical evaluation of BEA zeolite for the pre-concentration of polycyclic aromatic hydrocarbons and their subsequent chromatographic analysis in water samples.

    Science.gov (United States)

    Wilson, Walter B; Costa, Andréia A; Wang, Huiyong; Dias, José A; Dias, Sílvia C L; Campiglia, Andres D

    2012-07-06

    The analytical performance of BEA - a commercial zeolite - is evaluated for the pre-concentration of fifteen Environmental Protection Agency - polycyclic aromatic hydrocarbons and their subsequent HPLC analysis in tap and lake water samples. The pre-concentration factors obtained with BEA have led to a method with excellent analytical figures of merit. One milliliter aliquots were sufficient to obtain excellent precision of measurements at the parts-per-trillion concentration level with relative standard deviations varying from 4.1% (dibenzo[a,h]anthracene) to 13.4% (pyrene). The limits of detection were excellent as well and varied between 1.1 (anthracene) and 49.9 ng L(-1) (indeno[1,2,3-cd]pyrene). The recovery values of all the studied compounds meet the criterion for regulated polycyclic aromatic hydrocarbons, which mandates relative standard deviations equal or lower than 25%. The small volume of organic solvents (100 μL per sample) and amount of BEA (2 mg per sample) makes sample pre-concentration environmentally friendly and cost effective. The extraction procedure is well suited for numerous samples as the small working volume (1 mL) facilitates the implementation of simultaneous sample extraction. These are attractive features when routine monitoring of numerous samples is contemplated. Copyright © 2012 Elsevier B.V. All rights reserved.

  16. Materials and Methods for Streamlined Laboratory Analysis of Environmental Samples, FY 2016 Report

    Energy Technology Data Exchange (ETDEWEB)

    Addleman, Raymond S. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Naes, Benjamin E. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); McNamara, Bruce K. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Olsen, Khris B. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Chouyyok, Wilaiwan [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Willingham, David G. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Spigner, Angel C. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2016-11-30

    The International Atomic Energy Agency (IAEA) relies upon laboratory analysis of environmental samples (typically referred to as “swipes”) collected during on-site inspections of safeguarded facilities to support the detection and deterrence of undeclared activities. Unfortunately, chemical processing and assay of the samples is slow and expensive. A rapid, effective, and simple extraction process and analysis method is needed to provide certified results with improved timeliness at reduced costs (principally in the form of reduced labor), while maintaining or improving sensitivity and efficacy. To address these safeguard needs the Pacific Northwest National Laboratory (PNNL) explored and demonstrated improved methods for environmental sample (ES) analysis. Improvements for both bulk and particle analysis were explored. To facilitate continuity and adoption, the new sampling materials and processing methods will be compatible with existing IAEA protocols for ES analysis. PNNL collaborated with Oak Ridge National Laboratory (ORNL), which performed independent validation of the new bulk analysis methods and compared performance to traditional IAEA’s Network of Analytical Laboratories (NWAL) protocol. ORNL efforts are reported separately. This report describes PNNL’s FY 2016 progress, which was focused on analytical application supporting environmental monitoring of uranium enrichment plants and nuclear fuel processing. In the future the technology could be applied to other safeguard applications and analytes related to fuel manufacturing, reprocessing, etc. PNNL’s FY 2016 efforts were broken into two tasks and a summary of progress, accomplishments and highlights are provided below. Principal progress and accomplishments on Task 1, Optimize Materials and Methods for ICP-MS Environmental Sample Analysis, are listed below. • Completed initial procedure for rapid uranium extraction from ES swipes based upon carbonate-peroxide chemistry (delivered to ORNL for

  17. Problem Formulation in Knowledge Discovery via Data Analytics (KDDA) for Environmental Risk Management.

    Science.gov (United States)

    Li, Yan; Thomas, Manoj; Osei-Bryson, Kweku-Muata; Levy, Jason

    2016-12-15

    With the growing popularity of data analytics and data science in the field of environmental risk management, a formalized Knowledge Discovery via Data Analytics (KDDA) process that incorporates all applicable analytical techniques for a specific environmental risk management problem is essential. In this emerging field, there is limited research dealing with the use of decision support to elicit environmental risk management (ERM) objectives and identify analytical goals from ERM decision makers. In this paper, we address problem formulation in the ERM understanding phase of the KDDA process. We build a DM³ ontology to capture ERM objectives and to inference analytical goals and associated analytical techniques. A framework to assist decision making in the problem formulation process is developed. It is shown how the ontology-based knowledge system can provide structured guidance to retrieve relevant knowledge during problem formulation. The importance of not only operationalizing the KDDA approach in a real-world environment but also evaluating the effectiveness of the proposed procedure is emphasized. We demonstrate how ontology inferencing may be used to discover analytical goals and techniques by conceptualizing Hazardous Air Pollutants (HAPs) exposure shifts based on a multilevel analysis of the level of urbanization (and related economic activity) and the degree of Socio-Economic Deprivation (SED) at the local neighborhood level. The HAPs case highlights not only the role of complexity in problem formulation but also the need for integrating data from multiple sources and the importance of employing appropriate KDDA modeling techniques. Challenges and opportunities for KDDA are summarized with an emphasis on environmental risk management and HAPs.

  18. Problem Formulation in Knowledge Discovery via Data Analytics (KDDA) for Environmental Risk Management

    Science.gov (United States)

    Li, Yan; Thomas, Manoj; Osei-Bryson, Kweku-Muata; Levy, Jason

    2016-01-01

    With the growing popularity of data analytics and data science in the field of environmental risk management, a formalized Knowledge Discovery via Data Analytics (KDDA) process that incorporates all applicable analytical techniques for a specific environmental risk management problem is essential. In this emerging field, there is limited research dealing with the use of decision support to elicit environmental risk management (ERM) objectives and identify analytical goals from ERM decision makers. In this paper, we address problem formulation in the ERM understanding phase of the KDDA process. We build a DM3 ontology to capture ERM objectives and to inference analytical goals and associated analytical techniques. A framework to assist decision making in the problem formulation process is developed. It is shown how the ontology-based knowledge system can provide structured guidance to retrieve relevant knowledge during problem formulation. The importance of not only operationalizing the KDDA approach in a real-world environment but also evaluating the effectiveness of the proposed procedure is emphasized. We demonstrate how ontology inferencing may be used to discover analytical goals and techniques by conceptualizing Hazardous Air Pollutants (HAPs) exposure shifts based on a multilevel analysis of the level of urbanization (and related economic activity) and the degree of Socio-Economic Deprivation (SED) at the local neighborhood level. The HAPs case highlights not only the role of complexity in problem formulation but also the need for integrating data from multiple sources and the importance of employing appropriate KDDA modeling techniques. Challenges and opportunities for KDDA are summarized with an emphasis on environmental risk management and HAPs. PMID:27983713

  19. ISCO Grab Sample Ion Chromatography Analytical Data

    Data.gov (United States)

    U.S. Environmental Protection Agency — ISCO grab samples were collected from river, wastewater treatment plant discharge, and public drinking water intakes. Samples were analyzed for major ions (ppb)...

  20. Determination of uranium isotopes in environmental samples by anion exchange in sulfuric and hydrochloric acid media

    International Nuclear Information System (INIS)

    Popov, L.

    2016-01-01

    Method for determination of uranium isotopes in various environmental samples is presented. The major advantages of the method are the low cost of the analysis, high radiochemical yields and good decontamination factors from the matrix elements, natural and man-made radionuclides. The separation and purification of uranium is attained by adsorption with strong base anion exchange resin in sulfuric and hydrochloric acid media. Uranium is electrodeposited on a stainless steel disk and measured by alpha spectrometry. The analytical method has been applied for the determination of concentrations of uranium isotopes in mineral, spring and tap waters from Bulgaria. The analytical quality was checked by analyzing reference materials. - Highlights: • The method allows cost-effective determination of U isotopes. • High amounts of environmental samples can be analyzed. • High chemical yields, energy resolution and decontamination factors were achieved. • Uranium isotope concentrations in mineral waters from Bulgaria are presented.

  1. Analytical characterization of high-level mixed wastes using multiple sample preparation treatments

    International Nuclear Information System (INIS)

    King, A.G.; Baldwin, D.L.; Urie, M.W.; McKinley, S.G.

    1994-01-01

    The Analytical Chemistry Laboratory at the Pacific Northwest Laboratory in Richland, Washington, is actively involved in performing analytical characterization of high-level mixed waste from Hanford's single shell and double shell tank characterization programs. A full suite of analyses is typically performed on homogenized tank core samples. These analytical techniques include inductively-coupled plasma-atomic emission spectroscopy, total organic carbon methods and radiochemistry methods, as well as many others, all requiring some type of remote sample-preparation treatment to solubilize the tank sludge material for analysis. Most of these analytical methods typically use a single sample-preparation treatment, inherently providing elemental information only. To better understand and interpret tank chemistry and assist in identifying chemical compounds, selected analytical methods are performed using multiple sample-preparation treatments. The sample preparation treatments used at Pacific Northwest Laboratory for this work with high-level mixed waste include caustic fusion, acid digestion, and water leach. The type of information available by comparing results from different sample-prep treatments includes evidence for the presence of refractory compounds, acid-soluble compounds, or water-soluble compounds. Problems unique to the analysis of Hanford tank wastes are discussed. Selected results from the Hanford single shell ferrocyanide tank, 241-C-109, are presented, and the resulting conclusions are discussed

  2. 8. All Polish Conference on Analytical Chemistry: Analytical Chemistry for the Community of the 21. Century

    International Nuclear Information System (INIS)

    Koscielniak, P.; Wieczorek, M.; Kozak, J.

    2010-01-01

    Book of Abstracts contains short descriptions of lectures, communications and posters presented during 8 th All Polish Conference on Analytical Chemistry (Cracow, 4-9.07.2010). Scientific programme consisted of: basic analytical problems, preparation of the samples, chemometry and metrology, miniaturization of the analytical procedures, environmental analysis, medicinal analyses, industrial analyses, food analyses, biochemical analyses, analysis of relicts of the past. Several posters were devoted to the radiochemical separations, radiochemical analysis, environmental behaviour of the elements important for the nuclear science and the professional tests.

  3. A New Project-Based Lab for Undergraduate Environmental and Analytical Chemistry

    Science.gov (United States)

    Adami, Gianpiero

    2006-01-01

    A new project-based lab was developed for third year undergraduate chemistry students based on real world applications. The experience suggests that the total analytical procedure (TAP) project offers a stimulating alternative for delivering science skills and developing a greater interest for analytical chemistry and environmental sciences and…

  4. Radioactivity in environmental samples

    International Nuclear Information System (INIS)

    Fornaro, Laura

    2001-01-01

    The objective of this practical work is to familiarize the student with radioactivity measures in environmental samples. For that were chosen samples a salt of natural potassium, a salt of uranium or torio and a sample of drinkable water

  5. Accuracy and Precision in Elemental Analysis of Environmental Samples using Inductively Coupled Plasma-Atomic Emission Spectrometry

    International Nuclear Information System (INIS)

    Quraishi, Shamsad Begum; Chung, Yong-Sam; Choi, Kwang Soon

    2005-01-01

    Inductively Coupled Plasma-Atomic Emission Spectrometry followed by micro-wave digestion have been performed on different environmental Certified Reference Materials (CRMs). Analytical results show that accuracy and precision in ICP-AES analysis were acceptable and satisfactory in case of soil and hair CRM samples. The relative error of most of the elements in these two CRMs is within 10% with few exceptions and coefficient of variation is also less than 10%. Z-score as an analytical performance was also within the acceptable range (±2). ICP-AES was found as an inadequate method for Air Filter CRM due to incomplete dissolution, low concentration of elements and very low mass of the sample. However, real air filter sample could have been analyzed with high accuracy and precision by increasing sample mass during collection. (author)

  6. A Procedure for the Sequential Determination of Radionuclides in Environmental Samples. Liquid Scintillation Counting and Alpha Spectrometry for 90Sr, 241Am and Pu Radioisotopes

    International Nuclear Information System (INIS)

    2014-01-01

    Since 2004, IAEA activities related to the terrestrial environment have aimed at the development of a set of procedures to determine radionuclides in environmental samples. Reliable, comparable and ‘fit for purpose’ results are an essential requirement for any decision based on analytical measurements. For the analyst, tested and validated analytical procedures are extremely important tools for the production of analytical data. For maximum utility, such procedures should be comprehensive, clearly formulated and readily available for reference to both the analyst and the customer. This publication describes a combined procedure for the sequential determination of 90 Sr, 241 Am and Pu radioisotopes in environmental samples. The method is based on the chemical separation of strontium, americium and plutonium using ion exchange chromatography, extraction chromatography and precipitation followed by alpha spectrometric and liquid scintillation counting detection. The method was tested and validated in terms of repeatability and trueness in accordance with International Organization for Standardization (ISO) guidelines using reference materials and proficiency test samples. Reproducibility tests were performed later at the IAEA Terrestrial Environment Laboratory. The calculations of the massic activity, uncertainty budget, decision threshold and detection limit are also described in this publication. The procedure is introduced for the determination of 90 Sr, 241 Am and Pu radioisotopes in environmental samples such as soil, sediment, air filter and vegetation samples. It is expected to be of general use to a wide range of laboratories, including the Analytical Laboratories for the Measurement of Environmental Radioactivity (ALMERA) network for routine environmental monitoring purposes

  7. Problem Formulation in Knowledge Discovery via Data Analytics (KDDA for Environmental Risk Management

    Directory of Open Access Journals (Sweden)

    Yan Li

    2016-12-01

    Full Text Available With the growing popularity of data analytics and data science in the field of environmental risk management, a formalized Knowledge Discovery via Data Analytics (KDDA process that incorporates all applicable analytical techniques for a specific environmental risk management problem is essential. In this emerging field, there is limited research dealing with the use of decision support to elicit environmental risk management (ERM objectives and identify analytical goals from ERM decision makers. In this paper, we address problem formulation in the ERM understanding phase of the KDDA process. We build a DM3 ontology to capture ERM objectives and to inference analytical goals and associated analytical techniques. A framework to assist decision making in the problem formulation process is developed. It is shown how the ontology-based knowledge system can provide structured guidance to retrieve relevant knowledge during problem formulation. The importance of not only operationalizing the KDDA approach in a real-world environment but also evaluating the effectiveness of the proposed procedure is emphasized. We demonstrate how ontology inferencing may be used to discover analytical goals and techniques by conceptualizing Hazardous Air Pollutants (HAPs exposure shifts based on a multilevel analysis of the level of urbanization (and related economic activity and the degree of Socio-Economic Deprivation (SED at the local neighborhood level. The HAPs case highlights not only the role of complexity in problem formulation but also the need for integrating data from multiple sources and the importance of employing appropriate KDDA modeling techniques. Challenges and opportunities for KDDA are summarized with an emphasis on environmental risk management and HAPs.

  8. Microextraction Techniques Coupled to Liquid Chromatography with Mass Spectrometry for the Determination of Organic Micropollutants in Environmental Water Samples

    Directory of Open Access Journals (Sweden)

    Mª Esther Torres Padrón

    2014-07-01

    Full Text Available Until recently, sample preparation was carried out using traditional techniques, such as liquid–liquid extraction (LLE, that use large volumes of organic solvents. Solid-phase extraction (SPE uses much less solvent than LLE, although the volume can still be significant. These preparation methods are expensive, time-consuming and environmentally unfriendly. Recently, a great effort has been made to develop new analytical methodologies able to perform direct analyses using miniaturised equipment, thereby achieving high enrichment factors, minimising solvent consumption and reducing waste. These microextraction techniques improve the performance during sample preparation, particularly in complex water environmental samples, such as wastewaters, surface and ground waters, tap waters, sea and river waters. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS and time-of-flight mass spectrometric (TOF/MS techniques can be used when analysing a broad range of organic micropollutants. Before separating and detecting these compounds in environmental samples, the target analytes must be extracted and pre-concentrated to make them detectable. In this work, we review the most recent applications of microextraction preparation techniques in different water environmental matrices to determine organic micropollutants: solid-phase microextraction SPME, in-tube solid-phase microextraction (IT-SPME, stir bar sorptive extraction (SBSE and liquid-phase microextraction (LPME. Several groups of compounds are considered organic micropollutants because these are being released continuously into the environment. Many of these compounds are considered emerging contaminants. These analytes are generally compounds that are not covered by the existing regulations and are now detected more frequently in different environmental compartments. Pharmaceuticals, surfactants, personal care products and other chemicals are considered micropollutants. These

  9. Experience with environmental sampling at gas centrifuge enrichment plants

    International Nuclear Information System (INIS)

    Ekenstam, G. af; Bush, W.; Janov, J.; Kuhn, E.; Ryjinski, M.

    2001-01-01

    Environmental sampling has been used routinely by the IAEA since 1996 after the IAEA Board of Governors approved it in March 1995 as a new technique to strengthen safeguards and improve efficiency. In enrichment plants it is used to confirm that there has been no production of highly enriched uranium (HEU), or production of uranium at above the declared enrichment. The use of environmental sampling is based on the assumption that every process, no matter how leak tight, will release small amounts of process material to the environment. Even though these releases of nuclear material are extremely small in gas centrifuge enrichment plants, and well below levels of concern from a health physics and safety standpoint, they are detectable and their analysis provides an indication of the enrichment of the material that has been processed in the plant. The environmental samples at enrichment plants are collected by swiping selected areas of the plant with squares of cotton cloth (10x10 cm) from sampling kits prepared in ultra clean condition. The squares of cotton cloth sealed in plastic bags are sent for analysis to the Network Analytical Laboratories. The analysis includes the measurement of the uranium isotopic composition in uranium-containing particles by Thermal lonization Mass Spectroscopy (TIMS) or Secondary ION Mass Spectroscopy (SIMS). Since the implementation of environmental sampling, swipes have been collected from 240 sampling points at three gas centrifuge plants of URENCO, which have a total throughput of more than 8,000 tonnes of uranium per year. The particle analysis results generally reflected the known operational history of the plants and confirmed that they had only been operated to produce uranium with enrichment less than 5% 235 U. The information about the content of the minor isotopes 234 U and 236 U also indicates that depleted and recycled uranium were sometimes used as feed materials in some plants. An example is given of the TIMS particle

  10. Establishment of a clean laboratory for ultra trace analysis of nuclear materials in safeguards environmental samples

    International Nuclear Information System (INIS)

    Hanzawa, Yukiko; Magara, Masaaki; Watanabe, Kazuo

    2003-01-01

    The Japan Atomic Energy Research Institute has established a cleanroom facility with cleanliness of ISO Class 5: the Clean Laboratory for Environmental Analysis and Research (CLEAR). It was designed to be used for the analysis of nuclear materials in environmental samples mainly for the safeguards, in addition to the Comprehensive Nuclear-Test-Ban Treaty verification and research on environmental sciences. The CLEAR facility was designed to meet conflicting requirements of a cleanroom and for handling of nuclear materials according to Japanese regulations, i.e., to avoid contamination from outside and to contain nuclear materials inside the facility. This facility has been intended to be used for wet chemical treatment, instrumental analysis and particle handling. A fume-hood to provide a clean work surface for handling of nuclear materials was specially designed. Much attention was paid to the selection of construction materials for use to corrosive acids. The performance of the cleanroom and analytical background in the laboratory are discussed. This facility has satisfactory specification required for joining the International Atomic Energy Agency Network of Analytical Laboratories. It can be concluded that the CLEAR facility enables analysis of ultra trace amounts of nuclear materials at sub-pictogram level in environmental samples. (author)

  11. Determination of 22 elements in Marine Environmental Samples in special areas at the South of Vietnam

    International Nuclear Information System (INIS)

    Nguyen Ngoc Tuan; Nguyen Giang; Nguyen Thanh Tam; Truong Phuong Mai

    2007-01-01

    In 2007 year, we continued to determine the contents of 22 elements in marine environmental samples such as marine sediment, seawater and marine creature. The methods for the determination of elements in these objects are Neutron Activation Analysis and Atomic Absorption Spectrophotometer. The obtained analytical results are a database to monitor marine environmental pollution and to evaluate the impact of exploitation of rare earth- radioactive ores near by the sea coast; exploitation of crude oil in offshore and technology activities at the south of Vietnam in the future. The analytical results of toxic and trace element contents are also to attend the Forum for Nuclear Cooperation of Asia (FNCA) in which Vietnam is one of nine member counties. The analytical results have been presented in the FNCA 2007 workshop on utilization of the research reactor from 28 September-02 October in Serpong, Indonesia. (author)

  12. Determination of 241Am and 244Cm in environmental samples

    International Nuclear Information System (INIS)

    Bonino, N.O.; Grinman, A.D.R.; Serdeiro, N.H.

    1998-01-01

    The present technique describes a method to separate, purify and measure low levels of americium and curium in different environmental samples such as sediments, soils, water, vegetables, and air filters. The determination of radionuclides in theses environmental matrices have analytical problems, since a simple method doesn't exist for the purification, which is indispensable for its later measuring alpha spectrometry. The developed technique consist on taking an aliquot of the sample to analyze, to add tracer as americium 243 and curium 242, and to dissolve the matrix in a such way to have a clear solution. For the isolation of the americium and curium of the other actinides ar used as separation techniques: precipitation with Fe 3+ , anionic and cationic exchange, and extraction with a appropriate organic solvent. The purification of the americium and curium is followed by the electrodeposition habitually used. The measurement is carried out by alpha spectrometry with a detector of implanted ion. The detection limit for this techniques is of 0,002 Bq/l or 0,2 mBq in the case of filters. (author)

  13. Evaluation of analytical results on DOE Quality Assessment Program Samples

    International Nuclear Information System (INIS)

    Jaquish, R.E.; Kinnison, R.R.; Mathur, S.P.; Sastry, R.

    1985-01-01

    Criteria were developed for evaluating the participants analytical results in the DOE Quality Assessment Program (QAP). Historical data from previous QAP studies were analyzed using descriptive statistical methods to determine the interlaboratory precision that had been attained. Performance criteria used in other similar programs were also reviewed. Using these data, precision values and control limits were recommended for each type of analysis performed in the QA program. Results of the analysis performed by the QAP participants on the November 1983 samples were statistically analyzed and evaluated. The Environmental Measurements Laboratory (EML) values were used as the known values and 3-sigma precision values were used as control limits. Results were submitted by 26 participating laboratories for 49 different radionuclide media combinations. The participants reported 419 results and of these, 350 or 84% were within control limits. Special attention was given to the data from gamma spectral analysis of air filters and water samples. both normal probability and box plots were prepared for each nuclide to help evaluate the distribution of the data. Results that were outside the expected range were identified and suggestions made that laboratories check calculations, and procedures on these results

  14. Final report on the proficiency test of the Analytical Laboratories for the Measurement of Environmental Radioactivity (ALMERA) network

    International Nuclear Information System (INIS)

    Shakhashiro, A.; Radecki, Z.; Trinkl, A.; Sansone, U.; Benesch, T.

    2005-08-01

    This report presents the statistical evaluation of results from the analysis of 12 radionuclides in 8 samples within the frame of the First Proficiency Test of Analytical Laboratories for the Measurement Environmental RAdioactivity (ALMERA) organized in 2001-2002 by the Chemistry Unit, Agency's Laboratory in Seibersdorf. The results were evaluated by using appropriate statistical means to assess laboratory analytical performance and to estimate the overall performance for the determination of each radionuclide. Evaluation of the analytical data for gamma emitting radionuclides showed that 68% of data obtained a 'Passed' final score for both the trueness and precision criteria applied to this exercise. However, transuranic radionuclides obtained only 58% for the same criteria. (author)

  15. Rapid Determination of Plutonium Isotopes in Environmental Samples Using Sequential Injection Extraction Chromatography and Detection by Inductively Coupled Plasma Mass Spectrometry

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2009-01-01

    This article presents an automated method for the rapid determination of 239Pu and 240Pu in various environmental samples. The analytical method involves the in-line separation of Pu isotopes using extraction chromatography (TEVA) implemented in a sequential injection (SI) network followed...... by detection of isolated analytes with inductively coupled plasma mass spectrometry (ICP-MS). The method has been devised for the determination of Pu isotopes at environmentally relevant concentrations, whereby it has been successfully applied to the analyses of large volumes/amounts of samples, for example......, 100−200 g of soil and sediment, 20 g of seaweed, and 200 L of seawater following analyte preconcentration. The investigation of the separation capability of the assembled SI system revealed that up to 200 g of soil or sediment can be treated using a column containing about 0.70 g of TEVA resin...

  16. Experiences performed at the C:R: Saluggia of ENEA in low-level determination of plutonium in biological and environmental samples

    International Nuclear Information System (INIS)

    Spezzano, Pasquale

    1997-10-01

    This report describes some experiences performed at the Research Center Saluggia of ENEA concerning low-level determination of plutonium in biological and environmental samples, with discussions of practical analytical problems. The main characteristics and properties of plutonium with emphasis to aqueous solutions chemistry and environmental behaviour are also reported

  17. Identification of clinical biomarkers for pre-analytical quality control of blood samples.

    Science.gov (United States)

    Kang, Hyun Ju; Jeon, Soon Young; Park, Jae-Sun; Yun, Ji Young; Kil, Han Na; Hong, Won Kyung; Lee, Mee-Hee; Kim, Jun-Woo; Jeon, Jae-Pil; Han, Bok Ghee

    2013-04-01

    Pre-analytical conditions are key factors in maintaining the high quality of biospecimens. They are necessary for accurate reproducibility of experiments in the field of biomarker discovery as well as achieving optimal specificity of laboratory tests for clinical diagnosis. In research at the National Biobank of Korea, we evaluated the impact of pre-analytical conditions on the stability of biobanked blood samples by measuring biochemical analytes commonly used in clinical laboratory tests. We measured 10 routine laboratory analytes in serum and plasma samples from healthy donors (n = 50) with a chemistry autoanalyzer (Hitachi 7600-110). The analyte measurements were made at different time courses based on delay of blood fractionation, freezing delay of fractionated serum and plasma samples, and at different cycles (0, 1, 3, 6, 9) of freeze-thawing. Statistically significant changes from the reference sample mean were determined using the repeated-measures ANOVA and the significant change limit (SCL). The serum levels of GGT and LDH were changed significantly depending on both the time interval between blood collection and fractionation and the time interval between fractionation and freezing of serum and plasma samples. The glucose level was most sensitive only to the elapsed time between blood collection and centrifugation for blood fractionation. Based on these findings, a simple formula (glucose decrease by 1.387 mg/dL per hour) was derived to estimate the length of time delay after blood collection. In addition, AST, BUN, GGT, and LDH showed sensitive responses to repeated freeze-thaw cycles of serum and plasma samples. These results suggest that GGT and LDH measurements can be used as quality control markers for certain pre-analytical conditions (eg, delayed processing or repeated freeze-thawing) of blood samples which are either directly used in the laboratory tests or stored for future research in the biobank.

  18. Determination of Sr-90 in environmental samples using solid phase extraction disk

    International Nuclear Information System (INIS)

    Zal U'yun Wan Mahmood

    2002-01-01

    A method is described for determination of Sr-90 in environmental samples using solid phase extraction disk (Empore TM Strontium Rad Disk) and GM counter. To determine the optimum condition for capacity of Empore TM Strontium Rad Disk, its characterization studies such as the effects Sr content, acidity (molarity) of acids, presence of Ca 2+ and other major ions (Na + , Mg 2+ etc), influence of interference (Pb and Bi) and others were carried out. An optimized the using of Empore TM Strontium Rad Disk for determination of Sr-90 was validated by application to environmental samples. Quantitative recoveries above 95%for Sr (stable) were recorded in 6M HCl condition. Typical environmental samples may contain an assortment of anionic and cationic species, but in general, Empore TM Strontium Rad Disk has enough capacity to effectively separate Sr for wide variety of aqueous solutions. Sr recovery in a matrix-free or the content of matrix less than 300 mg/sample is typically greater than 99% is reported in this research work. In particular, sample, which may contain interference such as Pb and Bi would require an addition separation step before processing to ensure an accurate measurement of Sr. In this research work, radiotracer 85 Sr was used to monitor the behavior of Sr and calculation its recovery. For analytical methods that can count Y-90, the Sr-90 activity/concentration in environmental sample was calculated. The concentration of Sr-90 in ash sample (Quality Controled Sample) of 276 ± 18 Bq/kg ash was determined from Y-90 activity. The relative percent difference of 1.1% was achievable for Empore TM Sr-Rad Disk methods when compared to the conventional method (fumed-HNO 3 method) - 279 ± 11 Bq/kg ash. (Author)

  19. Sampling and analyte enrichment strategies for ambient mass spectrometry.

    Science.gov (United States)

    Li, Xianjiang; Ma, Wen; Li, Hongmei; Ai, Wanpeng; Bai, Yu; Liu, Huwei

    2018-01-01

    Ambient mass spectrometry provides great convenience for fast screening, and has showed promising potential in analytical chemistry. However, its relatively low sensitivity seriously restricts its practical utility in trace compound analysis. In this review, we summarize the sampling and analyte enrichment strategies coupled with nine modes of representative ambient mass spectrometry (desorption electrospray ionization, paper vhspray ionization, wooden-tip spray ionization, probe electrospray ionization, coated blade spray ionization, direct analysis in real time, desorption corona beam ionization, dielectric barrier discharge ionization, and atmospheric-pressure solids analysis probe) that have dramatically increased the detection sensitivity. We believe that these advances will promote routine use of ambient mass spectrometry. Graphical abstract Scheme of sampling stretagies for ambient mass spectrometry.

  20. Automated Ground-Water Sampling and Analysis of Hexavalent Chromium using a “Universal” Sampling/Analytical System

    Directory of Open Access Journals (Sweden)

    Richard J. Venedam

    2005-02-01

    Full Text Available The capabilities of a “universal platform” for the deployment of analyticalsensors in the field for long-term monitoring of environmental contaminants were expandedin this investigation. The platform was previously used to monitor trichloroethene inmonitoring wells and at groundwater treatment systems (1,2. The platform was interfacedwith chromium (VI and conductivity analytical systems to monitor shallow wells installedadjacent to the Columbia River at the 100-D Area of the Hanford Site, Washington. Agroundwater plume of hexavalent chromium is discharging into the Columbia River throughthe gravels beds used by spawning salmon. The sampling/analytical platform was deployedfor the purpose of collecting data on subsurface hexavalent chromium concentrations atmore frequent intervals than was possible with the previous sampling and analysis methodsemployed a the Site.

  1. Comparative study of modern extraction techniques for the determination of environmental samples (M14)

    International Nuclear Information System (INIS)

    Gfrerer, M.; Lankmayr, E.

    2002-01-01

    Full text: The aim of any extraction method in analytical chemistry is, to effectively separate the analytes from the matrix. The whole step should be fast and quantitative with minimal solvent and time required. The classical Soxhlet extraction usually requires large volumes (up to 200 ml) of solvent to be refluxed through the solid samples for several hours. Therefore, in the last decades, alternatives for this extraction method have been presented and investigated such as ultrasonic extraction (UE), supercritical fluid extraction (SFE), accelerated solvent extraction (ASE), microwave-assisted extraction (MAE) and fluidized-bed extraction (FBE). The actual choice for analytical application is frequently the initial capital cost, operating costs, simplicity of operation, amount of organic solvent required and sample throughput. Since sample preparation is a critical step in the analytical cycle, special care has to be taken for an accurate choice and optimization of extraction techniques and clean-up procedures. Therefore, MAE and FBE were investigated for their influential extraction parameters and these parameters were optimized for the extraction of organochlorine biocides, polychlorinated biphenyls and polycyclic aromatic hydrocarbons from environmental matrices like soil, sediment and sewage sludge. The extraction yields were compared with those obtained by Soxhlet extraction performed following DIN-methods. Finally, the optimized modern methods were validated by systematic experiments with certified reference materials. Refs. 3 (author)

  2. Environmental surveillance master sampling schedule

    International Nuclear Information System (INIS)

    Bisping, L.E.

    1997-01-01

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest National Laboratory (PNNL)(a) for the US Department of Energy (DOE). This document contains the planned 1997 schedules for routine collection of samples for the Surface Environmental Surveillance Project (SESP) and Drinking Water Monitoring Project. In addition, Section 3.0, Biota, also reflects a rotating collection schedule identifying the year a specific sample is scheduled for collection. The purpose of these monitoring projects is to evaluate levels of radioactive and nonradioactive pollutants in the Hanford environs, as required in DOE Order 5400.1, General Environmental Protection Program, and DOE Order 5400.5, Radiation Protection of the Public and the Environment. The sampling methods will be the same as those described in the Environmental Monitoring Plan, US Department of Energy, Richland Operations Office, DOE/RL91-50, Rev. 1, US Department of Energy, Richland, Washington

  3. Quality assurance program for determining the radioactivity in environmental samples at the Institute of Nuclear Energy Research in Taiwan

    International Nuclear Information System (INIS)

    Gone, J.K.; Wang, T.W.

    2000-01-01

    Interest in determining radioactivity in environmental samples has increased considerably in recent years after the Chernobyl accident in 1986. Environmental monitoring programs have been set up in different countries to measure the trace amount of radionuclides in the environment, and quality of the analytical results on these samples is important because the regulation and safety concerns. A good quality assurance program is essential to provide accurate information for the regulatory body and environmentalists to set proper reactions to protect the environment, and a good analytical result is also important for scientists to determine the transfer of radionuclides between environmental matrices. The Institute of Nuclear Energy Research (lNER) in Taiwan has been working on radionuclide analysis in environmental samples for years, and it's environmental media radioanalytical laboratory (EMRAL) has recently upgraded its quality assurance program for the international standard ISO/lEC guide 25 requirements. The general requirements of lSO/lEC guide 25 has been adapted by the Chinese National Laboratory Accreditation (CNLA) of Taiwan, and CNLA is also a member of International Laboratory Accreditation Cooperation (ILAC) and Asia Pacific Laboratory Accreditation Cooperation (APLAC). This paper summarizes the quality assurance program of lNER's EMRAL. It covers both management and technical sections. These sections have ensured the quality of INER's EMRAL, and they can be applied to different laboratories in the future. (author)

  4. Quality assurance program for determining the radioactivity in environmental samples at the Institute of Nuclear Energy Research in Taiwan

    Energy Technology Data Exchange (ETDEWEB)

    Gone, J.K. [TRR-II Project Team, Institute of Nuclear Energy Research, Taoyuan, Taiwan (China); Wang, T.W. [Division of Health Physics, Institute of Nuclear Energy Research, Taoyuan, Taiwan (China)

    2000-05-01

    Interest in determining radioactivity in environmental samples has increased considerably in recent years after the Chernobyl accident in 1986. Environmental monitoring programs have been set up in different countries to measure the trace amount of radionuclides in the environment, and quality of the analytical results on these samples is important because the regulation and safety concerns. A good quality assurance program is essential to provide accurate information for the regulatory body and environmentalists to set proper reactions to protect the environment, and a good analytical result is also important for scientists to determine the transfer of radionuclides between environmental matrices. The Institute of Nuclear Energy Research (lNER) in Taiwan has been working on radionuclide analysis in environmental samples for years, and it's environmental media radioanalytical laboratory (EMRAL) has recently upgraded its quality assurance program for the international standard ISO/lEC guide 25 requirements. The general requirements of lSO/lEC guide 25 has been adapted by the Chinese National Laboratory Accreditation (CNLA) of Taiwan, and CNLA is also a member of International Laboratory Accreditation Cooperation (ILAC) and Asia Pacific Laboratory Accreditation Cooperation (APLAC). This paper summarizes the quality assurance program of lNER's EMRAL. It covers both management and technical sections. These sections have ensured the quality of INER's EMRAL, and they can be applied to different laboratories in the future. (author)

  5. Correlated Raman micro-spectroscopy and scanning electron microscopy analyses of flame retardants in environmental samples: a micro-analytical tool for probing chemical composition, origin and spatial distribution.

    Science.gov (United States)

    Ghosal, Sutapa; Wagner, Jeff

    2013-07-07

    We present correlated application of two micro-analytical techniques: scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDS) and Raman micro-spectroscopy (RMS) for the non-invasive characterization and molecular identification of flame retardants (FRs) in environmental dusts and consumer products. The SEM/EDS-RMS technique offers correlated, morphological, molecular, spatial distribution and semi-quantitative elemental concentration information at the individual particle level with micrometer spatial resolution and minimal sample preparation. The presented methodology uses SEM/EDS analyses for rapid detection of particles containing FR specific elements as potential indicators of FR presence in a sample followed by correlated RMS analyses of the same particles for characterization of the FR sub-regions and surrounding matrices. The spatially resolved characterization enabled by this approach provides insights into the distributional heterogeneity as well as potential transfer and exposure mechanisms for FRs in the environment that is typically not available through traditional FR analysis. We have used this methodology to reveal a heterogeneous distribution of highly concentrated deca-BDE particles in environmental dust, sometimes in association with identifiable consumer materials. The observed coexistence of deca-BDE with consumer material in dust is strongly indicative of its release into the environment via weathering/abrasion of consumer products. Ingestion of such enriched FR particles in dust represents a potential for instantaneous exposure to high FR concentrations. Therefore, correlated SEM/RMS analysis offers a novel investigative tool for addressing an area of important environmental concern.

  6. Supercritical fluid extraction and ultra performance liquid chromatography of respiratory quinones for microbial community analysis in environmental and biological samples.

    Science.gov (United States)

    Hanif, Muhammad; Atsuta, Yoichi; Fujie, Koichi; Daimon, Hiroyuki

    2012-03-05

    Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA) detector was successfully applied to the simultaneous determination of ubiquinones (UQ) and menaquinones (MK) without tedious pretreatment. Supercritical carbon dioxide (scCO(2)) extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost) and biological samples (swine and Japanese quail feces).

  7. Environmental sampling accounting at the Savannah River Plant

    International Nuclear Information System (INIS)

    Zeigler, C.C.; Wood, M.B.

    1978-06-01

    At the Savannah River Plant Environmental Monitoring Laboratories, a computer-based systematic accounting method was developed to ensure that all scheduled samples are collected, processed through the laboratory, and counted without delay. The system employs an IBM 360/195 computer with a magnetic tape master file, an on-line disk file, and cathode ray tube (CRT) terminals. Scheduling and accounting are accomplished by using computer-generated schedules, collection labels, and output/input cards. For each scheduled sample and analysis, a printed card is issued for collection, laboratory analysis, and counting. The cards also contain information needed by personnel performing the jobs, such as sample location, aliquot to be processed, or procedure number. Manual entries are made on the cards when each step in the process is completed. Additional pertinent data are also manually entered on the cards; e.g., entries are made explaining why a sample is not collected, the sample aliquot in the event a nonstandard aliquot is processed, field measurement results, and analytical results. These manually entered data are keypunched and read into the computer files. The computer files are audited daily, and summaries of samples not processed in pre-established normal time intervals are issued. The progress of sample analyses can also be readily determined at any time using the CRT terminal. Historic data are also maintained on magnetic tape and workload summaries are issued showing the number of samples and number of determinations per month

  8. Sample preparation method for the speciation of polybrominated diphenyl ethers and their methoxylated and hydroxylated analogues in diverse environmental matrices.

    Science.gov (United States)

    Sun, Jianteng; Liu, Jiyan; Liu, Qian; Qu, Guangbo; Ruan, Ting; Jiang, Guibin

    2012-01-15

    A reliable analytical method was developed here for the simultaneous separation, identification and quantification of ten polybrominated diphenyl ethers (PBDEs), nine methoxylated PBDEs (MeO-PBDEs) and ten hydroxylated PBDEs (OH-PBDEs) in various environmental matrices, including water, soil, sediment, plant, mollusk and fish. PBDEs and MeO-PBDEs were measured by gas chromatography coupled with mass spectrometry (GC/MS) and liquid chromatography coupled with electrospray ionization (negative)-tandem quadrupole mass spectrometry (LC/ESI(-)-MS/MS) for the separation and determination of OH-PBDEs without prior derivatization. After preliminary sample cleaning using acid silica gel, water-impregnated silica column separation of PBDEs, MeO-PBDEs and OH-PBDEs was proved to be rapid, simple, and efficient. For phenolic analytes, the method detection limits (MDLs) were 3.2-11.6pg/L in water sample and 2.8-18.4pg/g dry weight in solid samples. For neutral compounds, MDLs were 48.8-150.3pg/L in water sample and 46.5-170.8pg/g dry weight in solid samples. The method was validated using six kinds of environmental samples spiked with all analytes at three concentration levels (0.3ng, 2ng and 5ng, respectively) for recovery (71-113%) and repeatability determination (4-12%RSD). Copyright © 2011 Elsevier B.V. All rights reserved.

  9. Green sample preparation for liquid chromatography and capillary electrophoresis of anionic and cationic analytes.

    Science.gov (United States)

    Wuethrich, Alain; Haddad, Paul R; Quirino, Joselito P

    2015-04-21

    A sample preparation device for the simultaneous enrichment and separation of cationic and anionic analytes was designed and implemented in an eight-channel configuration. The device is based on the use of an electric field to transfer the analytes from a large volume of sample into small volumes of electrolyte that was suspended into two glass micropipettes using a conductive hydrogel. This simple, economical, fast, and green (no organic solvent required) sample preparation scheme was evaluated using cationic and anionic herbicides as test analytes in water. The analytical figures of merit and ecological aspects were evaluated against the state-of-the-art sample preparation, solid-phase extraction. A drastic reduction in both sample preparation time (94% faster) and resources (99% less consumables used) was observed. Finally, the technique in combination with high-performance liquid chromatography and capillary electrophoresis was applied to analysis of quaternary ammonium and phenoxypropionic acid herbicides in fortified river water as well as drinking water (at levels relevant to Australian guidelines). The presented sustainable sample preparation approach could easily be applied to other charged analytes or adopted by other laboratories.

  10. Environmental concentrations of engineered nanomaterials: Review of modeling and analytical studies

    International Nuclear Information System (INIS)

    Gottschalk, Fadri; Sun, TianYin; Nowack, Bernd

    2013-01-01

    Scientific consensus predicts that the worldwide use of engineered nanomaterials (ENM) leads to their release into the environment. We reviewed the available literature concerning environmental concentrations of six ENMs (TiO 2 , ZnO, Ag, fullerenes, CNT and CeO 2 ) in surface waters, wastewater treatment plant effluents, biosolids, sediments, soils and air. Presently, a dozen modeling studies provide environmental concentrations for ENM and a handful of analytical works can be used as basis for a preliminary validation. There are still major knowledge gaps (e.g. on ENM production, application and release) that affect the modeled values, but over all an agreement on the order of magnitude of the environmental concentrations can be reached. True validation of the modeled values is difficult because trace analytical methods that are specific for ENM detection and quantification are not available. The modeled and measured results are not always comparable due to the different forms and sizes of particles that these two approaches target. -- Highlights: •Modeled environmental concentrations of engineered nanomaterials are reviewed. •Measured environmental concentrations of engineered nanomaterials are reviewed. •Possible validation of modeled data by measurements is critically evaluated. •Different approaches in modeling and measurement methods complicate validation. -- Modeled and measured environmental concentrations of engineered nanomaterials are reviewed and critically discussed

  11. INEL Sample Management Office

    International Nuclear Information System (INIS)

    Watkins, C.

    1994-01-01

    The Idaho National Engineering Laboratory (INEL) Sample Management Office (SMO) was formed as part of the EG ampersand G Idaho Environmental Restoration Program (ERP) in June, 1990. Since then, the SMO has been recognized and sought out by other prime contractors and programs at the INEL. Since December 1991, the DOE-ID Division Directors for the Environmental Restoration Division and Waste Management Division supported the expansion of the INEL ERP SMO into the INEL site wide SMO. The INEL SMO serves as a point of contact for multiple environmental analytical chemistry and laboratory issues (e.g., capacity, capability). The SMO chemists work with project managers during planning to help develop data quality objectives, select appropriate analytical methods, identify special analytical services needs, identify a source for the services, and ensure that requirements for sampling and analysis (e.g., preservations, sample volumes) are clear and technically accurate. The SMO chemists also prepare work scope statements for the laboratories performing the analyses

  12. Development for ultra-trace analysis method of U and Pu in safeguards environmental samples at the clean facility

    International Nuclear Information System (INIS)

    Takahashi, Masato; Magara, Masaaki; Sakurai, Satoshi

    2002-01-01

    Based on the strengthen safeguard program of the IAEA to detect undeclared nuclear activities and nuclear materials, the method of precise and accurate isotope ratio determination for uranium and plutonium in the environmental samples (cotton swipes) has been developed at JAERI. The samples should be treated in clean environment in order to secure the analytical reliability by eliminating external contamination from the samples containing trace amount of uranium and plutonium. Since the measurement by ICP-MS is favorable to bulk analysis from view points of analytical capacity and operation simplicity, we have studied sample preparation procedures for the trace amount of uranium and plutonium to be applied to ICP-MS. Up to the present, interfering factors involved during analytical processes and the ICP-MS measurement of uranium and plutonium were examined. As a result, uranium isotope measurement more than 100 pg became possible at JAERI clean facility by diminishing uranium blank introduced in the entire sample treatment procedure. And also, the estimation of plutonium recovery yield and uranium decontamination factor suggested the possibility in plutonium isotope measurement more than 100 fg. (author)

  13. Environmental surveillance master sampling schedule

    International Nuclear Information System (INIS)

    Bisping, L.E.

    1994-02-01

    This document contains the planned 1994 schedules for routine collection of samples for the Surface Environmental Surveillance Project (SESP), Drinking Water Project, and Ground-Water Surveillance Project. Samples are routinely collected for the SESP and analyzed to determine the quality of air, surface water, soil, sediment, wildlife, vegetation, foodstuffs, and farm products at Hanford Site and surrounding communities. The responsibility for monitoring the onsite drinking water falls outside the scope of the SESP. The Hanford Environmental Health Foundation is responsible for monitoring the nonradiological parameters as defined in the National Drinking Water Standards while PNL conducts the radiological monitoring of the onsite drinking water. PNL conducts the drinking water monitoring project concurrent with the SESP to promote efficiency and consistency, utilize the expertise developed over the years, and reduce costs associated with management, procedure development, data management, quality control and reporting. The ground-water sampling schedule identifies ground-water sampling events used by PNL for environmental surveillance of the Hanford Site

  14. Environmental surveillance master sampling schedule

    Energy Technology Data Exchange (ETDEWEB)

    Bisping, L.E.

    1994-02-01

    This document contains the planned 1994 schedules for routine collection of samples for the Surface Environmental Surveillance Project (SESP), Drinking Water Project, and Ground-Water Surveillance Project. Samples are routinely collected for the SESP and analyzed to determine the quality of air, surface water, soil, sediment, wildlife, vegetation, foodstuffs, and farm products at Hanford Site and surrounding communities. The responsibility for monitoring the onsite drinking water falls outside the scope of the SESP. The Hanford Environmental Health Foundation is responsible for monitoring the nonradiological parameters as defined in the National Drinking Water Standards while PNL conducts the radiological monitoring of the onsite drinking water. PNL conducts the drinking water monitoring project concurrent with the SESP to promote efficiency and consistency, utilize the expertise developed over the years, and reduce costs associated with management, procedure development, data management, quality control and reporting. The ground-water sampling schedule identifies ground-water sampling events used by PNL for environmental surveillance of the Hanford Site.

  15. Measurement of extremely (2) H-enriched water samples by laser spectrometry: application to batch electrolytic concentration of environmental tritium samples.

    Science.gov (United States)

    Wassenaar, L I; Kumar, B; Douence, C; Belachew, D L; Aggarwal, P K

    2016-02-15

    Natural water samples artificially or experimentally enriched in deuterium ((2) H) at concentrations up to 10,000 ppm are required for various medical, environmental and hydrological tracer applications, but are difficult to measure using conventional stable isotope ratio mass spectrometry. Here we demonstrate that off-axis integrated cavity output (OA-ICOS) laser spectrometry, along with (2) H-enriched laboratory calibration standards and appropriate analysis templates, allows for low-cost, fast, and accurate determinations of water samples having δ(2) HVSMOW-SLAP values up to at least 57,000 ‰ (~9000 ppm) at a processing rate of 60 samples per day. As one practical application, extremely (2) H-enriched samples were measured by laser spectrometry and compared to the traditional (3) H Spike-Proxy method in order to determine tritium enrichment factors in the batch electrolysis of environmental waters. Highly (2) H-enriched samples were taken from different sets of electrolytically concentrated standards and low-level (tritium samples, and all cases returned accurate and precise initial low-level (3) H results. The ability to quickly and accurately measure extremely (2) H-enriched waters by laser spectrometry will facilitate the use of deuterium as a tracer in numerous environmental and other applications. For low-level tritium operations, this new analytical ability facilitated a 10-20 % increase in sample productivity through the elimination of spike standards and gravimetrics, and provides immediate feedback on electrolytic enrichment cell performance. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  16. A sample preparation method for recovering suppressed analyte ions in MALDI TOF MS

    NARCIS (Netherlands)

    Lou, X.; Waal, de B.F.M.; Milroy, L.G.; Dongen, van J.L.J.

    2015-01-01

    In matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI TOF MS), analyte signals can be substantially suppressed by other compounds in the sample. In this technical note, we describe a modified thin-layer sample preparation method that significantly reduces the analyte

  17. Stability of volatile organics in environmental soil samples. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Maskarinec, M.P.; Bayne, C.K.; Jenkins, R.A.; Johnson, L.H.; Holladay, S.K.

    1992-11-01

    This report focuses on data generated for the purpose of establishing the stability of 19 volatile organic compounds in environmental soil samples. The study was carried out over a 56 day (for two soils) and a 111 day (for one reference soil) time frame and took into account as many variables as possible within the constraints of budget and time. The objectives of the study were: 1) to provide a data base which could be used to provide guidance on pre-analytical holding times for regulatory purposes; and 2) to provide a basis for the evaluation of data which is generated outside of the currently allowable holding times.

  18. Improvements to sample processing and measurement to enable more widespread environmental application of tritium.

    Science.gov (United States)

    Moran, James; Alexander, Thomas; Aalseth, Craig; Back, Henning; Mace, Emily; Overman, Cory; Seifert, Allen; Freeburg, Wilcox

    2017-08-01

    Previous measurements have demonstrated the wealth of information that tritium (T) can provide on environmentally relevant processes. We present modifications to sample preparation approaches that enable T measurement by proportional counting on small sample sizes equivalent to 120mg of water and demonstrate the accuracy of these methods on a suite of standardized water samples. We identify a current quantification limit of 92.2 TU which, combined with our small sample sizes, correlates to as little as 0.00133Bq of total T activity. This enhanced method should provide the analytical flexibility needed to address persistent knowledge gaps in our understanding of both natural and artificial T behavior in the environment. Copyright © 2017. Published by Elsevier Ltd.

  19. Comparison of soil sampling and analytical methods for asbestos at the Sumas Mountain Asbestos Site-Working towards a toolbox for better assessment.

    Science.gov (United States)

    Wroble, Julie; Frederick, Timothy; Frame, Alicia; Vallero, Daniel

    2017-01-01

    Established soil sampling methods for asbestos are inadequate to support risk assessment and risk-based decision making at Superfund sites due to difficulties in detecting asbestos at low concentrations and difficulty in extrapolating soil concentrations to air concentrations. Environmental Protection Agency (EPA)'s Office of Land and Emergency Management (OLEM) currently recommends the rigorous process of Activity Based Sampling (ABS) to characterize site exposures. The purpose of this study was to compare three soil analytical methods and two soil sampling methods to determine whether one method, or combination of methods, would yield more reliable soil asbestos data than other methods. Samples were collected using both traditional discrete ("grab") samples and incremental sampling methodology (ISM). Analyses were conducted using polarized light microscopy (PLM), transmission electron microscopy (TEM) methods or a combination of these two methods. Data show that the fluidized bed asbestos segregator (FBAS) followed by TEM analysis could detect asbestos at locations that were not detected using other analytical methods; however, this method exhibited high relative standard deviations, indicating the results may be more variable than other soil asbestos methods. The comparison of samples collected using ISM versus discrete techniques for asbestos resulted in no clear conclusions regarding preferred sampling method. However, analytical results for metals clearly showed that measured concentrations in ISM samples were less variable than discrete samples.

  20. Proteomic tools for environmental microbiology--a roadmap from sample preparation to protein identification and quantification.

    Science.gov (United States)

    Wöhlbrand, Lars; Trautwein, Kathleen; Rabus, Ralf

    2013-10-01

    The steadily increasing amount of (meta-)genomic sequence information of diverse organisms and habitats has a strong impact on research in microbial physiology and ecology. In-depth functional understanding of metabolic processes and overall physiological adaptation to environmental changes, however, requires application of proteomics, as the context specific proteome constitutes the true functional output of a cell. Considering the enormous structural and functional diversity of proteins, only rational combinations of various analytical approaches allow a holistic view on the overall state of the cell. Within the past decade, proteomic methods became increasingly accessible to microbiologists mainly due to the robustness of analytical methods (e.g. 2DE), and affordability of mass spectrometers and their relative ease of use. This review provides an overview on the complex portfolio of state-of-the-art proteomics and highlights the basic principles of key methods, ranging from sample preparation of laboratory or environmental samples, via protein/peptide separation (gel-based or gel-free) and different types of mass spectrometric protein/peptide analyses, to protein identification and abundance determination. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Study of New Analytical Methodologies for the Analysis of Polychlorinated Dibenzo-P-Dioxins (PcDDs) and Polychlorinated Di benzofurans (PCDFs) by Quadrupole Ion Storage Tandem-in-time Mass Spectrometry. Application to Environmental Samples

    International Nuclear Information System (INIS)

    Sanz Chichon, M. P.

    2008-01-01

    Two alternative analytical methodologies have been developed for the analysis of polychlorinated dibenzo-p-dioxins ( PCDDs) and di benzofurans (PCDFs) in environmental samples. The techniques studied have been: Pressurized Fluid Extraction (PFE) and Microwave-Assisted Extraction (MAE) versus Soxhlet extraction; the automated system Power-PrepTM versus the conventional cleanup using open chromatographic columns with different adsorbents and the application of tandem mass spectrometry (HRGC-MS/MS) versus high resolution mass spectrometry (HRGC-HRMS) for PCDD/Fs detection and quantification. (Author) 233 refs

  2. An intercomparison on radionuclides in environmental samples, Baltic-Danish co-operation project on radiation protection 2001-2003

    International Nuclear Information System (INIS)

    Nielsen, S.P.

    2004-07-01

    Sixteen laboratories participated in an intercomparison exercise carried out in 2003 on laboratory analyses of radionuclides in environmental samples. The sample types included seawater, lake water, soil, dry milk and seaweed and the exercise involved the radionuclides 137 Cs, 90 Sr, 60 Co, 239,240 Pu, 241 Am, 226 Ra, 2 40 K. The evaluation of analytical performance was based on comparison with median values, a 10% target standard deviation and statistical tests at the 99% level. For 137Cs the results from 10 out of 16 laboratories passed the evaluation tests. For 90 Sr the results from 5 out of 12 laboratories passed the evaluation tests. For 60 Co, 239,240 Pu and 241 Am two laboratories submitted results and both passed the tests. For the natural radionuclides 226 Ra, 232 Th and 40 K, only a few laboratories did not pass the tests. For all radionuclides combined, the results from 6 out of 16 laboratories passed the evaluation tests. The results indicate that for several of the laboratories there is room to improve the analytical quality on radionuclides in environmental samples to match an uncertainty corresponding to a relative standard deviation of 10%. (au)

  3. Aspects of cleaning environmental materials for multi-element analysis, e.g. plant samples

    International Nuclear Information System (INIS)

    Markert, B.

    1992-01-01

    Cleaning of samples is often the first step in the entire procedure of sample preparation in environmental trace element research. The question must generally be raised of whether cleaning is meaningful before chemical investigations with plant material (e.g. for the determination of transfer factors in the soil/plant system) or not (e.g. for food chain analysis in the plant/animal system). The most varied cleaning procedures for plant samples are currently available ranging from dry and wet wiping of the leaf or needle surface up to the complete removal of the cuticule with the aid of chlorofom. There is at present no standardized cleaning procedure for plant samples so that it is frequently not possible to compare analytical data from different working groups studying the same plant species. (orig.)

  4. The determination of arsenic, selenium, antimony, and tin in complex environmental samples by hydride generation AAS

    International Nuclear Information System (INIS)

    Johnson, D.; Beach, C.

    1990-01-01

    Hydride generation techniques are used routinely for the determination of As, Se, Sb and Sn in water samples. Advantages include high sensitivity, simplicity, and relative freedom from interferences. Continuous-flow designs greatly reduce analysis time as well as improve precision and allow for automation. However the accurate analysis of more complex environmental samples such as industrial sludges, soil samples, river sediments, and fly ash remains difficult. Numerous contributing factors influence the accuracy of the hydride technique. Sample digestion methods and sample preparation procedures are of critical importance. The digestion must adequately solubilize the elements of interest without loss by volatilization. Sample preparation procedures that guarantee the proper analyte oxidation state and eliminate the nitric acid and inter-element interferences are needed. In this study, difficult environmental samples were analyzed for As, Se, Sb, and Sn by continuous flow hydride generation. Sample preparation methods were optimized to eliminate interferences. The results of spike recovery studies will be presented. Data from the analysis of the same samples by graphite furnace AAS will be presented for comparison of accuracy, precision, and analysis time

  5. OPTIMAL METHOD FOR PREPARATION OF SILICATE ROCK SAMPLES FOR ANALYTICAL PURPOSES

    Directory of Open Access Journals (Sweden)

    Maja Vrkljan

    2004-12-01

    Full Text Available The purpose of this study was to determine an optimal dissolution method for silicate rock samples for further analytical purposes. Analytical FAAS method of determining cobalt, chromium, copper, nickel, lead and zinc content in gabbro sample and geochemical standard AGV-1 has been applied for verification. Dissolution in mixtures of various inorganic acids has been tested, as well as Na2CO3 fusion technique. The results obtained by different methods have been compared and dissolution in the mixture of HNO3 + HF has been recommended as optimal.

  6. Determination of Am-241, Cm-242 and Cm-244 in environmental samples

    International Nuclear Information System (INIS)

    Afsar, M.; Schuettelkopf, H.

    1988-01-01

    An analytical procedure for the determination of Am and Cm in environmental, liquid and gaseous effluent samples was developed. It is based on extraction chromatography with subsequent anion and cation exchange to remove matrix elements and to purify Am and Cm, which are then electrode posited from an oxalate/HCl medium. The mean value of the chemical yield is about 90%. A detection limit of 7 μBq/g is achieved. The decontamination factors for important α emitters are > 10 4 . Four analyses/week can be performed by one technician. (orig./RB) [de

  7. Supercritical Fluid Extraction and Ultra Performance Liquid Chromatography of Respiratory Quinones for Microbial Community Analysis in Environmental and Biological Samples

    Directory of Open Access Journals (Sweden)

    Koichi Fujie

    2012-03-01

    Full Text Available Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE and ultra performance liquid chromatography (UPLC method for the analysis of bacterial respiratory quinones (RQ in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA detector was successfully applied to the simultaneous determination of ubiquinones (UQ and menaquinones (MK without tedious pretreatment. Supercritical carbon dioxide (scCO2 extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost and biological samples (swine and Japanese quail feces.

  8. Sampling method of environmental radioactivity monitoring

    International Nuclear Information System (INIS)

    1984-01-01

    This manual provides sampling methods of environmental samples of airborne dust, precipitated dust, precipitated water (rain or snow), fresh water, soil, river sediment or lake sediment, discharged water from a nuclear facility, grains, tea, milk, pasture grass, limnetic organisms, daily diet, index organisms, sea water, marine sediment, marine organisms, and that for tritium and radioiodine determination for radiation monitoring from radioactive fallout or radioactivity release by nuclear facilities. This manual aims at the presentation of standard sampling procedures for environmental radioactivity monitoring regardless of monitoring objectives, and shows preservation method of environmental samples acquired at the samplingpoint for radiation counting for those except human body. Sampling techniques adopted in this manual is decided by the criteria that they are suitable for routine monitoring and any special skillfulness is not necessary. Based on the above-mentioned principle, this manual presents outline and aims of sampling, sampling position or object, sampling quantity, apparatus, equipment or vessel for sampling, sampling location, sampling procedures, pretreatment and preparation procedures of a sample for radiation counting, necessary recording items for sampling and sample transportation procedures. Special attention is described in the chapter of tritium and radioiodine because these radionuclides might be lost by the above-mentioned sample preservation method for radiation counting of less volatile radionuclides than tritium or radioiodine. (Takagi, S.)

  9. Rapid extraction and assay of uranium from environmental surface samples

    Energy Technology Data Exchange (ETDEWEB)

    Barrett, Christopher A.; Chouyyok, Wilaiwan; Speakman, Robert J.; Olsen, Khris B.; Addleman, Raymond Shane

    2017-10-01

    Extraction methods enabling faster removal and concentration of uranium compounds for improved trace and low-level assay are demonstrated for standard surface sampling material in support of nuclear safeguards efforts, health monitoring, and other nuclear analysis applications. A key problem with the existing surface sampling swipes is the requirement for complete digestion of sample and sampling matrix. This is a time-consuming and labour-intensive process that limits laboratory throughput, elevates costs, and increases background levels. Various extraction methods are explored for their potential to quickly and efficiently remove different chemical forms of uranium from standard surface sampling material. A combination of carbonate and peroxide solutions is shown to give the most rapid and complete form of uranyl compound extraction and dissolution. This rapid extraction process is demonstrated to be compatible with standard inductive coupled plasma mass spectrometry methods for uranium isotopic assay as well as screening techniques such as x-ray fluorescence. The general approach described has application beyond uranium to other analytes of nuclear forensic interest (e.g., rare earth elements and plutonium) as well as heavy metals for environmental and industrial hygiene monitoring.

  10. Hanford Site Environmental Surveillance Master Sampling Schedule

    International Nuclear Information System (INIS)

    Bisping, L.E.

    1999-01-01

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest National Laboratory (PNNL) for the U.S. Department of Energy (DOE). Sampling is conducted to evaluate levels of radioactive and nonradioactive pollutants in the Hanford environs, as required in DOE Order 5400.1, ''General Environmental protection Program,'' and DOE Order 5400.5, ''Radiation Protection of the Public and the Environment.'' The sampling methods are described in the Environmental Monitoring Plan, United States Department of Energy, Richland Operations Office, DOE/RL-91-50, Rev.2, U.S. Department of Energy, Richland, Washington. This document contains the CY1999 schedules for the routine collection of samples for the Surface Environmental Surveillance Project (SESP) and Drinking Water Monitoring Project. Each section includes the sampling location, sample type, and analyses to be performed on the sample. In some cases, samples are scheduled on a rotating basis and may not be collected in 1999 in which case the anticipated year for collection is provided. In addition, a map is included for each media showing approximate sampling locations

  11. Environmental surveillance master sampling schedule

    Energy Technology Data Exchange (ETDEWEB)

    Bisping, L.E.

    1993-01-01

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest Laboratory (PNL) for the US Department of Energy (DOE). Samples are routinely collected and analyzed to determine the quality of air, surface water, ground water, soil, sediment, wildlife, vegetation, foodstuffs, and farm products at Hanford Site and surrounding communities. This document contains the planned schedule for routine sample collection for the Surface Environmental Surveillance Project (SESP) and Drinking Water Project, and Ground-Water Surveillance Project.

  12. Applying the Analytic Hierarchy Process to Oil Sands Environmental Compliance Risk Management

    Science.gov (United States)

    Roux, Izak Johannes, III

    Oil companies in Alberta, Canada, invested $32 billion on new oil sands projects in 2013. Despite the size of this investment, there is a demonstrable deficiency in the uniformity and understanding of environmental legislation requirements that manifest into increased project compliance risks. This descriptive study developed 2 prioritized lists of environmental regulatory compliance risks and mitigation strategies and used multi-criteria decision theory for its theoretical framework. Information from compiled lists of environmental compliance risks and mitigation strategies was used to generate a specialized pairwise survey, which was piloted by 5 subject matter experts (SMEs). The survey was validated by a sample of 16 SMEs, after which the Analytic Hierarchy Process (AHP) was used to rank a total of 33 compliance risks and 12 mitigation strategy criteria. A key finding was that the AHP is a suitable tool for ranking of compliance risks and mitigation strategies. Several working hypotheses were also tested regarding how SMEs prioritized 1 compliance risk or mitigation strategy compared to another. The AHP showed that regulatory compliance, company reputation, environmental compliance, and economics ranked the highest and that a multi criteria mitigation strategy for environmental compliance ranked the highest. The study results will inform Alberta oil sands industry leaders about the ranking and utility of specific compliance risks and mitigations strategies, enabling them to focus on actions that will generate legislative and public trust. Oil sands leaders implementing a risk management program using the risks and mitigation strategies identified in this study will contribute to environmental conservation, economic growth, and positive social change.

  13. Road Transportable Analytical Laboratory system

    International Nuclear Information System (INIS)

    Finger, S.M.; Keith, V.F.; Spertzel, R.O.; De Avila, J.C.; O'Donnell, M.; Vann, R.L.

    1993-09-01

    This developmental effort clearly shows that a Road Transportable Analytical Laboratory System is a worthwhile and achievable goal. The RTAL is designed to fully analyze (radioanalytes, and organic and inorganic chemical analytes) 20 samples per day at the highest levels of quality assurance and quality control. It dramatically reduces the turnaround time for environmental sample analysis from 45 days (at a central commercial laboratory) to 1 day. At the same time each RTAL system will save the DOE over $12 million per year in sample analysis costs compared to the costs at a central commercial laboratory. If RTAL systems were used at the eight largest DOE facilities (at Hanford, Savannah River, Fernald, Oak Ridge, Idaho, Rocky Flats, Los Alamos, and the Nevada Test Site), the annual savings would be $96,589,000. The DOE's internal study of sample analysis needs projects 130,000 environmental samples requiring analysis in FY 1994, clearly supporting the need for the RTAL system. The cost and time savings achievable with the RTAL system will accelerate and improve the efficiency of cleanup and remediation operations throughout the DOE complex

  14. Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

    OpenAIRE

    Helena Prosen

    2014-01-01

    Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several...

  15. Requirements for quality control of analytical data for the Environmental Restoration Program

    International Nuclear Information System (INIS)

    Engels, J.

    1992-12-01

    The Environmental Restoration (ER) Program was established for the investigation and remediation of inactive US Department of Energy (DOE) sites and facilities that have been declared surplus in terms of their previous uses. The purpose of this document is to Specify ER requirements for quality control (QC) of analytical data. Activities throughout all phases of the investigation may affect the quality of the final data product, thus are subject to control specifications. Laboratory control is emphasized in this document, and field concerns will be addressed in a companion document Energy Systems, in its role of technical coordinator and at the request of DOE-OR, extends the application of these requirements to all participants in ER activities. Because every instance and concern may not be addressed in this document, participants are encouraged to discuss any questions with the ER Quality Assurance (QA) Office, the Analytical Environmental Support Group (AESG), or the Analytical Project Office (APO)

  16. Conformity Assessment in Nuclear Material and Environmental Sample Analysis

    International Nuclear Information System (INIS)

    Aregbe, Y.; Jakopic, R.; Richter, S.; Venchiarutti, C.

    2015-01-01

    Safeguards conclusions are based to a large extent on comparison of measurement results between operator and safeguards laboratories. Measurement results must state traceability and uncertainties to be comparable. Recent workshops held at the IAEA and in the frame of the European Safeguards Research and Development Association (ESARDA), reviewed different approaches for Nuclear Material Balance Evaluation (MBE). Among those, the ''bottom-up'' approach requires assessment of operators and safeguards laboratories measurement systems and capabilities. Therefore, inter-laboratory comparisons (ILCs) with independent reference values provided for decades by JRC-IRMM, CEA/CETAMA and US DOE are instrumental to shed light on the current state of practice in measurements of nuclear material and environmental swipe samples. Participating laboratories are requested to report the measurement results with associated uncertainties, and have the possibility to benchmark those results against independent and traceable reference values. The measurement capability of both the IAEA Network of Analytical Laboratories (NWAL) and the nuclear operator's analytical services participating in ILCs can be assessed against the independent reference values as well as against internationally agreed quality goals, in compliance with ISO 13528:2005. The quality goals for nuclear material analysis are the relative combined standard uncertainties listed in the ITV2010. Concerning environmental swipe sample analysis, the IAEA defined measurement quality goals applied in conformity assessment. The paper reports examples from relevant inter-laboratory comparisons, looking at laboratory performance according to the purpose of the measurement and the possible use of the result in line with the IUPAC International Harmonized Protocol. Tendencies of laboratories to either overestimate and/or underestimate uncertainties are discussed using straightforward graphical tools to evaluate

  17. The role of NAA in the environmental studies. Quantitative determination of heavy metals pollutant on environmental samples

    International Nuclear Information System (INIS)

    Sutisna; Yusuf, Saeful; Fisli, Adel; Rukihati; Wardhani, Sri; Th Rina M

    2003-01-01

    The neutron activation analysis technique was applied in the elemental analysis of environmental samples to solve an environmental pollution problem. We focused our study in the analysis of heavy metal which has potentially become a pollutant. The environmental samples analyzed were some water, sediment and an air particulate matter. The tap water sample was collected from five samplings points located at region of Serpong and Muria. Meanwhile the river water samples were taken from five samplings points of Ciliwung River. Eight samplings points of Cisadane river estuary located at Tanjung Burung were selected to collect sediment samples. Air particulate samples were collected from Jakarta Metropolitan and Serpong using high volume air sampler. Trace elements analyses of water samples were done using a combination of INAA and pre-concentration stage prior irradiation. All samples were irradiated at GA. Siwabessy reactor located at Serpong using a thermal neutron flux of about 10 12 n.cm -2 .sec -1 . After cooling time, the samples irradiated were counted by a high resolution HPGe detector coupled to a multichannel analyzer. The quantitative analyses have been done using a comparative method to a fresh laboratory standard and we used some standard references materials to validate our analytical result. The obtained result from the tap water analysis show that the elements of As, Cr, Co, Cd, Mn, Sb and Zn could be determine quantitatively and they have a concentration range from about 0.02 μg/L to 103.9 μg/L. The analysis result of Ciliwung river water samples show that elements of Ag, As, Co, Cu, Fe, Hg, Mn, V and Zn are present in the range of 2.4 μg/L to about 1365.8 μg/L. Meanwhile some important elements were obtained in the sediments samples taken from Cisadane River estuary such as Ce (40.4 - 63.6 mg/kg), Co (15.2 - 40.2 mg/kg), Cr (21.6 - 57.8 mg/kg), Eu (1.2 - 1.8 mg/kg), Fe (7.0 - 16.8 mg/kg), Mn (887 - 1810 mg/kg) and V (160 - 558 mg/kg). Finally the

  18. Hanford Site Environmental Surveillance Master Sampling Schedule

    International Nuclear Information System (INIS)

    Bisping, L.E.

    2000-01-01

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest National Laboratory (PNNL) for the U.S. Department of Energy (DOE). Sampling is conducted to evaluate levels of radioactive and nonradioactive pollutants in the Hanford environs, as required in DOE Order 5400.1, General Environmental Protection Program: and DOE Order 5400.5, Radiation Protection of the Public and the Environment. The sampling design is described in the Operations Office, Environmental Monitoring Plan, United States Department of Energy, Richland DOE/RL-91-50, Rev.2, U.S. Department of Energy, Richland, Washington. This document contains the CY 2000 schedules for the routine collection of samples for the Surface Environmental Surveillance Project (SESP) and Drinking Water Monitoring Project. Each section includes sampling locations, sample types, and analyses to be performed. In some cases, samples are scheduled on a rotating basis and may not be collected in 2000 in which case the anticipated year for collection is provided. In addition, a map showing approximate sampling locations is included for each media scheduled for collection

  19. Functional Analytic Multisensory Environmental Therapy for People with Dementia

    OpenAIRE

    Staal, Jason A.

    2012-01-01

    This paper introduces Functional Analytic Multisensory Environmental Therapy (FAMSET) for use with elders with dementia while using a multisensory environment/snoezelen room. The model introduces behavioral theory and practice to the multisensory environment treatment, addressing assessment, and, within session techniques, integrating behavioral interventions with emotion-oriented care. A modular approach is emphasized to delineate different treatment phases for multisensory environment thera...

  20. The environmental evaluation of substation based on the fuzzy analytic hierarchy process

    Science.gov (United States)

    Qian, Wenxiao; Zuo, Xiujiang; Chen, Yuandong; Ye, Ming; Fang, Zhankai; Yang, Fan

    2018-02-01

    This paper studies on the different influences on the environment of the substations and puts forward an index system of environmental protection through the fuzzy analytic hierarchy process. A comprehensive environmental evaluation on a substation is carried out through investigation and measurement of the current environmental factors, and the statistical data has validated the effectiveness and feasibility of this evaluation index system. The results indicate that the proposed model has high efficiency.

  1. Supercritical Fluid Extraction and Ultra Performance Liquid Chromatography of Respiratory Quinones for Microbial Community Analysis in Environmental and Biological Samples

    OpenAIRE

    Hanif, Muhammad; Atsuta, Yoichi; Fujie, Koichi; Daimon, Hiroyuki

    2012-01-01

    Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysi...

  2. X-ray fluorescence in Member States (Spain): Main activities related to the use of XRF techniques at the Analytical and Environmental Chemistry Research Group of the University of Girona (UdG)

    International Nuclear Information System (INIS)

    Marguí, Eva; Hidalgo, Manuela

    2014-01-01

    The Analytical and Environmental Chemistry Group (QAA) is a consolidated research group of the Department of Chemistry of the University of Girona (North- East Spain). The main research topics of the group are related to the development and application of analytical methodologies for the determination of inorganic and organic species in different kind of environmental, clinical and industrial samples. From the beginning of the 2000’s, one of the research focuses of the group, is the use of X-ray fluorescence spectrometry (XRF) for the determination of trace amounts of metals and metalloids mostly in samples related to the environmental and industrial fields. For instance, in collaboration with the Institute of Earth Sciences “Jaume Almera” (ICTJA-CSIC, Spain), we have developed and successfully applied several analytical approaches based on the use of EDXRF (Energy dispersive XRF), WDXRF (Wavelength dispersive XRF) and PEDXRF (Polarised EDXRF) for the determination of metals at trace levels in complex liquid samples such as sea water or electroplating waters in vegetation samples collected around mining environments or in active pharmaceutical ingredients. At present, the evaluation of the analytical possibilities of TXRF (Total reflection XRF) in the chemical analysis field is also one of the research topics of QAA. In this sense, several contributions related to the use of this technique for element determination in liquid and solid samples have been developed. A summary of these contributions is summarized in the last section of this review

  3. Superfund Site Information - Site Sampling Data

    Data.gov (United States)

    U.S. Environmental Protection Agency — This asset includes Superfund site-specific sampling information including location of samples, types of samples, and analytical chemistry characteristics of...

  4. Hanford site environmental surveillance master sampling schedule

    International Nuclear Information System (INIS)

    Bisping, L.E.

    1998-01-01

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest National Laboratory (PNNL) for the U.S. Department of Energy (DOE). Sampling is conducted to evaluate levels of radioactive and nonradioactive pollutants in the Hanford environs, as required in DOE Order 5400.1 open-quotes General Environmental Protection Program,close quotes and DOE Order 5400.5, open-quotes Radiation Protection of the Public and the Environment.close quotes The sampling methods are described in the Environmental Monitoring Plan, United States Department of Energy, Richland Operations Office, DOE/RL91-50, Rev. 2, U.S. Department of Energy, Richland, Washington. This document contains the 1998 schedules for routine collection of samples for the Surface Environmental Surveillance Project (SESP) and Drinking Water Monitoring Project. Each section of this document describes the planned sampling schedule for a specific media (air, surface water, biota, soil and vegetation, sediment, and external radiation). Each section includes the sample location, sample type, and analyses to be performed on the sample. In some cases, samples are scheduled on a rotating basis and may not be planned for 1998 in which case the anticipated year for collection is provided. In addition, a map is included for each media showing sample locations

  5. Ecotoxicity on a stick: A novel analytical tool for predicting the ecotoxicity of petroleum contaminated samples

    International Nuclear Information System (INIS)

    Parkerton, T.F.; Stone, M.A.

    1995-01-01

    Hydrocarbons generally elicit toxicity via a nonpolar narcotic mechanism. Recent research suggests that chemicals acting by this mode invoke ecotoxicity when the molar concentration in organisms lipid exceeds a critical threshold. Since ecotoxicity of nonpolar narcotic mixtures appears to be additive, the ecotoxicity of hydrocarbon mixtures thus depends upon: (1) the partitioning of individual hydrocarbons comprising the mixture from the environment to lipids and (2) the total molar sum of the constituent hydrocarbons in lipids. These insights have led previous investigators to advance the concept of biomimetic extraction as a novel tool for assessing potential narcosis-type or baseline ecotoxicity in aqueous samples. Drawing from this earlier work, the authors have developed a method to quantify Bioavailable Petroleum Hydrocarbons (BPHS) in hydrocarbon-contaminated aqueous and soil/sediment samples. A sample is equilibrated with a solid phase microextraction (SPME) fiber that serves as a surrogate for organism lipids. The total moles of hydrocarbons that partition to the SPME fiber is then quantified using a simple GC/FID procedure. Research conducted to support the development and initial validation of this method will be presented. Results suggest that BPH analyses provide a promising, cost-effective approach for predicting the ecotoxicity of environmental samples contaminated with hydrocarbon mixtures. Consequently, BPH analyses may provide a valuable analytical screening tool for ecotoxicity assessment in product and effluent testing, environmental monitoring and site remediation applications

  6. Metal-organic frameworks for analytical chemistry: from sample collection to chromatographic separation.

    Science.gov (United States)

    Gu, Zhi-Yuan; Yang, Cheng-Xiong; Chang, Na; Yan, Xiu-Ping

    2012-05-15

    In modern analytical chemistry researchers pursue novel materials to meet analytical challenges such as improvements in sensitivity, selectivity, and detection limit. Metal-organic frameworks (MOFs) are an emerging class of microporous materials, and their unusual properties such as high surface area, good thermal stability, uniform structured nanoscale cavities, and the availability of in-pore functionality and outer-surface modification are attractive for diverse analytical applications. This Account summarizes our research on the analytical applications of MOFs ranging from sampling to chromatographic separation. MOFs have been either directly used or engineered to meet the demands of various analytical applications. Bulk MOFs with microsized crystals are convenient sorbents for direct application to in-field sampling and solid-phase extraction. Quartz tubes packed with MOF-5 have shown excellent stability, adsorption efficiency, and reproducibility for in-field sampling and trapping of atmospheric formaldehyde. The 2D copper(II) isonicotinate packed microcolumn has demonstrated large enhancement factors and good shape- and size-selectivity when applied to on-line solid-phase extraction of polycyclic aromatic hydrocarbons in water samples. We have explored the molecular sieving effect of MOFs for the efficient enrichment of peptides with simultaneous exclusion of proteins from biological fluids. These results show promise for the future of MOFs in peptidomics research. Moreover, nanosized MOFs and engineered thin films of MOFs are promising materials as novel coatings for solid-phase microextraction. We have developed an in situ hydrothermal growth approach to fabricate thin films of MOF-199 on etched stainless steel wire for solid-phase microextraction of volatile benzene homologues with large enhancement factors and wide linearity. Their high thermal stability and easy-to-engineer nanocrystals make MOFs attractive as new stationary phases to fabricate MOF

  7. Nuclear analytical chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Brune, D.; Forkman, B.; Persson, B.

    1984-01-01

    This book covers the general theories and techniques of nuclear chemical analysis, directed at applications in analytical chemistry, nuclear medicine, radiophysics, agriculture, environmental sciences, geological exploration, industrial process control, etc. The main principles of nuclear physics and nuclear detection on which the analysis is based are briefly outlined. An attempt is made to emphasise the fundamentals of activation analysis, detection and activation methods, as well as their applications. The book provides guidance in analytical chemistry, agriculture, environmental and biomedical sciences, etc. The contents include: the nuclear periodic system; nuclear decay; nuclear reactions; nuclear radiation sources; interaction of radiation with matter; principles of radiation detectors; nuclear electronics; statistical methods and spectral analysis; methods of radiation detection; neutron activation analysis; charged particle activation analysis; photon activation analysis; sample preparation and chemical separation; nuclear chemical analysis in biological and medical research; the use of nuclear chemical analysis in the field of criminology; nuclear chemical analysis in environmental sciences, geology and mineral exploration; and radiation protection.

  8. Nuclear analytical chemistry

    International Nuclear Information System (INIS)

    Brune, D.; Forkman, B.; Persson, B.

    1984-01-01

    This book covers the general theories and techniques of nuclear chemical analysis, directed at applications in analytical chemistry, nuclear medicine, radiophysics, agriculture, environmental sciences, geological exploration, industrial process control, etc. The main principles of nuclear physics and nuclear detection on which the analysis is based are briefly outlined. An attempt is made to emphasise the fundamentals of activation analysis, detection and activation methods, as well as their applications. The book provides guidance in analytical chemistry, agriculture, environmental and biomedical sciences, etc. The contents include: the nuclear periodic system; nuclear decay; nuclear reactions; nuclear radiation sources; interaction of radiation with matter; principles of radiation detectors; nuclear electronics; statistical methods and spectral analysis; methods of radiation detection; neutron activation analysis; charged particle activation analysis; photon activation analysis; sample preparation and chemical separation; nuclear chemical analysis in biological and medical research; the use of nuclear chemical analysis in the field of criminology; nuclear chemical analysis in environmental sciences, geology and mineral exploration; and radiation protection

  9. Environmental surveillance master sampling schedule

    International Nuclear Information System (INIS)

    Bisping, L.E.

    1991-01-01

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest Laboratory (PNL) for the US Department of Energy (DOE). This document contains the planned schedule for routine sample collection for the Surface Environmental Surveillance Project (SESP) and Ground-Water Monitoring Project. The routine sampling plan for the SESP has been revised this year to reflect changing site operations and priorities. Some sampling previously performed at least annually has been reduced in frequency, and some new sampling to be performed at a less than annual frequency has been added. Therefore, the SESP schedule reflects sampling to be conducted in calendar year 1991 as well as future years. The ground-water sampling schedule is for 1991. This schedule is subject to modification during the year in response to changes in Site operation, program requirements, and the nature of the observed results. Operational limitations such as weather, mechanical failures, sample availability, etc., may also require schedule modifications. Changes will be documented in the respective project files, but this plan will not be reissued. The purpose of these monitoring projects is to evaluate levels of radioactive and nonradioactive pollutants in the Hanford evirons

  10. Environmental surveillance master sampling schedule

    Energy Technology Data Exchange (ETDEWEB)

    Bisping, L.E.

    1991-01-01

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest Laboratory (PNL) for the US Department of Energy (DOE). This document contains the planned schedule for routine sample collection for the Surface Environmental Surveillance Project (SESP) and Ground-Water Monitoring Project. The routine sampling plan for the SESP has been revised this year to reflect changing site operations and priorities. Some sampling previously performed at least annually has been reduced in frequency, and some new sampling to be performed at a less than annual frequency has been added. Therefore, the SESP schedule reflects sampling to be conducted in calendar year 1991 as well as future years. The ground-water sampling schedule is for 1991. This schedule is subject to modification during the year in response to changes in Site operation, program requirements, and the nature of the observed results. Operational limitations such as weather, mechanical failures, sample availability, etc., may also require schedule modifications. Changes will be documented in the respective project files, but this plan will not be reissued. The purpose of these monitoring projects is to evaluate levels of radioactive and nonradioactive pollutants in the Hanford evirons.

  11. Development of low-level environmental sampling capabilities for uranium at Brazilian and Argentine laboratories by ABACC

    International Nuclear Information System (INIS)

    Guidicini, Olga Mafra; Hembree Junior, Doyle M.; Carter, Joel A.; Hayes, Susan; Whitaker, Michael; Olsen, Khris

    2003-01-01

    The Brazilian-Argentine Agency for Accounting and Control of Nuclear Materials (ABACC) with assistance from the U.S. Department of Energy (DOE) began a program to evaluate environmental sampling capabilities at laboratories in Argentina and Brazil in June 1998. The program included staff training conducted in South America and the United States. Several laboratory evaluation exercises were also conducted using standard swipe samples prepared by the International Atomic Energy Agency (IAEA) and a National Institute of Standards and Technology Standard Reference Material 1547, Peach Leaves. The results of these exercises demonstrated that several laboratories were capable of accurately determining the total uranium and uranium isotopic distribution in the peach leaves. To build on these successes, another exercise using standard swipe samples prepared by the IAEA was conducted. A total of 8 sets of 15 swipe samples were prepared and distributed to the six ABACC support laboratories and to two of DOE's Network of Analytical Laboratories (NWAL) that support IAEA's environmental sampling program Throughout this project, the ABACC laboratories have shown steady progress in contamination control and improvements to the accuracy and precision of their measurements. The results of the latest exercises demonstrate that ABACC now has support laboratories in both Argentina and Brazil that have the capability to measure both the amount and isotopic composition of uranium at levels expected in typical environmental samples (i.e., sub-microgram quantities). This presentation will discuss the final results for the exercise with uranium swipe samples and discuss future activities to develop measurement capabilities for total and isotopic plutonium in environmental samples. (author)

  12. Simultaneous analysis of multiple classes of antimicrobials in environmental water samples using SPE coupled with UHPLC-ESI-MS/MS and isotope dilution.

    Science.gov (United States)

    Tran, Ngoc Han; Chen, Hongjie; Do, Thanh Van; Reinhard, Martin; Ngo, Huu Hao; He, Yiliang; Gin, Karina Yew-Hoong

    2016-10-01

    A robust and sensitive analytical method was developed for the simultaneous analysis of 21 target antimicrobials in different environmental water samples. Both single SPE and tandem SPE cartridge systems were investigated to simultaneously extract multiple classes of antimicrobials. Experimental results showed that good extraction efficiencies (84.5-105.6%) were observed for the vast majority of the target analytes when extraction was performed using the tandem SPE cartridge (SB+HR-X) system under an extraction pH of 3.0. HPLC-MS/MS parameters were optimized for simultaneous analysis of all the target analytes in a single injection. Quantification of target antimicrobials in water samples was accomplished using 15 isotopically labeled internal standards (ILISs), which allowed the efficient compensation of the losses of target analytes during sample preparation and correction of matrix effects during UHPLC-MS/MS as well as instrument fluctuations in MS/MS signal intensity. Method quantification limit (MQL) for most target analytes based on SPE was below 5ng/L for surface waters, 10ng/L for treated wastewater effluents, and 15ng/L for raw wastewater. The method was successfully applied to detect and quantify the occurrence of the target analytes in raw influent, treated effluent and surface water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Hanford environmental analytical methods: Methods as of March 1990

    International Nuclear Information System (INIS)

    Goheen, S.C.; McCulloch, M.; Daniel, J.L.

    1993-05-01

    This paper from the analytical laboratories at Hanford describes the method used to measure pH of single-shell tank core samples. Sludge or solid samples are mixed with deionized water. The pH electrode used combines both a sensor and reference electrode in one unit. The meter amplifies the input signal from the electrode and displays the pH visually

  14. Streamlined sample cleanup using combined dispersive solid-phase extraction and in-vial filtration for analysis of pesticides and environmental pollutants in shrimp

    Energy Technology Data Exchange (ETDEWEB)

    Han, Lijun [College of Science, China Agricultural University, Beijing (China); Sapozhnikova, Yelena [U.S. Dept. of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 19038 (United States); Lehotay, Steven J., E-mail: Steven.Lehotay@ars.usda.gov [U.S. Dept. of Agriculture, Agricultural Research Service, Eastern Regional Research Center, 600 East Mermaid Lane, Wyndmoor, PA 19038 (United States)

    2014-05-01

    Highlights: • The first report that combines in-vial filtration and dispersive-SPE for sample cleanup. • The unique application of ammonium formate for salting-out partitioning in QuEChERS. • Evaluations of a new zirconium-based and a non-friable GCB sorbent for d-SPE cleanup. • A new analytical method for 59 pesticides and environmental pollutants in shrimp. Abstract: A new method of sample preparation was developed and is reported for the first time. The approach combines in-vial filtration with dispersive solid-phase extraction (d-SPE) in a fast and convenient cleanup of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts. The method was applied to simultaneous analysis of 42 diverse pesticides and 17 environmental contaminants, including polycyclic aromatic hydrocarbons, polychlorinated biphenyls (PCBs), and flame retardants, in shrimp as the sample matrix. Final extracts were analyzed by both low-pressure gas chromatography – triple quadrupole tandem mass spectrometry (LPGC-MS/MS), and high-performance liquid chromatography – triple quadrupole tandem mass spectrometry (HPLC-MS/MS) to provide a wide scope of analysis for targeted analytes. During method development, several different commercial sorbents for d-SPE were investigated and compared with respect to analyte recoveries. The method was validated at 10, 50, and 100 ng g⁻¹ spiking levels (10-fold lower for PCBs), and the results for nearly all analytes were between 70 and 115% recoveries with ≤17% relative standard deviations. The method was shown to be simple, fast, and effective for multi-application analysis of chemical residues in the representative food and environmental marker matrix.

  15. The role of NAA in the environmental studies. Quantitative determination of heavy metals pollutant on environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Sutisna; Yusuf, Saeful; Fisli, Adel; Rukihati; Wardhani, Sri; Th Rina M [National Nuclear Energy Agency of Indonesia, Kawasan Puspiptek, Serpong (Indonesia)

    2003-03-01

    The neutron activation analysis technique was applied in the elemental analysis of environmental samples to solve an environmental pollution problem. We focused our study in the analysis of heavy metal which has potentially become a pollutant. The environmental samples analyzed were some water, sediment and an air particulate matter. The tap water sample was collected from five samplings points located at region of Serpong and Muria. Meanwhile the river water samples were taken from five samplings points of Ciliwung River. Eight samplings points of Cisadane river estuary located at Tanjung Burung were selected to collect sediment samples. Air particulate samples were collected from Jakarta Metropolitan and Serpong using high volume air sampler. Trace elements analyses of water samples were done using a combination of INAA and pre-concentration stage prior irradiation. All samples were irradiated at GA. Siwabessy reactor located at Serpong using a thermal neutron flux of about 10{sup 12} n.cm{sup -2}.sec{sup -1}. After cooling time, the samples irradiated were counted by a high resolution HPGe detector coupled to a multichannel analyzer. The quantitative analyses have been done using a comparative method to a fresh laboratory standard and we used some standard references materials to validate our analytical result. The obtained result from the tap water analysis show that the elements of As, Cr, Co, Cd, Mn, Sb and Zn could be determine quantitatively and they have a concentration range from about 0.02 {mu}g/L to 103.9 {mu}g/L. The analysis result of Ciliwung river water samples show that elements of Ag, As, Co, Cu, Fe, Hg, Mn, V and Zn are present in the range of 2.4 {mu}g/L to about 1365.8 {mu}g/L. Meanwhile some important elements were obtained in the sediments samples taken from Cisadane River estuary such as Ce (40.4 - 63.6 mg/kg), Co (15.2 - 40.2 mg/kg), Cr (21.6 - 57.8 mg/kg), Eu (1.2 - 1.8 mg/kg), Fe (7.0 - 16.8 mg/kg), Mn (887 - 1810 mg/kg) and V (160 - 558

  16. Pre-analytical sample quality: metabolite ratios as an intrinsic marker for prolonged room temperature exposure of serum samples.

    Directory of Open Access Journals (Sweden)

    Gabriele Anton

    Full Text Available Advances in the "omics" field bring about the need for a high number of good quality samples. Many omics studies take advantage of biobanked samples to meet this need. Most of the laboratory errors occur in the pre-analytical phase. Therefore evidence-based standard operating procedures for the pre-analytical phase as well as markers to distinguish between 'good' and 'bad' quality samples taking into account the desired downstream analysis are urgently needed. We studied concentration changes of metabolites in serum samples due to pre-storage handling conditions as well as due to repeated freeze-thaw cycles. We collected fasting serum samples and subjected aliquots to up to four freeze-thaw cycles and to pre-storage handling delays of 12, 24 and 36 hours at room temperature (RT and on wet and dry ice. For each treated aliquot, we quantified 127 metabolites through a targeted metabolomics approach. We found a clear signature of degradation in samples kept at RT. Storage on wet ice led to less pronounced concentration changes. 24 metabolites showed significant concentration changes at RT. In 22 of these, changes were already visible after only 12 hours of storage delay. Especially pronounced were increases in lysophosphatidylcholines and decreases in phosphatidylcholines. We showed that the ratio between the concentrations of these molecule classes could serve as a measure to distinguish between 'good' and 'bad' quality samples in our study. In contrast, we found quite stable metabolite concentrations during up to four freeze-thaw cycles. We concluded that pre-analytical RT handling of serum samples should be strictly avoided and serum samples should always be handled on wet ice or in cooling devices after centrifugation. Moreover, serum samples should be frozen at or below -80°C as soon as possible after centrifugation.

  17. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Science.gov (United States)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6-4.3%), repeatability (4-9%), reproducibility (9-11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as straightforward

  18. Analytical characterization using surface-enhanced Raman scattering (SERS) and microfluidic sampling

    International Nuclear Information System (INIS)

    Wang, Chao; Yu, Chenxu

    2015-01-01

    With the rapid development of analytical techniques, it has become much easier to detect chemical and biological analytes, even at very low detection limits. In recent years, techniques based on vibrational spectroscopy, such as surface enhanced Raman spectroscopy (SERS), have been developed for non-destructive detection of pathogenic microorganisms. SERS is a highly sensitive analytical tool that can be used to characterize chemical and biological analytes interacting with SERS-active substrates. However, it has always been a challenge to obtain consistent and reproducible SERS spectroscopic results at complicated experimental conditions. Microfluidics, a tool for highly precise manipulation of small volume liquid samples, can be used to overcome the major drawbacks of SERS-based techniques. High reproducibility of SERS measurement could be obtained in continuous flow generated inside microfluidic devices. This article provides a thorough review of the principles, concepts and methods of SERS-microfluidic platforms, and the applications of such platforms in trace analysis of chemical and biological analytes. (topical review)

  19. Analytical results and sample locality map for rock, stream-sediment, and soil samples, Northern and Eastern Coloado Desert BLM Resource Area, Imperial, Riverside, and San Bernardino Counties, California

    Science.gov (United States)

    King, Harley D.; Chaffee, Maurice A.

    2000-01-01

    Desert BLM Resource Area and vicinity. Included in the 1,245 stream-sediment samples collected by the USGS are 284 samples collected as part of the current study, 817 samples collected as part of investigations of the12 BLM WSAs and re-analyzed for the present study, 45 samples from the Needles 1? X 2? quadrangle, and 99 samples from the El Centro 1? X 2? quadrangle. The NURE stream-sediment and soil samples were re-analyzed as part of the USGS study in the Needles quadrangle. Analytical data for samples from the Chocolate Mountain Aerial Gunnery Range, which is located within the area of the NECD, were previously reported (King and Chaffee, 1999a). For completeness, these results are also included in this report. Analytical data for samples from the area of Joshua Tree National Park that is within the NECD have also been reported (King and Chaffee, 1999b). These results are not included in this report. The analytical data presented here can be used for baseline geochemical, mineral resource, and environmental geochemical studies.

  20. Radiochemistry methods in DOE Methods for Evaluating Environmental and Waste Management Samples: Addressing new challenges

    International Nuclear Information System (INIS)

    Fadeff, S.K.; Goheen, S.C.; Riley, R.G.

    1994-01-01

    Radiochemistry methods in Department of Energy Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) add to the repertoire of other standard methods in support of U.S. Department of Energy environmental restoration and waste management (DOE/EM) radiochemical characterization activities. Current standard sources of radiochemistry methods are not always applicable for evaluating DOE/EM samples. Examples of current sources include those provided by the US Environmental Protection Agency, the American Society for Testing and Materials, Standard Methods for the Examination of Water and Wastewater, and Environmental Measurements Laboratory Procedures Manual (HASL-300). The applicability of these methods is generally limited to specific matrices (usually water), low-level radioactive samples, and a limited number of analytes. DOE Methods complements these current standard methods by addressing the complexities of EM characterization needs. The process for determining DOE/EM radiochemistry characterization needs is discussed. In this context of DOE/EM needs, the applicability of other sources of standard radiochemistry methods is defined, and gaps in methodology are identified. Current methods in DOE Methods and the EM characterization needs they address are discussed. Sources of new methods and the methods incorporation process are discussed. The means for individuals to participate in (1) identification of DOE/EM needs, (2) the methods incorporation process, and (3) submission of new methods are identified

  1. Comparison of air samples, nasal swabs, ear-skin swabs and environmental dust samples for detection of Methicillin Resistant Staphylococcus aureus (MRSA) in pig herds

    DEFF Research Database (Denmark)

    Agersø, Yvonne; Vigre, Håkan; Cavaco, Lina

    2014-01-01

    To identify a cost-effective and practical method for detection of methicillin-resistant Staphylococcus aureus (MRSA) in pig herds, the relative sensitivity of four sample types: nasal swabs, ear-skin (skin behind the ears) swabs, environmental dust swabs and air was compared. Moreover, dependency......-herd prevalence ⩾25%]. The results indicate that taking swabs of skin behind the ears (ten pools of five) was even more sensitive than taking nasal swabs (ten pools of five) at the herd level and detected significantly more positive samples. spa types t011, t034 and t4208 were observed. In conclusion, MRSA...... detection by air sampling is easy to perform, reduces costs and analytical time compared to existing methods, and is recommended for initial testing of herds. Ear-skin swab sampling may be more sensitive for MRSA detection than air sampling or nasal swab sampling....

  2. Isotope dilution analysis of environmental samples

    International Nuclear Information System (INIS)

    Tolgyessy, J.; Lesny, J.; Korenova, Z.; Klas, J.; Klehr, E.H.

    1986-01-01

    Isotope dilution analysis has been used for the determination of several trace elements - especially metals - in a variety of environmental samples, including aerosols, water, soils, biological materials and geological materials. Variations of the basic concept include classical IDA, substoichiometric IDA, and more recently, sub-superequivalence IDA. Each variation has its advantages and limitations. A periodic chart has been used to identify those elements which have been measured in environmental samples using one or more of these methods. (author)

  3. Neutron activation analysis of 127I and 129I environmental samples

    International Nuclear Information System (INIS)

    Takeishi, Minoru; Namiki, Atsushi; Ishida, Junichiro; Iwai, Makoto

    1987-01-01

    The analytical method of 127 I and 129 I in environmental samples has been studied and the background levels of these nuclides in soils, seaweeds and milk were measured. The analytical method consists of the combustion technique and neutron activation analysis (N.A.A.). The iodine was separated from samples by ignition at about 1,000 deg C in a quartz combustion apparatus with an oxygen and a nitrogen stream, and was absorbed by small amounts of active charcoal. The iodine was then purified through the carbontetrachloride extraction method and the PdI 2 decomposition method. Irradiation was conducted by JRR-4 (n th : 8 x 10 13 n/cm 2 · sec) for 40 min. After irradiation, the iodine was purified by the solvent extraction method same as pre-irradiation extraction. Each activity of 126 I and 130 I, which was produced by 127 I(n,2n) 126 I and 129 I(n,γ) 130 I reaction respectively, was measured by γ-spectrometry using a Ge-detector. The lower detection limits of 129 I by this method were 4 x 10 -7 Bq/g for dry soil, 7 x 10 -8 Bq/g for fresh seaweeds and 7 x 10 -6 Bq/l for fresh milk, respectively. The relative standard deviation of 129 I measurements in soil and milk were less than 10 %. (author)

  4. Development and implementation of information systems for the DOE's National Analytical Management Program (NAMP)

    International Nuclear Information System (INIS)

    Streets, W. E.

    1999-01-01

    The Department of Energy (DOE) faces a challenging environmental management effort, including environmental protection, environmental restoration, waste management, and decommissioning. This effort requires extensive sampling and analysis to determine the type and level of contamination and the appropriate technology for cleanup, and to verify compliance with environmental regulations. Data obtained from these sampling and analysis activities are used to support environmental management decisions. Confidence in the data is critical, having legal, regulatory, and therefore, economic impact. To promote quality in the planning, management, and performance of these sampling and analysis operations, DOE's Office of Environmental Management (EM) has established the National Analytical Management Program (NAMP). With a focus on reducing the estimated costs of over $200M per year for EM's analytical services, NAMP has been charged with developing products that will decrease the costs for DOE complex-wide environmental management while maintaining quality in all aspects of the analytical data generation. As part of this thrust to streamline operations, NAMP is developing centralized information systems that will allow DOE complex personnel to share information about EM contacts at the various sites, pertinent methodologies for environmental restoration and waste management, costs of analyses, and performance of contracted laboratories

  5. Reengineering of Analytical Data Management for the Environmental Restoration Project at Los Alamos National Laboratory

    International Nuclear Information System (INIS)

    Bolivar, S.; Dorries, A.; Nasser, K.; Scherma, S.

    2003-01-01

    The Environmental Restoration (ER) Project at Los Alamos National Laboratory (LANL) is responsible for the characterization, clean up, and monitoring of over 2,124 identified potential release sites (PRS). These PRSs have resulted from operations associated with weapons and energy related research which has been conducted at LANL since 1942. To accomplish mission goals, the ER Project conducts field sampling to determine possible types and levels of chemical contamination as well as their geographic extent. Last fiscal year, approximately 4000 samples were collected during ER Project field sampling campaigns. In the past, activities associated with field sampling such as sample campaign planning, paperwork, shipping and analytical laboratory tracking; verification and order fulfillment; validation and data quality assurance were performed by multiple groups working with a variety of software applications, databases and hard copy reports. This resulted in significant management and communication difficulties, data delivery delays, and inconsistent processes; it also represented a potential threat to overall data integrity. Creation of an organization, software applications and a data process that could provide for cost-effective management of the activities and data mentioned above became a management priority, resulting in a development of a reengineering task. This reengineering effort--currently nearing completion--has resulted in personnel reorganization, the development of a centralized data repository, and a powerful web-based sample management system that allows for an appreciably streamlined and more efficient data process. These changes have collectively cut data delivery times, allowed for larger volumes of samples and data to be handled with fewer personnel, and resulted in significant cost savings. This paper will provide a case study of the reengineering effort undertaken by the ER Project of its analytical data management process. It includes

  6. Reengineering of Analytical Data Management for the Environmental Restoration Project at Los Alamos National Laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Bolivar, S.; Dorries, A.; Nasser, K.; Scherma, S.

    2003-02-27

    The Environmental Restoration (ER) Project at Los Alamos National Laboratory (LANL) is responsible for the characterization, clean up, and monitoring of over 2,124 identified potential release sites (PRS). These PRSs have resulted from operations associated with weapons and energy related research which has been conducted at LANL since 1942. To accomplish mission goals, the ER Project conducts field sampling to determine possible types and levels of chemical contamination as well as their geographic extent. Last fiscal year, approximately 4000 samples were collected during ER Project field sampling campaigns. In the past, activities associated with field sampling such as sample campaign planning, paperwork, shipping and analytical laboratory tracking; verification and order fulfillment; validation and data quality assurance were performed by multiple groups working with a variety of software applications, databases and hard copy reports. This resulted in significant management and communication difficulties, data delivery delays, and inconsistent processes; it also represented a potential threat to overall data integrity. Creation of an organization, software applications and a data process that could provide for cost-effective management of the activities and data mentioned above became a management priority, resulting in a development of a reengineering task. This reengineering effort--currently nearing completion--has resulted in personnel reorganization, the development of a centralized data repository, and a powerful web-based sample management system that allows for an appreciably streamlined and more efficient data process. These changes have collectively cut data delivery times, allowed for larger volumes of samples and data to be handled with fewer personnel, and resulted in significant cost savings. This paper will provide a case study of the reengineering effort undertaken by the ER Project of its analytical data management process. It includes

  7. Analytical simulation of RBS spectra of nanowire samples

    Energy Technology Data Exchange (ETDEWEB)

    Barradas, Nuno P., E-mail: nunoni@ctn.ist.utl.pt [Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 ao km 139,7, 2695-066 Bobadela LRS (Portugal); García Núñez, C. [Laboratorio de Electrónica y Semiconductores, Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Redondo-Cubero, A. [Laboratorio de Electrónica y Semiconductores, Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Centro de Micro-Análisis de Materiales, Universidad Autónoma de Madrid, 28049 Madrid (Spain); Shen, G.; Kung, P. [Department of Electrical and Computer Engineering, The University of Alabama, AL 35487 (United States); Pau, J.L. [Laboratorio de Electrónica y Semiconductores, Departamento de Física Aplicada, Universidad Autónoma de Madrid, 28049 Madrid (Spain)

    2016-03-15

    Almost all, if not all, general purpose codes for analysis of Ion Beam Analysis data have been originally developed to handle laterally homogeneous samples only. This is the case of RUMP, NDF, SIMNRA, and even of the Monte Carlo code Corteo. General-purpose codes usually include only limited support for lateral inhomogeneity. In this work, we show analytical simulations of samples that consist of a layer of parallel oriented nanowires on a substrate, using a model implemented in NDF. We apply the code to real samples, made of vertical ZnO nanowires on a sapphire substrate. Two configurations of the nanowires were studied: 40 nm diameter, 4.1 μm height, 3.5% surface coverage; and 55 nm diameter, 1.1 μm height, 42% surface coverage. We discuss the accuracy and limits of applicability of the analysis.

  8. Environmental data qualification system

    International Nuclear Information System (INIS)

    Hester, O.V.; Groh, M.R.

    1989-01-01

    The Integrated Environmental Data Management System (IEDMS) is a PC-based system that can support environmental investigations from their design stage and throughout the duration of the study. The system integrates data originating from the Sampling and Analysis Plan, field data and analytical findings. The IEDMS automated features include sampling guidance forms, barcoded sample labels and tags, field and analytical forms reproduction, sample tracking, analytical data qualification, completeness reports, and results and QC data reporting. The IEDMS has extensive automated capabilities that support a systematic and comprehensive process for performing quality assessment of EPA-CLP chemical analyses data. One product of this process is a unique and extremely useful tabular presentation of the data. One table contains the complete set of results and QC data included on the CLP data forms while presenting the information consistent with the chronology in which the analysis was performed. 3 refs., 1 fig

  9. Environmental surveillance master sampling schedule

    Energy Technology Data Exchange (ETDEWEB)

    Bisping, L E

    1992-01-01

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest Laboratory (PNL) for the US Department of Energy (DOE). This document contains the planned schedule for routine sample collection for the Surface Environmental Surveillance Project (SESP) and Ground-Water Monitoring Project. Samples for radiological analyses include Air-Particulate Filter, gases and vapor; Water/Columbia River, Onsite Pond, Spring, Irrigation, and Drinking; Foodstuffs/Animal Products including Whole Milk, Poultry and Eggs, and Beef; Foodstuffs/Produce including Leafy Vegetables, Vegetables, and Fruit; Foodstuffs/Farm Products including Wine, Wheat and Alfalfa; Wildlife; Soil; Vegetation; and Sediment. Direct Radiation Measurements include Terrestrial Locations, Columbia River Shoreline Locations, and Onsite Roadway, Railway and Aerial, Radiation Surveys.

  10. Tank 214-AW-105, grab samples, analytical results for the final report

    International Nuclear Information System (INIS)

    Esch, R.A.

    1997-01-01

    This document is the final report for tank 241-AW-105 grab samples. Twenty grabs samples were collected from risers 10A and 15A on August 20 and 21, 1996, of which eight were designated for the K Basin sludge compatibility and mixing studies. This document presents the analytical results for the remaining twelve samples. Analyses were performed in accordance with the Compatibility Grab Sampling and Analysis Plan (TSAP) and the Data Quality Objectives for Tank Farms Waste Compatibility Program (DO). The results for the previous sampling of this tank were reported in WHC-SD-WM-DP-149, Rev. 0, 60-Day Waste Compatibility Safety Issue and Final Results for Tank 241-A W-105, Grab Samples 5A W-95-1, 5A W-95-2 and 5A W-95-3. Three supernate samples exceeded the TOC notification limit (30,000 microg C/g dry weight). Appropriate notifications were made. No immediate notifications were required for any other analyte. The TSAP requested analyses for polychlorinated biphenyls (PCB) for all liquids and centrifuged solid subsamples. The PCB analysis of the liquid samples has been delayed and will be presented in a revision to this document

  11. Analysis of selected phytotoxins and mycotoxins in environmental samples.

    Science.gov (United States)

    Hoerger, Corinne C; Schenzel, Judith; Strobel, Bjarne W; Bucheli, Thomas D

    2009-11-01

    Natural toxins such as phytotoxins and mycotoxins have been studied in food and feed for decades, but little attention has yet been paid to their occurrence in the environment. Because of increasing awareness of the presence and potential relevance of micropollutants in the environment, phytotoxins and mycotoxins should be considered and investigated as part of the chemical cocktail in natural samples. Here, we compile chemical analytical methods to determine important phytotoxins (i.e. phenolic acids, quinones, benzoxazinones, terpenoids, glycoalkaloids, glucosinolates, isothiocyanates, phytosterols, flavonoids, coumestans, lignans, and chalcones) and mycotoxins (i.e. resorcyclic acid lactones, trichothecenes, fumonisins, and aflatoxins) in environmentally relevant matrices such as surface water, waste water-treatment plant influent and effluent, soil, sediment, manure, and sewage sludge. The main problems encountered in many of the reviewed methods were the frequent unavailability of suitable internal standards (especially isotope-labelled analogues) and often absent or fragmentary method optimization and validation.

  12. Toward greener analytical techniques for the absolute quantification of peptides in pharmaceutical and biological samples.

    Science.gov (United States)

    Van Eeckhaut, Ann; Mangelings, Debby

    2015-09-10

    Peptide-based biopharmaceuticals represent one of the fastest growing classes of new drug molecules. New reaction types included in the synthesis strategies to reduce the rapid metabolism of peptides, along with the availability of new formulation and delivery technologies, resulted in an increased marketing of peptide drug products. In this regard, the development of analytical methods for quantification of peptides in pharmaceutical and biological samples is of utmost importance. From the sample preparation step to their analysis by means of chromatographic or electrophoretic methods, many difficulties should be tackled to analyze them. Recent developments in analytical techniques emphasize more and more on the use of green analytical techniques. This review will discuss the progresses in and challenges observed during green analytical method development for the quantification of peptides in pharmaceutical and biological samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Distribution of Heavy Metal Content Hg and Cr of Environmental Samples at Surabaya Area

    International Nuclear Information System (INIS)

    Agus Taftazani

    2007-01-01

    Determination of Hg and Cr content of Surabaya river and coastal environmental samples using Instrumental Neutron Activation Analysis (INAA) have been done. The environmental samples were water, sediment, Eichhornia crassipes (Mart) Solmms, Rhizophora stylosa, Johnius (Johnieops) borneensis fish, and Moolgarda delicate fish at 12 locations selected of Surabaya area. Dry powder of sediment and biotic samples and concentrate water samples was irradiated by neutron flux 1.05 x 10 11 n.cm -2 .det -1 during 12 hours. The analytical result showed that the concentration of the heavy metals of river water are smaller than Perda Surabaya City No. 02/2004 for the 4 th level water which are Hg (0.005 ppm) and Cr (1.000 ppm). All locations coastal water samples have Hg and Cr concentrations are higher than Kepmen LH No.51/2004 Hg (0.001 ppm) and Cr (0.005 ppm). The Hg concentration of fish samples have exceeded the threshold according to Kep. Dirjen POM No.03725/B/SK/VII/89 about the maximum concentration of metal pollution in food. The concentration of heavy metals in sediment, Eichhornia crassipes (Mart) Solmms and Rhizophora stylosa are not regulated, so then heavy metals pollution can not be referred to. The concentration of Hg and Cr elements of water samples are smaller than that of biotic and sediment samples. The distribution factor (F d ) is bigger than bioaccumulation factor (F b ). (author)

  14. Use of robotic systems for radiochemical sample changing and for analytical sample preparation

    International Nuclear Information System (INIS)

    Delmastro, J.R.; Hartenstein, S.D.; Wade, M.A.

    1989-01-01

    Two uses of the Perkin-Elmer (PE) robotic system will be presented. In the first, a PE robot functions as an automatic sample changer for up to five low energy photon spectrometry (LEPS) detectors operated with a Nuclear Data ND 6700 system. The entire system, including the robot, is controlled by an IBM PC-AT using software written in compiled BASIC. Problems associated with the development of the system and modifications to the robot will be presented. In the second, an evaluation study was performed to assess the abilities of the PE robotic system for performing complex analytical sample preparation procedures. For this study, a robotic system based upon the PE robot and auxiliary devices was constructed and programmed to perform the preparation of final product samples (UO 3 ) for accountability and impurity specification analyses. These procedures require sample dissolution, dilution, and liquid-liquid extraction steps. The results of an in-depth evaluation of all system components will be presented

  15. Development of a radiochemical neutron activation analysis procedure for determination of rhenium in biological and environmental samples at ultratrace level

    Czech Academy of Sciences Publication Activity Database

    Kučera, Jan; Byrne, A. R.; Mizera, Jiří; Lučaníková, M.; Řanda, Zdeněk

    2006-01-01

    Roč. 269, č. 2 (2006), s. 251-257 ISSN 0236-5731 R&D Projects: GA ČR(CZ) GA203/04/0943 Institutional research plan: CEZ:AV0Z10480505 Keywords : radiochemical neutron activation analysis * rhenium * biological and environmental samples Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.509, year: 2006

  16. Implementation of Mass Spectrometry for Bulk Analysis of Environmental and Nuclear Material Inspection Samples

    International Nuclear Information System (INIS)

    Bulyha, S.; Cunningham, A.; Koepf, A.; Macsik, Z.; Poths, J.

    2015-01-01

    In the frame of the ECAS project (Enhancing Capabilities of Safeguards Analytical Services) the IAEA Office of Safeguards Analytical Services has implemented the latest-generation inductively coupled plasma mass spectrometers, or ICP-MS, for (i) bulk analysis of uranium and plutonium isotopes in environmental inspection samples and (ii) impurity analyzes in uranium samples. The measurement accuracy for n(U-235)/ n(U-238) ratios has been improved by approximately five times with the new multi-collector ICP-MS equipment. Use of modern ICP-MS enabled also an improvement of instrumental detection limits for U-233 and U-236 and Pu isotopes by at least one order of magnitude in comparison to the values, which had been achieved with the previously used methods. The improved accuracy and precision for isotope ratio measurements is mainly due to the higher sensitivity and the possibility to simultaneously detect several U isotopes with a multi-collector detector block. Implementation of the ICP-MS has also demonstrated a possibility for an increased sample throughput. In parallel to the implementation of the ICP-MS, a new version of the ''modified total evaporation'' (MTE) method has been developed for isotopic analysis of uranium samples by multi-collector thermal ionization mass spectrometry (TIMS). The MTE method provides a measurement performance which is, in particular for minor uranium isotopes, by several orders of magnitude superior compared to the commonly used ''total evaporation'' method. The new mass spectrometric techniques significantly improve the capability of the IAEA safeguards laboratories to detect the presence of non-natural uranium and plutonium isotopes in environmental swipe samples and to identify previously imperceptible differences in nuclear ''signatures''. Thus, they enhance the IAEA's ability to obtain independent, timely and quality-assured safeguards-relevant data and ensure

  17. Recent advances in analytical methods for the determination of 4-alkylphenols and bisphenol A in solid environmental matrices: A critical review.

    Science.gov (United States)

    Salgueiro-González, N; Castiglioni, S; Zuccato, E; Turnes-Carou, I; López-Mahía, P; Muniategui-Lorenzo, S

    2018-09-18

    The problem of endocrine disrupting compounds (EDCs) in the environment has become a worldwide concern in recent decades. Besides their toxicological effects at low concentrations and their widespread use in industrial and household applications, these pollutants pose a risk for non-target organisms and also for public safety. Analytical methods to determine these compounds at trace levels in different matrices are urgently needed. This review critically discusses trends in analytical methods for well-known EDCs like alkylphenols and bisphenol A in solid environmental matrices, including sediment and aquatic biological samples (from 2006 to 2018). Information about extraction, clean-up and determination is covered in detail, including analytical quality parameters (QA/QC). Conventional and novel analytical techniques are compared, with their advantages and drawbacks. Ultrasound assisted extraction followed by solid phase extraction clean-up is the most widely used procedure for sediment and aquatic biological samples, although softer extraction conditions have been employed for the latter. The use of liquid chromatography followed by tandem mass spectrometry has greatly increased in the last five years. The majority of these methods have been employed for the analysis of river sediments and bivalve molluscs because of their usefulness in aquatic ecosystem (bio)monitoring programs. Green, simple, fast analytical methods are now needed to determine these compounds in complex matrices. Copyright © 2018 Elsevier B.V. All rights reserved.

  18. Best-Matched Internal Standard Normalization in Liquid Chromatography-Mass Spectrometry Metabolomics Applied to Environmental Samples.

    Science.gov (United States)

    Boysen, Angela K; Heal, Katherine R; Carlson, Laura T; Ingalls, Anitra E

    2018-01-16

    The goal of metabolomics is to measure the entire range of small organic molecules in biological samples. In liquid chromatography-mass spectrometry-based metabolomics, formidable analytical challenges remain in removing the nonbiological factors that affect chromatographic peak areas. These factors include sample matrix-induced ion suppression, chromatographic quality, and analytical drift. The combination of these factors is referred to as obscuring variation. Some metabolomics samples can exhibit intense obscuring variation due to matrix-induced ion suppression, rendering large amounts of data unreliable and difficult to interpret. Existing normalization techniques have limited applicability to these sample types. Here we present a data normalization method to minimize the effects of obscuring variation. We normalize peak areas using a batch-specific normalization process, which matches measured metabolites with isotope-labeled internal standards that behave similarly during the analysis. This method, called best-matched internal standard (B-MIS) normalization, can be applied to targeted or untargeted metabolomics data sets and yields relative concentrations. We evaluate and demonstrate the utility of B-MIS normalization using marine environmental samples and laboratory grown cultures of phytoplankton. In untargeted analyses, B-MIS normalization allowed for inclusion of mass features in downstream analyses that would have been considered unreliable without normalization due to obscuring variation. B-MIS normalization for targeted or untargeted metabolomics is freely available at https://github.com/IngallsLabUW/B-MIS-normalization .

  19. International Congress on Analytical Chemistry. Abstracts. V. 2

    International Nuclear Information System (INIS)

    1997-01-01

    The collection of materials of the international congress on analytical chemistry taken place in Moscow in June 1997 is presented. The main directs of investigations are elucidated in such regions of analytical chemistry as quantitative and qualitative chemical analysis, sample preparation, express test methods of environmental and biological materials, clinical analysis, analysis of food and agricultural products

  20. International Congress on Analytical Chemistry. Abstracts. V. 2

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1998-12-31

    The collection of materials of the international congress on analytical chemistry taken place in Moscow in June 1997 is presented. The main directs of investigations are elucidated in such regions of analytical chemistry as quantitative and qualitative chemical analysis, sample preparation, express test methods of environmental and biological materials, clinical analysis, analysis of food and agricultural products

  1. ENVIRONMENTAL SAMPLING USING LOCATION SPECIFIC AIR MONITORING IN BULK HANDLING FACILITIES

    Energy Technology Data Exchange (ETDEWEB)

    Sexton, L.; Hanks, D.; Degange, J.; Brant, H.; Hall, G.; Cable-Dunlap, P.; Anderson, B.

    2011-06-07

    Since the introduction of safeguards strengthening measures approved by the International Atomic Energy Agency (IAEA) Board of Governors (1992-1997), international nuclear safeguards inspectors have been able to utilize environmental sampling (ES) (e.g. deposited particulates, air, water, vegetation, sediments, soil and biota) in their safeguarding approaches at bulk uranium/plutonium handling facilities. Enhancements of environmental sampling techniques used by the IAEA in drawing conclusions concerning the absence of undeclared nuclear materials or activities will soon be able to take advantage of a recent step change improvement in the gathering and analysis of air samples at these facilities. Location specific air monitoring feasibility tests have been performed with excellent results in determining attribute and isotopic composition of chemical elements present in an actual test-bed sample. Isotopic analysis of collected particles from an Aerosol Contaminant Extractor (ACE) collection, was performed with the standard bulk sampling protocol used throughout the IAEA network of analytical laboratories (NWAL). The results yielded bulk isotopic values expected for the operations. Advanced designs of air monitoring instruments such as the ACE may be used in gas centrifuge enrichment plants (GCEP) to detect the production of highly enriched uranium (HEU) or enrichments not declared by a State. Researchers at Savannah River National Laboratory in collaboration with Oak Ridge National Laboratory are developing the next generation of ES equipment for air grab and constant samples that could become an important addition to the international nuclear safeguards inspector's toolkit. Location specific air monitoring to be used to establish a baseline environmental signature of a particular facility employed for comparison of consistencies in declared operations will be described in this paper. Implementation of air monitoring will be contrasted against the use of smear

  2. Manual of selected physico-chemical analytical methods. IV

    International Nuclear Information System (INIS)

    Beran, M.; Klosova, E.; Krtil, J.; Sus, F.; Kuvik, V.; Vrbova, L.; Hamplova, M.; Lengyel, J.; Kelnar, L.; Zakouril, K.

    1990-11-01

    The Central Testing Laboratory of the Nuclear Research Institute at Rez has for a decade been participating in the development of analytical procedures and has been providing analyses of samples of different types and origin. The analytical procedures developed have been published in special journals and a number of them in the Manuals of analytical methods, in three parts. The 4th part of the Manual contains selected physico-chemical methods developed or modified by the Laboratory in the years 1986-1990 within the project ''Development of physico-chemical analytical methods''. In most cases, techniques are involved for non-nuclear applications. Some can find wider applications, especially in analyses of environmental samples. Others have been developed for specific cases of sample analyses or require special instrumentation (mass spectrometer), which partly restricts their applicability by other institutions. (author)

  3. A GPU code for analytic continuation through a sampling method

    Directory of Open Access Journals (Sweden)

    Johan Nordström

    2016-01-01

    Full Text Available We here present a code for performing analytic continuation of fermionic Green’s functions and self-energies as well as bosonic susceptibilities on a graphics processing unit (GPU. The code is based on the sampling method introduced by Mishchenko et al. (2000, and is written for the widely used CUDA platform from NVidia. Detailed scaling tests are presented, for two different GPUs, in order to highlight the advantages of this code with respect to standard CPU computations. Finally, as an example of possible applications, we provide the analytic continuation of model Gaussian functions, as well as more realistic test cases from many-body physics.

  4. 40 CFR 90.421 - Dilute gaseous exhaust sampling and analytical system description.

    Science.gov (United States)

    2010-07-01

    ... gas mixture temperature, measured at a point immediately ahead of the critical flow venturi, must be... analytical system description. (a) General. The exhaust gas sampling system described in this section is... requirements are as follows: (1) This sampling system requires the use of a Positive Displacement Pump—Constant...

  5. Interpolation and sampling in spaces of analytic functions

    CERN Document Server

    Seip, Kristian

    2004-01-01

    The book is about understanding the geometry of interpolating and sampling sequences in classical spaces of analytic functions. The subject can be viewed as arising from three classical topics: Nevanlinna-Pick interpolation, Carleson's interpolation theorem for H^\\infty, and the sampling theorem, also known as the Whittaker-Kotelnikov-Shannon theorem. The book aims at clarifying how certain basic properties of the space at hand are reflected in the geometry of interpolating and sampling sequences. Key words for the geometric descriptions are Carleson measures, Beurling densities, the Nyquist rate, and the Helson-Szegő condition. The book is based on six lectures given by the author at the University of Michigan. This is reflected in the exposition, which is a blend of informal explanations with technical details. The book is essentially self-contained. There is an underlying assumption that the reader has a basic knowledge of complex and functional analysis. Beyond that, the reader should have some familiari...

  6. Study of Long-Lived Radionuclides in Environmental Samples by ICP-MS

    International Nuclear Information System (INIS)

    Conde, E.; Navarro, N.; Fernández, M.

    2015-01-01

    Thorium is considered as one of the highly radiotoxic elements, because following its decay a number of other α, β and/or γ emitting daughters are produced. Uranium mining and processing, as well as remediation of impacted soils, are one of the principal anthropogenic sources of thorium release to the air, soil and water. Measurement of Th isotopes requires the use of analytical techniques capable of reliably measure the content of Th isotopes at trace levels. 230Th determination has generally been performed by α-spectrometry. However, this method needs sample preparation of 3-4 days and counting times from days to up to two weeks. A way to face this difficulty is the use of inductively coupled plasma mass spectrometry (ICP-MS). This technique is adequate for the determination of 232Th and 238U, long-lived radionuclides, and it can be applied, successfully, in the determination of 230Th, particularly if it is associated with a pre-concentration stage. This work presents the development of a rapid and simple analytical procedure based on mass spectrometry for the determination of 230Th and the results obtained in the analysis of environmental filters.

  7. AN APPLICATION OF FLOW INJECTION ANALYSIS WITH GAS DIFFUSION AND SPECTROPHOTOMETRIC DETECTION FOR THE MONITORING OF DISSOLVED SULPHIDE CONCENTRATION IN ENVIRONMENTAL SAMPLES

    Directory of Open Access Journals (Sweden)

    Malwina Cykowska

    2014-10-01

    Full Text Available The monitoring of the concentration of sulphide is very important from the environment point of view because of high toxicity of hydrogen sulphide. What is more hydrogen sulphide is an important pollution indicator. In many cases the determination of sulphide is very difficult due to complicated matrix of some environmental samples, which causes that most analytical methods cannot be used. Flow injection analysis allows to avoid matrix problem what makes it suitable for a wide range of applications in analytical laboratories. In this paper determination of dissolved sulphide in environmental samples by gas-diffusion flow injection analysis with spectrophotometric detection was presented. Used gas-diffusion separation ensures the elimination of interferences caused by sample matrix and gives the ability of determination of sulphides in coloured and turbid samples. Studies to optimize the measurement conditions and to determine the value of the validation parameters (e.g. limit of detection, limit of quantification, precision, accuracy were carried out. Obtained results confirm the usefulness of the method for monitoring the concentration of dissolved sulphides in water and waste water. Full automation and work in a closed system greatly reduces time of analysis, minimizes consumption of sample and reagents and increases safety of analyst’s work.

  8. Advances in organic-inorganic hybrid sorbents for the extraction of organic and inorganic pollutants in different types of food and environmental samples.

    Science.gov (United States)

    Ng, Nyuk-Ting; Kamaruddin, Amirah Farhan; Wan Ibrahim, Wan Aini; Sanagi, Mohd Marsin; Abdul Keyon, Aemi S

    2018-01-01

    The efficiency of the extraction and removal of pollutants from food and the environment has been an important issue in analytical science. By incorporating inorganic species into an organic matrix, a new material known as an organic-inorganic hybrid material is formed. As it possesses high selectivity, permeability, and mechanical and chemical stabilities, organic-inorganic hybrid materials constitute an emerging research field and have become popular to serve as sorbents in various separaton science methods. Here, we review recent significant advances in analytical solid-phase extraction employing organic-inorganic composite/nanocomposite sorbents for the extraction of organic and inorganic pollutants from various types of food and environmental matrices. The physicochemical characteristics, extraction properties, and analytical performances of sorbents are discussed; including morphology and surface characteristics, types of functional groups, interaction mechanism, selectivity and sensitivity, accuracy, and regeneration abilities. Organic-inorganic hybrid sorbents combined with extraction techniques are highly promising for sample preparation of various food and environmental matrixes with analytes at trace levels. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Means of introducing an analyte into liquid sampling atmospheric pressure glow discharge

    Science.gov (United States)

    Marcus, R. Kenneth; Quarles, Jr., Charles Derrick; Russo, Richard E.; Koppenaal, David W.; Barinaga, Charles J.; Carado, Anthony J.

    2017-01-03

    A liquid sampling, atmospheric pressure, glow discharge (LS-APGD) device as well as systems that incorporate the device and methods for using the device and systems are described. The LS-APGD includes a hollow capillary for delivering an electrolyte solution to a glow discharge space. The device also includes a counter electrode in the form of a second hollow capillary that can deliver the analyte into the glow discharge space. A voltage across the electrolyte solution and the counter electrode creates the microplasma within the glow discharge space that interacts with the analyte to move it to a higher energy state (vaporization, excitation, and/or ionization of the analyte).

  10. On-line preconcentration and determination of mercury in biological and environmental samples by cold vapor-atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Ferrua, N.; Cerutti, S.; Salonia, J.A.; Olsina, R.A.; Martinez, L.D.

    2007-01-01

    An on-line procedure for the determination of traces of total mercury in environmental and biological samples is described. The present methodology combines cold vapor generation associated to atomic absorption spectrometry (CV-AAS) with preconcentration of the analyte on a minicolumn packed with activated carbon. The retained analyte was quantitatively eluted from the minicolumn with nitric acid. After that, volatile specie of mercury was generated by merging the acidified sample and sodium tetrahydroborate(III) in a continuous flow system. The gaseous analyte was subsequently introduced via a stream of Ar carrier into the atomizer device. Optimizations of both, preconcentration and mercury volatile specie generation variables were carried out using two level full factorial design (2 3 ) with 3 replicates of the central point. Considering a sample consumption of 25 mL, an enrichment factor of 13-fold was obtained. The detection limit (3σ) was 10 ng L -1 and the precision (relative standard deviation) was 3.1% (n = 10) at the 5 μg L -1 level. The calibration curve using the preconcentration system for mercury was linear with a correlation coefficient of 0.9995 at levels near the detection limit up to at least 1000 μg L -1 . Satisfactory results were obtained for the analysis of mercury in tap water and hair samples

  11. Environmental Monitoring Plan: Environmental Monitoring Section. Appendix A, Procedures

    International Nuclear Information System (INIS)

    1995-02-01

    This document presents information about the environmental monitoring program at Lawrence Livermore National Laboratory. Topics discussed include: air sampling; air tritium calibrations; storm water discharge; non-storm water discharge; sampling locations; ground water sampling; noise and blast forecasting; analytical laboratory auditing; document retention; procedure writing; quality assurance programs for sampling; soil and sediment sampling; sewage sampling; diversion facility tank sampling; vegetation and foodstuff sampling; and radiological dose assessments

  12. Environmental Monitoring Plan: Environmental Monitoring Section. Appendix A, Procedures

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1995-02-01

    This document presents information about the environmental monitoring program at Lawrence Livermore National Laboratory. Topics discussed include: air sampling; air tritium calibrations; storm water discharge; non-storm water discharge; sampling locations; ground water sampling; noise and blast forecasting; analytical laboratory auditing; document retention; procedure writing; quality assurance programs for sampling; soil and sediment sampling; sewage sampling; diversion facility tank sampling; vegetation and foodstuff sampling; and radiological dose assessments.

  13. Molecularly imprinted polymers--potential and challenges in analytical chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Mahony, J.O. [Dublin City University, School of Chemical Sciences, Glasnevin, Dublin 9 (Ireland); Nolan, K. [Dublin City University, School of Chemical Sciences, Glasnevin, Dublin 9 (Ireland); Smyth, M.R. [Dublin City University, School of Chemical Sciences, Glasnevin, Dublin 9 (Ireland); Mizaikoff, B. [Georgia Institute of Technology, School of Chemistry and Biochemistry, 770 State Street, Boggs Building, Atlanta, GA 30332-0400 (United States)]. E-mail: boris.mizaikoff@chemistry.gatech.edu

    2005-04-04

    Among the variety of biomimetic recognition schemes utilizing supramolecular approaches molecularly imprinted polymers (MIPs) have proven their potential as synthetic receptors in numerous applications ranging from liquid chromatography to assays and sensor technology. Their inherent advantages compared to biochemical/biological recognition systems include robustness, storage endurance and lower costs. However, until recently only few contributions throughout the relevant literature describe quantitative analytical applications of MIPs for practically relevant analyte molecules and real-world samples. Increased motivation to thoroughly evaluate the true potential of MIP technology is clearly attributed to the demands of modern analytical chemistry, which include enhanced sensitivity, selectivity and applicability of molecular recognition building blocks at decreasing costs. In particular, the areas of environmental monitoring, food and beverage analysis and industrial process surveillance require analytical tools capable of discriminating chemicals with high molecular specificity considering increasing numbers of complex environmental contaminants, pollution of raw products and rigorous quality control requested by legislation and consumer protection. Furthermore, efficient product improvement and development of new products requires precise qualitative and quantitative analytical methods. Finally, environmental, food and process safety control issues favor the application of on-line in situ analytical methods with high molecular selectivity. While biorecognition schemes frequently suffer from degrading bioactivity and long-term stability when applied in real-world sample environments, MIPs serving as synthetic antibodies have successfully been applied as stationary phase separation matrix (e.g. HPLC and SPE), recognition component in bioassays (e.g. ELISA) or biomimetic recognition layer in chemical sensor systems. Examples such as MIP-based selective analysis of

  14. Molecularly imprinted polymers--potential and challenges in analytical chemistry

    International Nuclear Information System (INIS)

    Mahony, J.O.; Nolan, K.; Smyth, M.R.; Mizaikoff, B.

    2005-01-01

    Among the variety of biomimetic recognition schemes utilizing supramolecular approaches molecularly imprinted polymers (MIPs) have proven their potential as synthetic receptors in numerous applications ranging from liquid chromatography to assays and sensor technology. Their inherent advantages compared to biochemical/biological recognition systems include robustness, storage endurance and lower costs. However, until recently only few contributions throughout the relevant literature describe quantitative analytical applications of MIPs for practically relevant analyte molecules and real-world samples. Increased motivation to thoroughly evaluate the true potential of MIP technology is clearly attributed to the demands of modern analytical chemistry, which include enhanced sensitivity, selectivity and applicability of molecular recognition building blocks at decreasing costs. In particular, the areas of environmental monitoring, food and beverage analysis and industrial process surveillance require analytical tools capable of discriminating chemicals with high molecular specificity considering increasing numbers of complex environmental contaminants, pollution of raw products and rigorous quality control requested by legislation and consumer protection. Furthermore, efficient product improvement and development of new products requires precise qualitative and quantitative analytical methods. Finally, environmental, food and process safety control issues favor the application of on-line in situ analytical methods with high molecular selectivity. While biorecognition schemes frequently suffer from degrading bioactivity and long-term stability when applied in real-world sample environments, MIPs serving as synthetic antibodies have successfully been applied as stationary phase separation matrix (e.g. HPLC and SPE), recognition component in bioassays (e.g. ELISA) or biomimetic recognition layer in chemical sensor systems. Examples such as MIP-based selective analysis of

  15. Determination of total mercury for marine environmental monitoring studies by solid sampling continuum source high resolution atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mandjukov, Petko; Orani, Anna Maria; Han, Eunmi; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    The most critical step in almost all commonly used analytical procedures for Hg determination is the sample preparation due to its extreme volatility. One of the possible solutions of this problem is the application of methods for direct analysis of solid samples. The possibilities for solid sampling high resolution continuum source atomic absorption spectrometry (HR CS AAS) determination of total mercury in various marine environmental samples e.g. sediments and biota are object of the present study. The instrumental parameters were optimized in order to obtain reproducible and interference free analytical signal. A calibration technique based on the use of solid standard certified reference materials similar to the nature of the analyzed sample was developed and applied to various CRMs and real samples. This technique allows simple and reliable evaluation of the uncertainty of the result and the metrological characteristics of the method. A validation approach in line with the requirements of ISO 17025 standard and Eurachem guidelines was followed. With this in mind, selectivity, working range (0.06 to 25 ng for biota and 0.025 to 4 ng for sediment samples, expressed as total Hg) linearity (confirmed by Student's t-test), bias (1.6–4.3%), repeatability (4–9%), reproducibility (9–11%), and absolute limit of detection (0.025 ng for sediment, 0.096 ng for marine biota) were systematically assessed using solid CRMs. The relative expanded uncertainty was estimated at 15% for sediment sample and 8.5% for marine biota sample (k = 2). Demonstration of traceability of measurement results is also presented. The potential of the proposed analytical procedure, based on solid sampling HR CS AAS technique was demonstrated by direct analysis of sea sediments form the Caribbean region and various CRMs. Overall, the use of solid sampling HR CS AAS permits obtaining significant advantages for the determination of this complex analyte in marine samples, such as

  16. Microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid for the determination of sulfonamides in environmental water samples.

    Science.gov (United States)

    Song, Ying; Wu, Lijie; Lu, Chunmei; Li, Na; Hu, Mingzhu; Wang, Ziming

    2014-12-01

    An easy, quick, and green method, microwave-assisted liquid-liquid microextraction based on solidification of ionic liquid, was first developed and applied to the extraction of sulfonamides in environmental water samples. 1-Ethy-3-methylimidazolium hexafluorophosphate, which is a solid-state ionic liquid at room temperature, was used as extraction solvent in the present method. After microwave irradiation for 90 s, the solid-state ionic liquid was melted into liquid phase and used to finish the extraction of the analytes. The ionic liquid and sample matrix can be separated by freezing and centrifuging. Several experimental parameters, including amount of extraction solvent, microwave power and irradiation time, pH of sample solution, and ionic strength, were investigated and optimized. Under the optimum experimental conditions, good linearity was observed in the range of 2.00-400.00 μg/L with the correlation coefficients ranging from 0.9995 to 0.9999. The limits of detection for sulfathiazole, sulfachlorpyridazine, sulfamethoxazole, and sulfaphenazole were 0.39, 0.33, 0.62, and 0.85 μg/L, respectively. When the present method was applied to the analysis of environmental water samples, the recoveries of the analytes ranged from 75.09 to 115.78% and relative standard deviations were lower than 11.89%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Rapid Gamma Screening of Shipments of Analytical Samples to Meet DOT Regulations

    International Nuclear Information System (INIS)

    Wojtaszek, P.A.; Remington, D.L.; Ideker-Mulligan, V.

    2006-01-01

    The accelerated closure program at Rocky Flats required the capacity to ship up to 1000 analytical samples per week to off-site commercial laboratories, and to conduct such shipment within 24 hours of sample collection. During a period of near peak activity in the closure project, a regulatory change significantly increased the level of radionuclide data required for shipment of each package. In order to meet these dual challenges, a centralized and streamlined sample management program was developed which channeled analytical samples through a single, high-throughput radiological screening facility. This trailerized facility utilized high purity germanium (HPGe) gamma spectrometers to conduct screening measurements of entire packages of samples at once, greatly increasing throughput compared to previous methods. The In Situ Object Counting System (ISOCS) was employed to calibrate the HPGe systems to accommodate the widely varied sample matrices and packing configurations encountered. Optimum modeling and configuration parameters were determined. Accuracy of the measurements of grouped sample jars was confirmed with blind samples in multiple configurations. Levels of radionuclides not observable by gamma spectroscopy were calculated utilizing a spreadsheet program that can accommodate isotopic ratios for large numbers of different waste streams based upon acceptable knowledge. This program integrated all radionuclide data and output all information required for shipment, including the shipping class of the package. (authors)

  18. Sample preparation of environmental samples using benzene synthesis followed by high-performance LSC

    International Nuclear Information System (INIS)

    Filippis, S. De; Noakes, J.E.

    1991-01-01

    Liquid scintillation counting (LSC) techniques have been widely employed as the detection method for determining environmental levels of tritium and 14 C. Since anthropogenic and nonanthropogenic inputs to the environment are a concern, sampling the environment surrounding a nuclear power facility or fuel reprocessing operation requires the collection of many different sample types, including agriculture products, water, biota, aquatic life, soil, and vegetation. These sample types are not suitable for the direct detection of tritium of 14 C for liquid scintillation techniques. Each sample type must be initially prepared in order to obtain the carbon or hydrogen component of interest and present this in a chemical form that is compatible with common chemicals used in scintillation counting applications. Converting the sample of interest to chemically pure benzene as a sample preparation technique has been widely accepted for processing samples for radiocarbon age-dating applications. The synthesized benzene is composed of the carbon or hydrogen atoms from the original sample and is ideal as a solvent for LSC with excellent photo-optical properties. Benzene synthesis followed by low-background scintillation counting can be applied to the preparation and measurement of environmental samples yielding good detection sensitivities, high radionuclide counting efficiency, and shorter preparation time. The method of benzene synthesis provides a unique approach to the preparation of a wide variety of environmental sample types using similar chemistry for all samples

  19. Future analytical provision - Relocation of Sellafield Ltd Analytical Services Laboratory

    International Nuclear Information System (INIS)

    Newell, B.

    2015-01-01

    Sellafield Ltd Analytical Services provide an essential view on the environmental, safety, process and high hazard risk reduction performances by analysis of samples. It is the largest and most complex analytical services laboratory in Europe, with 150 laboratories (55 operational) and 350 staff (including 180 analysts). Sellafield Ltd Analytical Services Main Laboratory is in need of replacement. This is due to the age of the facility and changes to work streams. This relocation is an opportunity to -) design and commission bespoke MA (Medium-Active) cells, -) modify HA (High-Active) cell design to facilitate an in-cell laboratory, -) develop non-destructive techniques, -) open light building for better worker morale. The option chosen was to move the activities to the NNL Central laboratory (NNLCL) that is based at Sellafield and is the UK's flagship nuclear research and development facility. This poster gives a time schedule

  20. The Development of Low-Level Measurement Capabilities for Total and Isotopic Uranium in Environmental Samples at Brazilian and Argentine Laboratories by ABACC

    International Nuclear Information System (INIS)

    Guidicini, Olga M.; Olsen, Khris B.; Hembree, Doyle M.; Carter, Joel A.; Whitaker, Michael; Hayes, Susan M.

    2005-01-01

    In June 1998, the Brazilian-Argentine Agency for Accounting and Control of Nuclear Materials (ABACC), with assistance from the U.S. Department of Energy (DOE), began a program to assess environmental sampling and analysis capabilities at laboratories in Argentina and Brazil. The program began with staff training conducted in South America and the United States by Oak Ridge National Laboratory (ORNL) and Pacific Northwest National Laboratory (PNNL). Both laboratories are participating members of DOE's Network of Analytical Laboratories (NWAL) that support IAEA's environmental sampling program. During the initial planning meeting, representatives from ABACC and all the participating analytical laboratories supporting ABACC were briefed on how the first exercise would be managed and on key aspects necessary to analyze low-level environmental samples for uranium. Subsequent to this training, a laboratory evaluation exercise (Exercise 1) was conducted using standard swipe samples prepared for this exercise by the International Atomic Energy Agency (IAEA). The results of Exercise 1 determined that sample contamination was a major factor in the analysis, and a thorough review of laboratory procedures was required to reduce the level of contamination to acceptable levels. Following modification of sample preparation procedures, the laboratories performed Exercise 2, an analysis of a National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) 1547, Peach Leaves. The results of Exercise 2 demonstrated that several laboratories were capable of accurately determining the total uranium and uranium isotopic distribution in the peach leaves. To build on these successes, Exercise 3 was performed using a series of standard swipe samples prepared by the IAEA and distributed to laboratories supporting ABACC and to PNNL and ORNL. The results of Exercise 3 demonstrate that ABACC now has support laboratories in both Argentina and Brazil, which are capable of

  1. Road Transportable Analytical Laboratory system. Phase 1

    Energy Technology Data Exchange (ETDEWEB)

    Finger, S.M.; Keith, V.F.; Spertzel, R.O.; De Avila, J.C.; O`Donnell, M.; Vann, R.L.

    1993-09-01

    This developmental effort clearly shows that a Road Transportable Analytical Laboratory System is a worthwhile and achievable goal. The RTAL is designed to fully analyze (radioanalytes, and organic and inorganic chemical analytes) 20 samples per day at the highest levels of quality assurance and quality control. It dramatically reduces the turnaround time for environmental sample analysis from 45 days (at a central commercial laboratory) to 1 day. At the same time each RTAL system will save the DOE over $12 million per year in sample analysis costs compared to the costs at a central commercial laboratory. If RTAL systems were used at the eight largest DOE facilities (at Hanford, Savannah River, Fernald, Oak Ridge, Idaho, Rocky Flats, Los Alamos, and the Nevada Test Site), the annual savings would be $96,589,000. The DOE`s internal study of sample analysis needs projects 130,000 environmental samples requiring analysis in FY 1994, clearly supporting the need for the RTAL system. The cost and time savings achievable with the RTAL system will accelerate and improve the efficiency of cleanup and remediation operations throughout the DOE complex.

  2. Environmental science and technology

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2008-07-01

    The environmental Science and Technology Program was structured based on the continuous growth of environmental activities on areas related to nuclear programs at IPEN. The program comprehends five main areas: Environmental analysis: Chemical technology; Polymer technology nucleus: Chemical and Isotope characterization and Analytical Chemistry for the Nuclear Fuel Cycle samples.

  3. Surface-enhanced Raman scattering detection of silver nanoparticles in environmental and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Guo, Huiyuan [Stockbridge School of Agriculture, University of Massachusetts, Amherst, MA 01003 (United States); Xing, Baoshan, E-mail: bx@umass.edu [Stockbridge School of Agriculture, University of Massachusetts, Amherst, MA 01003 (United States); Hamlet, Leigh C.; Chica, Andrea [Stockbridge School of Agriculture, University of Massachusetts, Amherst, MA 01003 (United States); He, Lili, E-mail: lilihe@foodsci.umass.edu [Department of Food Science, University of Massachusetts, Amherst, MA 01003 (United States)

    2016-06-01

    Growing concerns over the potential release and threat of silver nanoparticles (AgNPs) to environmental and biological systems urge researchers to investigate their fate and behavior. However, current analytical techniques cannot meet the requirements for rapidly, sensitively and reliably probing AgNPs in complex matrices. Surface-enhanced Raman spectroscopy (SERS) has shown great capability for rapid detection of AgNPs based on an indicator molecule that can bind on the AgNP surface. The objective of this study was to exploit SERS to detect AgNPs in environmental and biological samples through optimizing the Raman indicator for SERS. Seven indicator molecules were selected and determined to obtain their SERS signals at optimal concentrations. Among them, 1,2-di(4-pyridyl)ethylene (BPE), crystal violet and ferric dimethyl-dithiocarbamate (ferbam) produced the highest SERS intensities. Further experiments on binding competition between each two of the three candidates showed that ferbam had the highest AgNPs-binding ability. The underlying mechanism lies in the strong binding affinity of ferbam with AgNPs via multiple sulfur atoms. We further validated ferbam to be an effective indicator for SERS detection of as low as 0.1 mg/L AgNPs in genuine surface water and 0.57 mg/L in spinach juice. Moreover, limited interference on SERS detection of AgNPs was found from environmentally relevant inorganic ions, organic matter, inorganic particles, as well as biologically relevant components, demonstrating the ferbam-assisted SERS is an effective and sensitive method to detect AgNPs in complex environmental and biological samples. - Graphical abstract: SERS signal intensity of ferbam indicates the concentration of AgNPs. - Highlights: • Ferbam was found to be the best indicator for SERS detection of AgNPs. • SERS was able to detect AgNPs in both environmental and biological samples. • Major components in the two matrices had limited effect on AgNP detection.

  4. Surface-enhanced Raman scattering detection of silver nanoparticles in environmental and biological samples

    International Nuclear Information System (INIS)

    Guo, Huiyuan; Xing, Baoshan; Hamlet, Leigh C.; Chica, Andrea; He, Lili

    2016-01-01

    Growing concerns over the potential release and threat of silver nanoparticles (AgNPs) to environmental and biological systems urge researchers to investigate their fate and behavior. However, current analytical techniques cannot meet the requirements for rapidly, sensitively and reliably probing AgNPs in complex matrices. Surface-enhanced Raman spectroscopy (SERS) has shown great capability for rapid detection of AgNPs based on an indicator molecule that can bind on the AgNP surface. The objective of this study was to exploit SERS to detect AgNPs in environmental and biological samples through optimizing the Raman indicator for SERS. Seven indicator molecules were selected and determined to obtain their SERS signals at optimal concentrations. Among them, 1,2-di(4-pyridyl)ethylene (BPE), crystal violet and ferric dimethyl-dithiocarbamate (ferbam) produced the highest SERS intensities. Further experiments on binding competition between each two of the three candidates showed that ferbam had the highest AgNPs-binding ability. The underlying mechanism lies in the strong binding affinity of ferbam with AgNPs via multiple sulfur atoms. We further validated ferbam to be an effective indicator for SERS detection of as low as 0.1 mg/L AgNPs in genuine surface water and 0.57 mg/L in spinach juice. Moreover, limited interference on SERS detection of AgNPs was found from environmentally relevant inorganic ions, organic matter, inorganic particles, as well as biologically relevant components, demonstrating the ferbam-assisted SERS is an effective and sensitive method to detect AgNPs in complex environmental and biological samples. - Graphical abstract: SERS signal intensity of ferbam indicates the concentration of AgNPs. - Highlights: • Ferbam was found to be the best indicator for SERS detection of AgNPs. • SERS was able to detect AgNPs in both environmental and biological samples. • Major components in the two matrices had limited effect on AgNP detection.

  5. Analytical quality assurance in laboratories using tracers for biological and environmental studies

    International Nuclear Information System (INIS)

    Melaj, Mariana; Martin, Olga; Lopez, Silvia; Rojas de Tramontini, Susana

    1999-01-01

    This work describe the way we are organizing a quality assurance system to apply in the analytical measurements of the relation 14 N/ 15 N in biological and soil material. The relation 14 / 15 is measured with a optic emission spectrometer (NOI6PC), which distinguish the differences in wave length of electromagnetic radiation emitted by N-28, N-29 and N-30. The major problem is the 'cross contamination' of samples with different enrichments. The elements that are been considered to reach satisfactory analytical results are: 1) A proper working area; 2) The samples must be homogeneous and the samples must represent the whole sampled system; 3) The use of reference materials. In each digestion, a known reference sample must be added; 4) Adequate equipment operation; 5) Standard operating procedures; 6) Control charts, laboratory and equipment books. All operations using the equipment is registered in a book; 7) Training of the operators. (author)

  6. Results Of Analytical Sample Crosschecks For Next Generation Solvent Extraction Samples Isopar L Concentration And pH

    International Nuclear Information System (INIS)

    Peters, T.; Fink, S.

    2011-01-01

    As part of the implementation process for the Next Generation Cesium Extraction Solvent (NGCS), SRNL and F/H Lab performed a series of analytical cross-checks to ensure that the components in the NGCS solvent system do not constitute an undue analytical challenge. For measurement of entrained Isopar(reg s ign) L in aqueous solutions, both labs performed similarly with results more reliable at higher concentrations (near 50 mg/L). Low bias occurred in both labs, as seen previously for comparable blind studies for the baseline solvent system. SRNL recommends consideration to use of Teflon(trademark) caps on all sample containers used for this purpose. For pH measurements, the labs showed reasonable agreement but considerable positive bias for dilute boric acid solutions. SRNL recommends consideration of using an alternate analytical method for qualification of boric acid concentrations.

  7. Comparative evaluation of the US Environmental Protection Agency's and the Oak Ridge Institute for Science and Education's environmental survey and site assessment program field sampling procedures

    International Nuclear Information System (INIS)

    Vitkus, T.J.; Bright, T.L.; Roberts, S.A.

    1997-10-01

    At the request of the U.S. Nuclear Regulatory Commission's (NRC's) Headquarters Office, the Environmental Survey and Site Assessment Program (ESSAP) of the Oak Ridge Institute for Science and Education (ORISE) compared the documented procedures that the U.S. Environmental Protection Agency (EPA) and ESSAP use for collecting environmental samples. The project objectives were to review both organizations' procedures applicable to collecting various sample matrices, compare the procedures for similarities and differences, and then to evaluate the reason for any identified procedural differences and their potential impact on ESSAP's sample data quality. The procedures reviewed included those for sampling surface and subsurface soil, surface and groundwater, vegetation, air, and removable surface contamination. ESSAP obtained copies of relevant EPA documents and reviewed and prepared a tabulated summary of each applicable procedure. The methods for collecting and handling each type of sample were evaluated for differences, and where these were identified, the significance and effect of the differences on analytical quality were determined. The results of the comparison showed that, overall, the procedures and methods that EPA and ESSAP use for sample collection are very similar. The number of minor differences noted were the result of restrictions or procedures necessary to ensure sample integrity and prevent the introduction of interfering compounds when samples are to be analyzed for chemical parameters. For most radio nuclide analyses, these additional procedures are not necessary. Another item noted was EPA's inclusion of steps that reduce the potential for sample cross-contamination by preparing (dressing) a location prior to collecting a sample or removing a portion of a sample prior to containerization

  8. Streamlined sample cleanup using combined dispersive solid-phase extraction and in-vial filtration for analysis of pesticides and environmental pollutants in shrimp.

    Science.gov (United States)

    Han, Lijun; Sapozhnikova, Yelena; Lehotay, Steven J

    2014-05-27

    A new method of sample preparation was developed and is reported for the first time. The approach combines in-vial filtration with dispersive solid-phase extraction (d-SPE) in a fast and convenient cleanup of QuEChERS (quick, easy, cheap, effective, rugged, and safe) extracts. The method was applied to simultaneous analysis of 42 diverse pesticides and 17 environmental contaminants, including polycyclic aromatic hydrocarbons, polychlorinated biphenyls (PCBs), and flame retardants, in shrimp as the sample matrix. Final extracts were analyzed by both low-pressure gas chromatography - triple quadrupole tandem mass spectrometry (LPGC-MS/MS), and high-performance liquid chromatography - triple quadrupole tandem mass spectrometry (HPLC-MS/MS) to provide a wide scope of analysis for targeted analytes. During method development, several different commercial sorbents for d-SPE were investigated and compared with respect to analyte recoveries. The method was validated at 10, 50, and 100 ng g(-1) spiking levels (10-fold lower for PCBs), and the results for nearly all analytes were between 70 and 115% recoveries with ≤17% relative standard deviations. The method was shown to be simple, fast, and effective for multi-application analysis of chemical residues in the representative food and environmental marker matrix. Copyright © 2014. Published by Elsevier B.V.

  9. Analytic continuation of quantum Monte Carlo data. Stochastic sampling method

    Energy Technology Data Exchange (ETDEWEB)

    Ghanem, Khaldoon; Koch, Erik [Institute for Advanced Simulation, Forschungszentrum Juelich, 52425 Juelich (Germany)

    2016-07-01

    We apply Bayesian inference to the analytic continuation of quantum Monte Carlo (QMC) data from the imaginary axis to the real axis. Demanding a proper functional Bayesian formulation of any analytic continuation method leads naturally to the stochastic sampling method (StochS) as the Bayesian method with the simplest prior, while it excludes the maximum entropy method and Tikhonov regularization. We present a new efficient algorithm for performing StochS that reduces computational times by orders of magnitude in comparison to earlier StochS methods. We apply the new algorithm to a wide variety of typical test cases: spectral functions and susceptibilities from DMFT and lattice QMC calculations. Results show that StochS performs well and is able to resolve sharp features in the spectrum.

  10. Estimating the uncertainty from sampling in pollution crime investigation: The importance of metrology in the forensic interpretation of environmental data.

    Science.gov (United States)

    Barazzetti Barbieri, Cristina; de Souza Sarkis, Jorge Eduardo

    2018-07-01

    The forensic interpretation of environmental analytical data is usually challenging due to the high geospatial variability of these data. The measurements' uncertainty includes contributions from the sampling and from the sample handling and preparation processes. These contributions are often disregarded in analytical techniques results' quality assurance. A pollution crime investigation case was used to carry out a methodology able to address these uncertainties in two different environmental compartments, freshwater sediments and landfill leachate. The methodology used to estimate the uncertainty was the duplicate method (that replicates predefined steps of the measurement procedure in order to assess its precision) and the parameters used to investigate the pollution were metals (Cr, Cu, Ni, and Zn) in the leachate, the suspect source, and in the sediment, the possible sink. The metal analysis results were compared to statutory limits and it was demonstrated that Cr and Ni concentrations in sediment samples exceeded the threshold levels at all sites downstream the pollution sources, considering the expanded uncertainty U of the measurements and a probability of contamination >0.975, at most sites. Cu and Zn concentrations were above the statutory limits at two sites, but the classification was inconclusive considering the uncertainties of the measurements. Metal analyses in leachate revealed that Cr concentrations were above the statutory limits with a probability of contamination >0.975 in all leachate ponds while the Cu, Ni and Zn probability of contamination was below 0.025. The results demonstrated that the estimation of the sampling uncertainty, which was the dominant component of the combined uncertainty, is required for a comprehensive interpretation of the environmental analyses results, particularly in forensic cases. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Radiochemistry methods in DOE methods for evaluating environmental and waste management samples

    International Nuclear Information System (INIS)

    Fadeff, S.K.; Goheen, S.C.

    1994-08-01

    Current standard sources of radiochemistry methods are often inappropriate for use in evaluating US Department of Energy environmental and waste management (DOE/EW) samples. Examples of current sources include EPA, ASTM, Standard Methods for the Examination of Water and Wastewater and HASL-300. Applicability of these methods is limited to specific matrices (usually water), radiation levels (usually environmental levels), and analytes (limited number). Radiochemistry methods in DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods) attempt to fill the applicability gap that exists between standard methods and those needed for DOE/EM activities. The Radiochemistry chapter in DOE Methods includes an ''analysis and reporting'' guidance section as well as radiochemistry methods. A basis for identifying the DOE/EM radiochemistry needs is discussed. Within this needs framework, the applicability of standard methods and targeted new methods is identified. Sources of new methods (consolidated methods from DOE laboratories and submissions from individuals) and the methods review process will be discussed. The processes involved in generating consolidated methods add editing individually submitted methods will be compared. DOE Methods is a living document and continues to expand by adding various kinds of methods. Radiochemistry methods are highlighted in this paper. DOE Methods is intended to be a resource for methods applicable to DOE/EM problems. Although it is intended to support DOE, the guidance and methods are not necessarily exclusive to DOE. The document is available at no cost through the Laboratory Management Division of DOE, Office of Technology Development

  12. Evaluation of NAA laboratory results in inter-comparison on determination of trace elements in food and environmental samples

    International Nuclear Information System (INIS)

    Diah Dwiana Lestiani; Syukria Kurniawati; Natalia Adventini

    2012-01-01

    Inter-comparison program is a good tool for improving quality and to enhance the accuracy and precision of the analytical techniques. By participating in this program, laboratories could demonstrate their capability and ensuring the quality of analysis results generated by analytical laboratories. The Neutron Activation Analysis (NAA) laboratory at National Nuclear Energy Agency of Indonesia (BATAN), Nuclear Technology Center for Materials and Radiometry-PTNBR laboratory participated in inter-comparison tests organized by NAA working group. Inter-comparison BATAN 2009 was the third inter-laboratory analysis test within that project. The participating laboratories were asked to analyze for trace elements using neutron activation analysis as the primary technique. Three materials were distributed to the participants representing foodstuff, and environmental material samples. Samples were irradiated in rabbit facility of G.A. Siwabessy reactor with neutron flux ~ 10 13 n.cm -2 .s -1 , and counted with HPGe detector of gamma spectrometry. Several trace elements in these samples were detected. The accuracy and precision evaluation based on International Atomic Energy Agency (IAEA) criteria was applied. In this paper the PTNBR NAA laboratory results is evaluated. (author)

  13. Aquatic concentrations of chemical analytes compared to ecotoxicity estimates

    Data.gov (United States)

    U.S. Environmental Protection Agency — We describe screening level estimates of potential aquatic toxicity posed by 227 chemical analytes that were measured in 25 ambient water samples collected as part...

  14. Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging

    Science.gov (United States)

    Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee

    2017-08-01

    Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed.

  15. Sample Preparation of Corn Seed Tissue to Prevent Analyte Relocations for Mass Spectrometry Imaging.

    Science.gov (United States)

    Kim, Shin Hye; Kim, Jeongkwon; Lee, Young Jin; Lee, Tae Geol; Yoon, Sohee

    2017-08-01

    Corn seed tissue sections were prepared by the tape support method using an adhesive tape, and mass spectrometry imaging (MSI) was performed. The effect of heat generated during sample preparation was investigated by time-of-flight secondary mass spectrometry (TOF-SIMS) imaging of corn seed tissue prepared by the tape support and the thaw-mounted methods. Unlike thaw-mounted sample preparation, the tape support method does not cause imaging distortion because of the absence of heat, which can cause migration of the analytes on the sample. By applying the tape-support method, the corn seed tissue was prepared without structural damage and MSI with accurate spatial information of analytes was successfully performed. Graphical Abstract ᅟ.

  16. Recent bibliography on analytical and sampling problems of a PWR primary coolant

    International Nuclear Information System (INIS)

    Illy, H.

    1980-07-01

    An extensive bibliography on the problems of analysis and sampling of the primary cooling water of PWRs is presented. The aim was to collect the analytical methods for dissolved gases. The sampling and preparation are also taken into account. last 8-10 years is included. The bibliography is arranged into alphabetical order by topics. The most important topics are as follows: boric acid, gas analysis, hydrogen isotopes, iodine, noble gases, radiation monitoring, sampling and preparation, water chemistry. (R.J.)

  17. MoonDB — A Data System for Analytical Data of Lunar Samples

    Science.gov (United States)

    Lehnert, K.; Ji, P.; Cai, M.; Evans, C.; Zeigler, R.

    2018-04-01

    MoonDB is a data system that makes analytical data from the Apollo lunar sample collection and lunar meteorites accessible by synthesizing published and unpublished datasets in a relational database with an online search interface.

  18. Gamma spectrometric analyses of environmental samples at PINSTECH

    International Nuclear Information System (INIS)

    Faruq, M.U.; Parveen, N.; Ahmed, B.; Aziz, A.

    1979-01-01

    Gamma spectrometric analyses of air and other environmental samples from PINSTECH were carried out. Air particulate samples were analyzed by a Ge(Li) detector on a computer-based multichannel analyzer. Other environmental samples were analyzed by a Na(T1) scintillation detector spectrometer and a multichannel analyzer with manual analysis. Concentration of radionuclides in the media was determined and the sources of their production were identified. Age of the fall out was estimated from the ratios of the fission products. (authors)

  19. Sampling quality assurance guidance in support of EM environmental sampling and analysis activities

    International Nuclear Information System (INIS)

    1994-05-01

    This document introduces quality assurance guidance pertaining to the design and implementation of sampling procedures and processes for collecting environmental data for DOE's Office of EM (Environmental Restoration and Waste Management)

  20. TECHNIQUES WITH POTENTIAL FOR HANDLING ENVIRONMENTAL SAMPLES IN CAPILLARY ELECTROPHORESIS

    Science.gov (United States)

    An assessment of the methods for handling environmental samples prior to capillary electrophoresis (CE) is presented for both aqueous and solid matrices. Sample handling in environmental analyses is the subject of ongoing research at the Environmental Protection Agency's National...

  1. Monitoring of emerging pollutants in Guadiamar River basin (South of Spain): analytical method, spatial distribution and environmental risk assessment.

    Science.gov (United States)

    Garrido, Eva; Camacho-Muñoz, Dolores; Martín, Julia; Santos, Antonio; Santos, Juan Luis; Aparicio, Irene; Alonso, Esteban

    2016-12-01

    Guadiamar River is located in the southwest of the Iberian Peninsula and connects two protected areas in the South of Spain: Sierra Morena and Doñana National Park. It is sited in an area affected by urban, industrial and agriculture sewage pollution and with tradition on intensive mining activities. Most of the studies performed in this area have been mainly focused on the presence of heavy metals and, until now, little is known about the occurrence of other contaminants such as emerging organic pollutants (EOPs). In this work, an analytical method has been optimized and validated for monitoring of forty-seven EOPs in surface water. The analytical method has been applied to study the distribution and environmental risk of these pollutants in Guadiamar River basin. The analytical method was based on solid-phase extraction and determination by liquid chromatography-triple quadrupole-tandem mass spectrometry. The 60 % of the target compounds were found in the analyzed samples. The highest concentrations were found for two plasticizers (bisphenol A and di(2-ethyhexyl)phthalate, mean concentration up to 930 ng/L) and two pharmaceutical compounds (caffeine (up to 623 ng/L) and salicylic acid (up to 318 ng/L)). This study allowed to evaluate the potential sources (industrial or urban) of the studied compounds and the spatial distribution of their concentrations along the river. Environmental risk assessment showed a major risk on the south of the river, mainly due to discharges of wastewater effluents.

  2. Functional analytic multisensory environmental therapy for people with dementia.

    Science.gov (United States)

    Staal, Jason A

    2012-01-01

    This paper introduces Functional Analytic Multisensory Environmental Therapy (FAMSET) for use with elders with dementia while using a multisensory environment/snoezelen room. The model introduces behavioral theory and practice to the multisensory environment treatment, addressing assessment, and, within session techniques, integrating behavioral interventions with emotion-oriented care. A modular approach is emphasized to delineate different treatment phases for multisensory environment therapy. The aim of the treatment is to provide a safe and effective framework for reducing the behavioral disturbance of the disease process, increasing elder well-being, and to promote transfer of positive effects to other environments outside of the multisensory treatment room.

  3. Analytical and sampling problems in primary coolant circuits of PWR-type reactors

    International Nuclear Information System (INIS)

    Illy, H.

    1980-10-01

    Details of recent analytical methods on the analysis and sampling of a PWR primary coolant are given in the order as follows: sampling and preparation; analysis of the gases dissolved in the water; monitoring of radiating substances; checking of boric acid concentration which controls the reactivity. The bibliography of this work and directions for its use are published in a separate report: KFKI-80-48 (1980). (author)

  4. Evaluation of polyethersulfone performance for the microextraction of polar chlorinated herbicides from environmental water samples.

    Science.gov (United States)

    Prieto, Ailette; Rodil, Rosario; Quintana, José Benito; Cela, Rafael; Möder, Monika; Rodríguez, Isaac

    2014-05-01

    In this work, the suitability of bulk polyethersulfone (PES) for sorptive microextraction of eight polar, chlorinated phenoxy acids and dicamba from environmental water samples is assessed and the analytical features of the optimized method are compared to those reported for other microextraction techniques. Under optimized conditions, extractions were performed with samples (18 mL) adjusted at pH 2 and containing a 30% (w/v) of sodium chloride, using a tubular PES sorbent (1 cm length × 0.7 mm o.d., sorbent volume 8 µL). Equilibrium conditions were achieved after 3h of direct sampling, with absolute extraction efficiencies ranging from 39 to 66%, depending on the compound. Analytes were recovered soaking the polymer with 0.1 mL of ethyl acetate, derivatized and determined by gas chromatography-mass spectrometry (GC-MS). Achieved quantification limits (LOQs) varied between 0.005 and 0.073 ng mL(-1). After normalization with the internal surrogate (IS), the efficiency of the extraction was only moderately affected by the particular characteristics of different water samples (surface and sewage water); thus, pseudo-external calibration, using spiked ultrapure water solutions, can be used as quantification technique. The reduced cost of the PES polymer allowed considering it as a disposable sorbent, avoiding variations in the performance of the extraction due to cross-contamination problems and/or surface modification with usage. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. Natural Radioactivity Pattern of Surabaya Water Environmental Samples

    International Nuclear Information System (INIS)

    Rosidi; Agus Taftazani

    2007-01-01

    The gross β radioactivity and natural radionuclide of Surabaya environmental samples pattern have been evaluated. The environmental samples were chosen randomly at 12 locations. The environment samples were water (fresh, estuary and coastal), sediment, eichhornia crassipes (Mart) Solms, Mangrove (Rhizophora stylosa), (Moolgarda delicatus) fish and (Johnius (Johnieops) borneensis) (Sharpnose hammer croaker) fish. The water sample was evaporated; the sediment sample was dried and ground; the biotic samples was burnt at the temperature 500 °C ; The gross β measurement using GM detector and the radionuclides has been identified by γ spectrometer. From the investigation results could be concluded that the natural radioactivity of environmental samples was very low. gross-β of water samples were lower than the threshold value of local government regulation of Surabaya no: 2 year 2004 (1 Bq/L). The distribution of gross-β activity of eichhornia crassipes (Mart) Solms was higher than the other biotic, water and sediment samples as well as the accumulation of radionuclides in the water organism was taken place. The result of identification using γ spectrometer has detected 7 of radionuclides, i.e 210 Pb, 212 Pb, 214 Pb, 208 Tl, 214 Bi, 228 Ac, and 40 K in all sample. The distribution factor of sediment F D was less than bioaccumulation factor of biotic F B and it indicates that there the radionuclide accumulation migration follows the pattern of water - sediment - biotic sample. (author)

  6. Hanford Site Environmental Surveillance Master Sampling Schedule for Calendar Year 2008

    Energy Technology Data Exchange (ETDEWEB)

    Bisping, Lynn E.

    2008-01-01

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by Pacific Northwest National Laboratory for the U.S. Department of Energy. Sampling is conducted to evaluate levels of radioactive and nonradioactive pollutants in the Hanford environs, as required in DOE Order 450.1, "Environmental Protection Program," and DOE Order 5400.5, "Radiation Protection of the Public and the Environment." The environmental surveillance sampling design is described in the "Hanford Site Environmental Monitoring Plan, United States Department of Energy, Richland Operations Office." This document contains the calendar year 2008 schedule for the routine collection of samples for the Surface Environmental Surveillance Project and Drinking Water Monitoring Project. Each section includes sampling locations, sampling frequencies, sample types, and analyses to be performed. In some cases, samples are scheduled on a rotating basis. If a sample will not be collected in 2008, the anticipated year for collection is provided. Maps showing approximate sampling locations are included for media scheduled for collection in 2008.

  7. An analytical examination of distortions in power spectra due to sampling errors

    International Nuclear Information System (INIS)

    Njau, E.C.

    1982-06-01

    Distortions introduced into spectral energy densities of sinusoid signals as well as those of more complex signals through different forms of errors in signal sampling are developed and shown analytically. The approach we have adopted in doing this involves, firstly, developing for each type of signal and for the corresponding form of sampling errors an analytical expression that gives the faulty digitization process involved in terms of the features of the particular signal. Secondly, we take advantage of a method described elsewhere [IC/82/44] to relate, as much as possible, the true spectral energy density of the signal and the corresponding spectral energy density of the faulty digitization process. Thirdly, we then develop expressions which reveal the distortions that are formed in the directly computed spectral energy density of the digitized signal. It is evident from the formulations developed herein that the types of sampling errors taken into consideration may create false peaks and other distortions that are of non-negligible concern in computed power spectra. (author)

  8. Making Decisions by Analytical Chemistry

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov

    . These discrepancies are very unfortunate because erroneous conclusions may arise from an otherwise meticulous and dedicated effort of research staff. This may eventually lead to unreliable conclusions thus jeopardizing investigations of environmental monitoring, climate changes, food safety, clinical chemistry......It has been long recognized that results of analytical chemistry are not flawless, owing to the fact that professional laboratories and research laboratories analysing the same type of samples by the same type of instruments are likely to obtain significantly different results. The European......, forensics and other fields of science where analytical chemistry is the key instrument of decision making. In order to elucidate the potential origin of the statistical variations found among laboratories, a major program was undertaken including several analytical technologies where the purpose...

  9. Sampling analytical tests and destructive tests for quality assurance

    International Nuclear Information System (INIS)

    Saas, A.; Pasquini, S.; Jouan, A.; Angelis, de; Hreen Taywood, H.; Odoj, R.

    1990-01-01

    In the context of the third programme of the European Communities on the monitoring of radioactive waste, various methods have been developed for the performance of sampling and measuring tests on encapsulated waste of low and medium level activity, on the one hand, and of high level activity, on the other hand. The purpose was to provide better quality assurance for products to be stored on an interim or long-term basis. Various testing sampling means are proposed such as: - sampling of raw waste before conditioning and determination of the representative aliquot, - sampling of encapsulated waste on process output, - sampling of core specimens subjected to measurement before and after cutting. Equipment suitable for these sampling procedures have been developed and, in the case of core samples, a comparison of techniques has been made. The results are described for the various analytical tests carried out on the samples such as: - mechanical tests, - radiation resistance, - fire resistance, - lixiviation, - determination of free water, - biodegradation, - water resistance, - chemical and radiochemical analysis. Every time it was possible, these tests were compared with non-destructive tests on full-scale packages and some correlations are given. This word has made if possible to improve and clarify sample optimization, with fine sampling techniques and methodologies and draw up characterization procedures. It also provided an occasion for a first collaboration between the laboratories responsible for these studies and which will be furthered in the scope of the 1990-1994 programme

  10. Determination of 129I/127I isotope ratios in liquid solutions and environmental soil samples by ICP-MS with hexapole collision cell

    OpenAIRE

    Izmer, A. V.; Boulyga, S. F.; Becker, J. S.

    2003-01-01

    The determination of I-129 in environmental samples at ultratrace levels is very difficult by ICP-MS due to a high noise caused by Xe impurities in argon plasma gas (interference of Xe-129(+)), possible (IH2+)-I-127 interference and an insufficient abundance ratio sensitivity of the ICP mass spectrometer for I-129/I-127 isotope ratio measurement. A sensitive, powerful and fast analytical technique for iodine isotope ratio measurements in aqueous solutions and contaminated soil samples directl...

  11. Determination of elemental concentrations in environmental plant samples by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Datta, J.; Chowdhury, D.P.; Verma, R.; Reddy, A.V.R.

    2012-01-01

    The intake of leafy vegetables in daily diet is very important to meet our nutritional needs. Vegetables provide the essential elements which are necessary and recommended for human growth. However, due to rapid industrialization and urbanization our environment becomes polluted and this affects the normal growth of agricultural products and composition of environmental species. The elemental concentrations present in the environmental samples are good indicators to assess the toxicological levels due to pollution affects. In the present work we have analysed several vegetable plant samples by instrumental neutron activation analysis to determine the elemental concentrations at major, minor and trace levels. The leafy vegetables like spinach, red leafy vegetable, pui, gourd leaf, lettuce and katoua were chosen as these are extensively consumed by local people in eastern part of India. We have determined 15 elements in the above mentioned vegetable samples and some of these are essential elements and some are toxic elements. It was found that Na and K were present as major elements, Fe and Zn as minor elements and As, Ce, Cr, Co, La, Mo, Rb, Sc, Sm, Sr as trace elements. The concentration level of Cr was found to be higher than that of recommended value certified by WHO and National environment quality control for human consumption. The validation of our analytical results have been performed by the Z-score tests through the determination of concentrations of the elements of interest in certified reference materials. (author)

  12. Removal of impurities from environmental water samples for tritium measurement by means of liquid scintillation counter

    International Nuclear Information System (INIS)

    Sakuma, Yoichi; Noda, Mitsuyasu

    2000-01-01

    Tritium concentration in environmental water samples is usually measured by means of liquid scintillation counting. Before the counting distillation operation is necessarily required to remove impurities, which have possibility of bad influence on the measurement, from the samples. But the operation usually takes long time and it is also troublesome. If you could simplify the purification process, you would be much easily able to measure it. Then, we have studied the probability of replacement the process by filtration aiming to simplify the procedure. We prepared several environmental water samples and also several water samples added quenching materials. These samples were purified by means of the distillation and the filtration and the impurities in them were examined. The purified samples were mixed with scintillation cocktail and the tritium concentration was measured. We added small amount of tritium in the same samples and investigated their scintillation spectra and their ESCR values in order to compare the two purification methods. Two kinds of filters were used for the filtration: 0.45 μm and 0.1 μm pore sized membrane filters. The liquid scintillation counter was LB-3 produced by Aloka Co. and Ltd. The scintillation cocktail was Ultima Gold LLT made by Packard Instrument Co and Ltd. The vial was Polyvial 145 LSD made by Zinsser Analytic Co. and Ltd. As the result, there was no significant difference between the two purification methods then the filtration method is feasible instead of the distillation. (author)

  13. Diagnostic herd sensitivity using environmental samples

    DEFF Research Database (Denmark)

    Vigre, Håkan; Josefsen, Mathilde Hartmann; Seyfarth, Anne Mette

    either at farm or slaughter. Three sample matrices were collected; dust samples (5 environmental swabs), nasal swabs (10 pools with 5 animals per pool) and air samples (1 filter). Based on the assumption that MRSA occurred in all 48 herds the overall herd sensitivity was 58% for nasal swabs, 33% for dust....... In our example, the prevalence of infected pigs in each herd was estimated from the pooled samples of nasal swabs. Logistic regression was used to estimate the effect of animal prevalence on the probability to detect MRSA in the dust and air samples at herd level. The results show a significant increase...

  14. Hanford analytical services quality assurance requirements documents. Volume 1: Administrative Requirements

    International Nuclear Information System (INIS)

    Hyatt, J.E.

    1997-01-01

    Hanford Analytical Services Quality Assurance Requirements Document (HASQARD) is issued by the Analytical Services, Program of the Waste Management Division, US Department of Energy (US DOE), Richland Operations Office (DOE-RL). The HASQARD establishes quality requirements in response to DOE Order 5700.6C (DOE 1991b). The HASQARD is designed to meet the needs of DOE-RL for maintaining a consistent level of quality for sampling and field and laboratory analytical services provided by contractor and commercial field and laboratory analytical operations. The HASQARD serves as the quality basis for all sampling and field/laboratory analytical services provided to DOE-RL through the Analytical Services Program of the Waste Management Division in support of Hanford Site environmental cleanup efforts. This includes work performed by contractor and commercial laboratories and covers radiological and nonradiological analyses. The HASQARD applies to field sampling, field analysis, and research and development activities that support work conducted under the Hanford Federal Facility Agreement and Consent Order Tri-Party Agreement and regulatory permit applications and applicable permit requirements described in subsections of this volume. The HASQARD applies to work done to support process chemistry analysis (e.g., ongoing site waste treatment and characterization operations) and research and development projects related to Hanford Site environmental cleanup activities. This ensures a uniform quality umbrella to analytical site activities predicated on the concepts contained in the HASQARD. Using HASQARD will ensure data of known quality and technical defensibility of the methods used to obtain that data. The HASQARD is made up of four volumes: Volume 1, Administrative Requirements; Volume 2, Sampling Technical Requirements; Volume 3, Field Analytical Technical Requirements; and Volume 4, Laboratory Technical Requirements. Volume 1 describes the administrative requirements

  15. Analytical Methods to Distinguish the Positive and Negative Spectra of Mineral and Environmental Elements Using Deep Ablation Laser-Induced Breakdown Spectroscopy (LIBS).

    Science.gov (United States)

    Kim, Dongyoung; Yang, Jun-Ho; Choi, Soojin; Yoh, Jack J

    2018-01-01

    Environments affect mineral surfaces, and the surface contamination or alteration can provide potential information to understanding their regional environments. However, when investigating mineral surfaces, mineral and environmental elements appear mixed in data. This makes it difficult to determine their atomic compositions independently. In this research, we developed four analytical methods to distinguish mineral and environmental elements into positive and negative spectra based on depth profiling data using laser-induced breakdown spectroscopy (LIBS). The principle of the methods is to utilize how intensity varied with depth for creating a new spectrum. The methods were applied to five mineral samples exposed to four environmental conditions including seawater, crude oil, sulfuric acid, and air as control. The proposed methods are then validated by applying the resultant spectra to principal component analysis and data were classified by the environmental conditions and atomic compositions of mineral. By applying the methods, the atomic information of minerals and environmental conditions were successfully inferred in the resultant spectrum.

  16. Analytical strategic environmental assessment (ANSEA) developing a new approach to SEA

    International Nuclear Information System (INIS)

    Dalkmann, Holger; Herrera, Rodrigo Jiliberto; Bongardt, Daniel

    2004-01-01

    The objective of analytical strategic environmental assessment (ANSEA) is to provide a decision-centred approach to the SEA process. The ANSEA project evolved from the realisation that, in many cases, SEA, as currently practised, is not able to ensure an appropriate integration of environmental values. The focus of SEA is on predicting impacts, but the tool takes no account of the decision-making processes it is trying to influence. At strategic decision-making levels, in turn, it is often difficult to predict impacts with the necessary exactitude. The decision-making sciences could teach some valuable lessons here. Instead of focusing on the quantitative prediction of environmental consequences, the ANSEA approach concentrates on the integration of environmental objectives into decision-making processes. Thus, the ANSEA approach provides a framework for analysing and assessing the decision-making processes of policies, plans and programmes (PPP). To enhance environmental integration into the decision-making process, decision windows (DW) can be identified. The approach is designed to be objective and transparent to ensure that environmental considerations are taken into account, or--from an ex-post perspective--to allow an evaluation of how far environmental considerations have been integrated into the decision-making process under assessment. The paper describes the concepts and the framework of the ANSEA approach and discusses its relation to SEA and the EC Directive

  17. Quality assurance guidance for laboratory assessment plates in support of EM environmental sampling and analysis activities

    International Nuclear Information System (INIS)

    1994-05-01

    This document is one of several guidance documents developed to support the EM (DOE Environmental Restoration and Waste Management) Analytical Services program. Its purpose is to introduce assessment plates that can be used to conduct performance assessments of an organization's or project's ability to meet quality goals for analytical laboratory activities. These assessment plates are provided as non-prescriptive guidance to EM-support organizations responsible for collection of environmental data for remediation and waste management programs at DOE facilities. The assessments evaluate objectively all components of the analytical laboratory process to determine their proper selection and use

  18. Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

    Directory of Open Access Journals (Sweden)

    Eloy Yordad Companioni Damas

    2009-01-01

    Full Text Available This work describes a validation of an analytical procedure for the analysis of petroleum hydrocarbons in marine sediment samples. The proposed protocol is able to measure n-alkanes and polycyclic aromatic hydrocarbons (PAH in samples at concentrations as low as 30 ng/g, with a precision better than 15% for most of analytes. The extraction efficiency of fortified sediments varied from 65.1 to 105.6% and 59.7 to 97.8%, for n-alkanes and PAH in the ranges: C16 - C32 and fluoranthene - benzo(apyrene, respectively. The analytical protocol was applied to determine petroleum hydrocarbons in sediments collected from a marine coastal zone.

  19. Detection of the actinides and cesium from environmental samples

    Science.gov (United States)

    Snow, Mathew Spencer

    Detection of the actinides and cesium in the environment is important for a variety of applications ranging from environmental remediation to safeguards and nuclear forensics. The utilization of multiple different elemental concentrations and isotopic ratios together can significantly improve the ability to attribute contamination to a unique source term and/or generation process; however, the utilization of multiple elemental "signatures" together from environmental samples requires knowledge of the impact of chemical fractionation for various elements under a variety of environmental conditions (including predominantly aqueous versus arid conditions). The research reported in this dissertation focuses on three major areas: 1. Improving the understanding of actinide-mineral interactions at ultra-low concentrations. Chapter 2 reports a batch sorption and modeling study of Np(V) sorption to the mineral goethite from attomolar to micromolar concentrations. 2. Improving the detection capabilities for Thermal Ionization Mass Spectrometry (TIMS) analyses of ultra-trace cesium from environmental samples. Chapter 4 reports a new method which significantly improves the chemical yields, purification, sample processing time, and ultimately, the detection limits for TIMS analyses of femtogram quantities of cesium from a variety of environmental sample matrices. 3. Demonstrating how actinide and cesium concentrations and isotopic ratios from environmental samples can be utilized together to determine a wealth of information including environmental transport mechanisms (e.g. aqueous versus arid transport) and information on the processes which generated the original material. Chapters1, 3 and 5 demonstrate these principles using Pu, Am, Np, and Cs concentrations and isotopic ratios from contaminated soils taken near the Subsurface Disposal Area (SDA) of Idaho National Laboratory (INL) (a low level radioactive waste disposal site in southeastern Idaho).

  20. Functional Analytic Multisensory Environmental Therapy for People with Dementia

    Directory of Open Access Journals (Sweden)

    Jason A. Staal

    2012-01-01

    Full Text Available This paper introduces Functional Analytic Multisensory Environmental Therapy (FAMSET for use with elders with dementia while using a multisensory environment/snoezelen room. The model introduces behavioral theory and practice to the multisensory environment treatment, addressing assessment, and, within session techniques, integrating behavioral interventions with emotion-oriented care. A modular approach is emphasized to delineate different treatment phases for multisensory environment therapy. The aim of the treatment is to provide a safe and effective framework for reducing the behavioral disturbance of the disease process, increasing elder well-being, and to promote transfer of positive effects to other environments outside of the multisensory treatment room.

  1. Computerized Analytical Data Management System and Automated Analytical Sample Transfer System at the COGEMA Reprocessing Plants in La Hague

    International Nuclear Information System (INIS)

    Flament, T.; Goasmat, F.; Poilane, F.

    2002-01-01

    Managing the operation of large commercial spent nuclear fuel reprocessing plants, such as UP3 and UP2-800 in La Hague, France, requires an extensive analytical program and the shortest possible analysis response times. COGEMA, together with its engineering subsidiary SGN, decided to build high-performance laboratories to support operations in its plants. These laboratories feature automated equipment, safe environments for operators, and short response times, all in centralized installations. Implementation of a computerized analytical data management system and a fully automated pneumatic system for the transfer of radioactive samples was a key factor contributing to the successful operation of the laboratories and plants

  2. Near-facility environmental monitoring

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, J.W.; Johnson, A.R.; Markes, B.M.; McKinney, S.M.; Perkins, C.J.

    1995-06-01

    This section of the 1994 Hanford Site Environmental Report summarizes the routine near-facility environmental monitoring programs which are presently being conducted at the Hanford Site. Several types of environmental media are sampled near nuclear facilities to monitor the effectiveness of waste management and restoration activities, and effluent treatment and control practices. These media include air, surface water and springs, surface contamination, soil and vegetation, investigative sampling (which can include wildlife), and external radiation. Sampling and analysis information and analytical results for 1994 for each of these media are summarized in this section. Additional data and more detailed information may be found in Westinghouse Hanford Company Operational Environmental Monitoring Annual Report, Calendar Year 1994.

  3. Environmental report for 1991

    International Nuclear Information System (INIS)

    Hunter, S.; Wilt, G.; Balke, B.K.; Surano, K.A.; Hoppes, W.G.; Tate, P.J.; Steenhoven, J.C.; Fields, B.C.; Garcia, L.M.; Lamson, K.C.

    1991-01-01

    As part of its commitment to environmental compliance and accountability, LLNL prepares this report each year to communicate the results of monitoring and compliance activities. Analytical data are produced from sampling of air, sewage effluent, groundwater, surface water, soil, vegetation and foodstuff, and through measurement of environmental radiation. The Environmental Protection Department performed more than 150,000 analyses of environmental samples during 1991. This Executive Summary provides a comprehensive synopsis, organized along the general outline of the report, and furnishes an overview of the supporting methodologies, data, and findings that are presented in the chapters that follow

  4. Analytical chemistry instrumentation

    International Nuclear Information System (INIS)

    Laing, W.R.

    1986-01-01

    In nine sections, 48 chapters cover 1) analytical chemistry and the environment 2) environmental radiochemistry 3) automated instrumentation 4) advances in analytical mass spectrometry 5) fourier transform spectroscopy 6) analytical chemistry of plutonium 7) nuclear analytical chemistry 8) chemometrics and 9) nuclear fuel technology

  5. Automated Sample Preparation for Radiogenic and Non-Traditional Metal Isotopes: Removing an Analytical Barrier for High Sample Throughput

    Science.gov (United States)

    Field, M. Paul; Romaniello, Stephen; Gordon, Gwyneth W.; Anbar, Ariel D.; Herrmann, Achim; Martinez-Boti, Miguel A.; Anagnostou, Eleni; Foster, Gavin L.

    2014-05-01

    MC-ICP-MS has dramatically improved the analytical throughput for high-precision radiogenic and non-traditional isotope ratio measurements, compared to TIMS. The generation of large data sets, however, remains hampered by tedious manual drip chromatography required for sample purification. A new, automated chromatography system reduces the laboratory bottle neck and expands the utility of high-precision isotope analyses in applications where large data sets are required: geochemistry, forensic anthropology, nuclear forensics, medical research and food authentication. We have developed protocols to automate ion exchange purification for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U) using the new prepFAST-MC™ (ESI, Nebraska, Omaha). The system is not only inert (all-flouropolymer flow paths), but is also very flexible and can easily facilitate different resins, samples, and reagent types. When programmed, precise and accurate user defined volumes and flow rates are implemented to automatically load samples, wash the column, condition the column and elute fractions. Unattended, the automated, low-pressure ion exchange chromatography system can process up to 60 samples overnight. Excellent reproducibility, reliability, recovery, with low blank and carry over for samples in a variety of different matrices, have been demonstrated to give accurate and precise isotopic ratios within analytical error for several isotopic systems (B, Ca, Fe, Cu, Zn, Sr, Cd, Pb and U). This illustrates the potential of the new prepFAST-MC™ (ESI, Nebraska, Omaha) as a powerful tool in radiogenic and non-traditional isotope research.

  6. Sample diagnosis using indicator elements and non-analyte signals for inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Antler, Margaret; Ying Hai; Burns, David H.; Salin, Eric D.

    2003-01-01

    A sample diagnosis procedure that uses both non-analyte and analyte signals to estimate matrix effects in inductively coupled plasma-mass spectrometry is presented. Non-analyte signals are those of background species in the plasma (e.g. N + , ArO + ), and changes in these signals can indicate changes in plasma conditions. Matrix effects of Al, Ba, Cs, K and Na on 19 non-analyte signals and 15 element signals were monitored. Multiple linear regression was used to build the prediction models, using a genetic algorithm for objective feature selection. Non-analyte elemental signals and non-analyte signals were compared for diagnosing matrix effects, and both were found to be suitable for estimating matrix effects. Individual analyte matrix effect estimation was compared with the overall matrix effect prediction, and models used to diagnose overall matrix effects were more accurate than individual analyte models. In previous work [Spectrochim. Acta Part B 57 (2002) 277], we tested models for analytical decision making. The current models were tested in the same way, and were able to successfully diagnose matrix effects with at least an 80% success rate

  7. Analytical artefacts in the speciation of arsenic in clinical samples

    International Nuclear Information System (INIS)

    Slejkovec, Zdenka; Falnoga, Ingrid; Goessler, Walter; Elteren, Johannes T. van; Raml, Reingard; Podgornik, Helena; Cernelc, Peter

    2008-01-01

    Urine and blood samples of cancer patients, treated with high doses of arsenic trioxide were analysed for arsenic species using HPLC-HGAFS and, in some cases, HPLC-ICPMS. Total arsenic was determined with either flow injection-HGAFS in urine or radiochemical neutron activation analysis in blood fractions (in serum/plasma, blood cells). The total arsenic concentrations (during prolonged, daily/weekly arsenic trioxide therapy) were in the μg mL -1 range for urine and in the ng g -1 range for blood fractions. The main arsenic species found in urine were As(III), MA and DMA and in blood As(V), MA and DMA. With proper sample preparation and storage of urine (no preservation agents/storage in liquid nitrogen) no analytical artefacts were observed and absence of significant amounts of alleged trivalent metabolites was proven. On the contrary, in blood samples a certain amount of arsenic can get lost in the speciation procedure what was especially noticeable for the blood cells although also plasma/serum gave rise to some disappearance of arsenic. The latter losses may be attributed to precipitation of As(III)-containing proteins/peptides during the methanol/water extraction procedure whereas the former losses were due to loss of specific As(III)-complexing proteins/peptides (e.g. cysteine, metallothionein, reduced GSH, ferritin) on the column (Hamilton PRP-X100) during the separation procedure. Contemporary analytical protocols are not able to completely avoid artefacts due to losses from the sampling to the detection stage so that it is recommended to be careful with the explanation of results, particularly regarding metabolic and pharmacokinetic interpretations, and always aim to compare the sum of species with the total arsenic concentration determined independently

  8. Determination of short half-life elements in biological, foodstuff, and environmental samples qualitatively by neutron activation analysis

    International Nuclear Information System (INIS)

    Syukria Kurniawati; Muhayatun Santoso; Diah Dwiana Lestiani

    2010-01-01

    NAA applications at routine operation power of 15 MW at Multipurpose Reactor GA Siwabessy (MPR-GAS) for sample matrices analysis have been widely applied. However, the results are not optimum for some matrices especially for short half-live elements. Preliminary study of short half-life elements determination in biological, foodstuff, and environmental samples using 1 MW power have been conducted to solve this problem. The samples were irradiated in rabbit system of MPR-GAS for 5 minutes, counted for 200 seconds by HPGe detector, and the spectrum were analyzed further using software Genie 2000 and Bandung NAA Utility. Analysis under 1 MW power on biological and foodstuff samples were capable to detect eight elements: Al, Br, CI, Ca, I, K, Mg, Ti, and Na for biological samples; Al, Br, CI, Ca, I, K, Mg, Mn, and Na for foodstuff samples, while at 15 MW power only three elements (CI, K, Na) were detected. At 1 MW power the counting process is more optimum due to smaller radiation exposure and dead time. For the environmental samples, the number of elements detected by 1 MW and 15 MW powers did not differ significantly. Generally, the results on the three types of samples showed that the elements of short half-life are better detected at 1 MW than that of 15 MW power. Further research needs to be done to obtain the optimum analytical conditions for irradiation and counting time determination. (author)

  9. Arsenic speciation in environmental samples by hydride generation and electrothermal atomic absorption spectrometry.

    Science.gov (United States)

    Anawar, Hossain Md

    2012-01-15

    For the past few years many studies have been performed to determine arsenic (As) speciation in drinking water, food chain and other environmental samples due to its well-recognized carcinogenic and toxic effects relating to its chemical forms and oxidation states. This review provides an overview of analytical methods, preconcentration and separation techniques, developed up to now, using HGAAS and ETAAS for the determination of inorganic As and organoarsenic species in environmental samples. Specific advantages, disadvantages, selectivity, sensitivity, efficiency, rapidity, detection limit (DL), and some aspects of recent improvements and modifications for different analytical and separation techniques, that can define their application for a particular sample analysis, are highlighted. HG-AAS has high sensitivity, selectivity and low DL using suitable separation techniques; and it is a more suitable, affordable and much less expensive technique than other detectors. The concentrations of HCl and NaBH(4) have a critical effect on the HG response of As species. Use of l-cysteine as pre-reductant is advantageous over KI to obtain the same signal response for different As species under the same, optimum and mild acid concentration, and to reduce the interference of transition metals on the arsine generation. Use of different pretreatment, digestion, separation techniques and surfactants can determine As species with DL from ngL(-1) to μgL(-1). Out of all the chromatographic techniques coupled with HGAAS/ETAAS, ion-pair reversed-phase chromatography (IP-RP) is the most popular due to its higher separation efficiency, resolution selectivity, simplicity, and ability to separate up to seven As species for both non-ionic and ionic compounds in a signal run using the same column and short time. However, a combination of anion- and cation-exchange chromatography seems the most promising for complete resolution up to eight As species. The ETAAS method using different

  10. Paper Capillary Enables Effective Sampling for Microfluidic Paper Analytical Devices.

    Science.gov (United States)

    Shangguan, Jin-Wen; Liu, Yu; Wang, Sha; Hou, Yun-Xuan; Xu, Bi-Yi; Xu, Jing-Juan; Chen, Hong-Yuan

    2018-06-06

    Paper capillary is introduced to enable effective sampling on microfluidic paper analytical devices. By coupling mac-roscale capillary force of paper capillary and microscale capillary forces of native paper, fluid transport can be flexibly tailored with proper design. Subsequently, a hybrid-fluid-mode paper capillary device was proposed, which enables fast and reliable sampling in an arrayed form, with less surface adsorption and bias for different components. The resulting device thus well supports high throughput, quantitative, and repeatable assays all by hands operation. With all these merits, multiplex analysis of ions, proteins, and microbe have all been realized on this platform, which has paved the way to level-up analysis on μPADs.

  11. Determination of radium-226 in environmental samples

    International Nuclear Information System (INIS)

    Powers, R.P.; Turnage, N.E.; Kanipe, L.G.

    1980-01-01

    The analysis of soil and water samples for 226 Ra by gamma spectrometry with a Ge(Li) detector was compared with that by radiochemical separation followed by 222 Rn de-emanation. Lower limits of detection (LLD) for 226 Ra were calculated for the two analytical techniques. The Ge(Li) system was found to have an LLD for soil comparable to that calculated for the de-emanation procedure, but the Ge(Li) system was found to have a significantly higher LLD for water samples. Cost analysis indicated that the cost of 222 Ra determination with a Ge(Li) system can be less than with the de-emanation procedure if the Ge(Li) system can perform at least one other isotopic anaysis per sample

  12. Applied research on environmental pollution using INAA. A study on the environmental indicator analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Nak Bae; Lee, Gil Yong; Yoon, Yoon Yul; Chon, Sang Ki [Korea Institute of Geology Mining and Research, Taejon (Korea, Republic of)

    1995-08-01

    Among the many kinds of environmental indicator samples such as moss, lichen, pine needle, pine needle was selected as a bio-monitor and collected sample was divided two groups and one was washed with 1% hydrochloric acid to remove the elements deposited on surface. Trace elements in pine needle were analyzed by the decay time of each nuclide. Analytical accuracy was tested by analyzing NIST SRM 1575 pine needle. Results are follows: (1) Environmental indicator as a bio-monitor pine needle was selected. (2) The content difference of the trace elements between sampling period was monitored. And as content was varied with sampling time. (3) To monitor the influence of atmospheric deposition the surface of pine needle was washed with 1% hydrochloric acid. Therefore, As, Ce, La, Na, W, and Zn contents were decreased by washing. (4) Non-destructive INAA (Instrumental Neutron Activation Analysis) technique was developed for the determination of trace elements in environmental samples. (5) Analytical accuracy was tested by analyzing NIST SRM 1575 pine needle, and the accuracy was well agreed within 10% deviation. summarized. (author). 18 refs., 8 figs., 5 tabs.

  13. Development of a low-cost method of analysis for the qualitative and quantitative analysis of butyltins in environmental samples.

    Science.gov (United States)

    Bangkedphol, Sornnarin; Keenan, Helen E; Davidson, Christine; Sakultantimetha, Arthit; Songsasen, Apisit

    2008-12-01

    Most analytical methods for butyltins are based on high resolution techniques with complicated sample preparation. For this study, a simple application of an analytical method was developed using High Performance Liquid Chromatography (HPLC) with UV detection. The developed method was studied to determine tributyltin (TBT), dibutyltin (DBT) and monobutyltin (MBT) in sediment and water samples. The separation was performed in isocratic mode on an ultra cyanopropyl column with a mobile phase of hexane containing 5% THF and 0.03% acetic acid. This method was confirmed using standard GC/MS techniques and verified by statistical paired t-test method. Under the experimental conditions used, the limit of detection (LOD) of TBT and DBT were 0.70 and 0.50 microg/mL, respectively. The optimised extraction method for butyltins in water and sediment samples involved using hexane containing 0.05-0.5% tropolone and 0.2% sodium chloride in water at pH 1.7. The quantitative extraction of butyltin compounds in a certified reference material (BCR-646) and naturally contaminated samples was achieved with recoveries ranging from 95 to 108% and at %RSD 0.02-1.00%. This HPLC method and optimum extraction conditions were used to determine the contamination level of butyltins in environmental samples collected from the Forth and Clyde canal, Scotland, UK. The values obtained severely exceeded the Environmental Quality Standard (EQS) values. Although high resolution methods are utilised extensively for this type of research, the developed method is cheaper in both terms of equipment and running costs, faster in analysis time and has comparable detection limits to the alternative methods. This is advantageous not just as a confirmatory technique but also to enable further research in this field.

  14. Dynamic Headspace Sampling as an Initial Step for Sample Preparation in Chromatographic Analysis.

    Science.gov (United States)

    Wojnowski, Wojciech; Majchrzak, Tomasz; Dymerski, Tomasz; Gębicki, Jacek; Namieśnik, Jacek

    2017-11-01

    This work represents a brief summary of the use of dynamic headspace (DHS) as a technique for sample preparation in chromatographic analysis. Despite numerous developments in the area of analyte isolation and enrichment, DHS remains one of the fundamental methods used with GC. In our opinion, interest in this technique will not diminish significantly because it conforms to stipulations of green analytical chemistry. Moreover, DHS fulfills the need for methods that facilitate detection and determination of analytes present at ultratrace levels in complex matrixes. The main focus of this work was placed on the theoretical fundamentals of this method. Also described herein were DHS development, the advantages and disadvantages of this technique compared with other headspace sampling techniques, and selected examples of its applications in food and environmental analyses.

  15. Analysis of polychlorinated n-alkanes in environmental samples.

    Science.gov (United States)

    Santos, F J; Parera, J; Galceran, M T

    2006-10-01

    Polychlorinated n-alkanes (PCAs), also known as chlorinated paraffins (CPs), are highly complex technical mixtures that contain a huge number of structural isomers, theoretically more than 10,000 diastereomers and enantiomers. As a consequence of their persistence, tendency to bioaccumulation, and widespread and unrestricted use, PCAs have been found in aquatic and terrestrial food webs, even in rural and remote areas. Recently, these compounds have been included in regulatory programs of several international organizations, including the US Environmental Protection Agency and the European Union. Consequently, there is a growing demand for reliable methods with which to analyze PCAs in environmental samples. Here, we review current trends and recent developments in the analysis of PCAs in environmental samples such as air, water, sediment, and biota. Practical aspects of sample preparation, chromatographic separation, and detection are covered, with special emphasis placed on analysis of PCAs using gas chromatography-mass spectrometry. The advantages and limitations of these techniques as well as recent improvements in quantification procedures are discussed.

  16. Time and temperature dependent analytical stability of dry-collected Evalyn HPV self-sampling brush for cervical cancer screening

    DEFF Research Database (Denmark)

    Ejegod, Ditte Møller; Pedersen, Helle; Alzua, Garazi Peña

    2018-01-01

    As a new initiative, HPV self-sampling to non-attenders using the dry Evalyn self-sampling brush is offered in the Capital Region of Denmark. The use of a dry brush is largely uncharted territory in terms of analytical stability. In this study we aim to provide evidence on the analytical quality...

  17. Environmental report 1992

    Energy Technology Data Exchange (ETDEWEB)

    Wilt, G.C. [ed.; Gallegos, G.M.; Wander, S.M. [and others

    1992-12-31

    Lawrence Livermore National Laboratory (LLNL), a US Department of Energy facility operated by the University of California, serves as a national resource of scientific, technical, and engineering capability with a special focus on national security. During 1992, the Environmental Protection Department conducted sampling of air, sewage effluent, ground water, surface water, soil, vegetation and foodstuffs, and took measurements of environmental radiation. It performed more than 150,000 analyses of environmental samples. The analytical results are summarized in the chapters that follow, along with evaluations of the impact of radioactive and nonradioactive materials, a discussion of the effects of LLNL operations on the environment, and a summary of the activities undertaken to comply with local, state, and federal environmental laws.

  18. Environmental report 1992

    International Nuclear Information System (INIS)

    Wilt, G.C.; Gallegos, G.M.; Wander, S.M.

    1992-01-01

    Lawrence Livermore National Laboratory (LLNL), a US Department of Energy facility operated by the University of California, serves as a national resource of scientific, technical, and engineering capability with a special focus on national security. During 1992, the Environmental Protection Department conducted sampling of air, sewage effluent, ground water, surface water, soil, vegetation and foodstuffs, and took measurements of environmental radiation. It performed more than 150,000 analyses of environmental samples. The analytical results are summarized in the chapters that follow, along with evaluations of the impact of radioactive and nonradioactive materials, a discussion of the effects of LLNL operations on the environment, and a summary of the activities undertaken to comply with local, state, and federal environmental laws

  19. Determination of 228Th, 230Th, and 232Th in environmental samples from uranium mining and milling operations

    International Nuclear Information System (INIS)

    Durham, R.W.; Joshi, S.R.

    1979-01-01

    A method is described for the determination of 228 Th, 230 Th, and 232 Th in environmental samples from uranium mining and milling operations. The analytical procedure is based on the direct determination of 228 Th in the sample by high resolution γ-spectrometry followed by extraction and purification of the thorium fraction using high molecular weight amines and an anion-exchange technique, respectively, prior to α-spectrometry to determine isotopic ratios. The lowest level of detection for each thorium isotope is 0.01 pCi/g for solid samples and 20 pCi/l for aqueous samples. Replicate analyses of a typical mine waste stream gave a standard deviation of +-3% for 228 Th. Standard deviations of the 230 Th and 232 Th increased to +-11% apparently due to traces of 210 Po interfering in the α-spectrometry. (author)

  20. Trends in analytical methodologies for the determination of alkylphenols and bisphenol A in water samples.

    Science.gov (United States)

    Salgueiro-González, N; Muniategui-Lorenzo, S; López-Mahía, P; Prada-Rodríguez, D

    2017-04-15

    In the last decade, the impact of alkylphenols and bisphenol A in the aquatic environment has been widely evaluated because of their high use in industrial and household applications as well as their toxicological effects. These compounds are well-known endocrine disrupting compounds (EDCs) which can affect the hormonal system of humans and wildlife, even at low concentrations. Due to the fact that these pollutants enter into the environment through waters, and it is the most affected compartment, analytical methods which allow the determination of these compounds in aqueous samples at low levels are mandatory. In this review, an overview of the most significant advances in the analytical methodologies for the determination of alkylphenols and bisphenol A in waters is considered (from 2002 to the present). Sample handling and instrumental detection strategies are critically discussed, including analytical parameters related to quality assurance and quality control (QA/QC). Special attention is paid to miniaturized sample preparation methodologies and approaches proposed to reduce time- and reagents consumption according to Green Chemistry principles, which have increased in the last five years. Finally, relevant applications of these methods to the analysis of water samples are examined, being wastewater and surface water the most investigated. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. DEP-On-Go for Simultaneous Sensing of Multiple Heavy Metals Pollutants in Environmental Samples

    Directory of Open Access Journals (Sweden)

    Madhu Biyani

    2016-12-01

    Full Text Available We describe a simple and affordable “Disposable electrode printed (DEP-On-Go” sensing platform for the rapid on-site monitoring of trace heavy metal pollutants in environmental samples for early warning by developing a mobile electrochemical device composed of palm-sized potentiostat and disposable unmodified screen-printed electrode chips. We present the analytical performance of our device for the sensitive detection of major heavy metal ions, namely, mercury, cadmium, lead, arsenic, zinc, and copper with detection limits of 1.5, 2.6, 4.0, 5.0, 14.4, and, 15.5 μg·L−1, respectively. Importantly, the utility of this device is extended to detect multiple heavy metals simultaneously with well-defined voltammograms and similar sensitivity. Finally, “DEP-On-Go” was successfully applied to detect heavy metals in real environmental samples from groundwater, tap water, house dust, soil, and industry-processed rice and noodle foods. We evaluated the efficiency of this system with a linear correlation through inductively coupled plasma mass spectrometry, and the results suggested that this system can be reliable for on-site screening purposes. On-field applications using real samples of groundwater for drinking in the northern parts of India support the easy-to-detect, low-cost (<1 USD, rapid (within 5 min, and reliable detection limit (ppb levels performance of our device for the on-site detection and monitoring of multiple heavy metals in resource-limited settings.

  2. Simple Sensitive Spectrophotometric Determination of Vanadium in Biological and Environmental Samples

    Directory of Open Access Journals (Sweden)

    B. Krishna Priya

    2006-01-01

    Full Text Available Novel, rapid, highly sensitive and selective spectrophotometric method for the determination of traces of vanadium (V in environmental and biological samples, pharmaceutical and steel samples was studied. The method is based on oxidation of 2,4- dinitro phenyl hydrazine(2,4-DNPH by vanadium (V followed by coupling reaction with N-(1-naphthalene-1-ylethane-1,2-diamine-dihydrochloride (NEDA in acidic medium to give red colored derivative or on oxidation of 4-Amino Pyridine by vanadium (V followed by coupling reaction with NEDA in basic medium to give pink colored derivative. The red colored derivative having an λmax 495 nm which is stable for 8 days and the pink colored derivative with 525 nm is stable for more than 7 days at 350C. Beer's law is obeyed for vanadium (V in the concentration range of 0.02 - 3.5 μg mL–1 (red derivative and 0.03 – 4.5 μg mL–1 (pink derivative at the wave length of maximum absorption. The optimum reaction conditions and other analytical parameters were investigated to enhance the sensitivity of the present method. The detailed study of various interferences made the method more selective. The proposed method was successfully applied to the analysis of vanadium in natural water samples, plant material, soil samples, synthetic mixtures, pharmaceutical samples and biological samples. The results obtained were agreed with the reported methods at the 95 % confidence level. The performance of proposed method was evaluated in terms of Student's t-test and Variance ratio f-test which indicates the significance of proposed method over reported method.

  3. Analytical methods for the determination of mixtures of bisphenols and derivatives in human and environmental exposure sources and biological fluids. A review

    International Nuclear Information System (INIS)

    Caballero-Casero, N.; Lunar, L.; Rubio, S.

    2016-01-01

    Bisphenol A (BPA) is ubiquitous in humans and the environment. Its potential adverse effects through genomic and non-genomic pathways have fostered BPA replacement by bisphenol analogs that, unfortunately, exert similar adverse effects. Many of these analogs, as well as their derivatives, have already found in humans and the environment and major concerns have arisen over their low dose- and mixture-related effects. This review aims to discuss the characteristics of the main analytical methods reported so far for the determination of mixtures of bisphenol analogs and/or derivatives in human and environmental exposure sources and biological fluids. Approaches followed for removal of background contamination, sample preparation and separation and detection of mixtures of bisphenols and derivatives are critically discussed. Sample treatment is matrix-dependent and common steps include analyte isolation, removal of interferences, evaporation of the extracts and solvent reconstitution. Separation and quantification has been almost exclusively carried out by liquid chromatography tandem mass spectrometry (LC-MS/MS) or gas chromatography mass spectrometry (GC–MS), in the last case prior derivatization, but LC-fluorescence detection has also found some applications. Main characteristics, advantages and drawbacks of these methods will be comparatively discussed. Although at an early stage, some approaches for the assessment of the risk to mixtures of bisphenols, mainly based on the combination of chemical target analysis and toxicity evaluation, have been already applied and they will be here presented. Current knowledge gaps hindering a reliable assessment of human and environmental risk to mixtures of bisphenols and derivatives will be outlined. - Highlights: • Analytical methods for the (bio)monitoring of mixtures of bisphenols are reviewed. • LC and CG coupled to MS are the preferred techniques. • Method-dependent sample treatments are required to remove matrix

  4. Analytical methods for the determination of mixtures of bisphenols and derivatives in human and environmental exposure sources and biological fluids. A review

    Energy Technology Data Exchange (ETDEWEB)

    Caballero-Casero, N.; Lunar, L.; Rubio, S., E-mail: qa1rubrs@uco.es

    2016-02-18

    Bisphenol A (BPA) is ubiquitous in humans and the environment. Its potential adverse effects through genomic and non-genomic pathways have fostered BPA replacement by bisphenol analogs that, unfortunately, exert similar adverse effects. Many of these analogs, as well as their derivatives, have already found in humans and the environment and major concerns have arisen over their low dose- and mixture-related effects. This review aims to discuss the characteristics of the main analytical methods reported so far for the determination of mixtures of bisphenol analogs and/or derivatives in human and environmental exposure sources and biological fluids. Approaches followed for removal of background contamination, sample preparation and separation and detection of mixtures of bisphenols and derivatives are critically discussed. Sample treatment is matrix-dependent and common steps include analyte isolation, removal of interferences, evaporation of the extracts and solvent reconstitution. Separation and quantification has been almost exclusively carried out by liquid chromatography tandem mass spectrometry (LC-MS/MS) or gas chromatography mass spectrometry (GC–MS), in the last case prior derivatization, but LC-fluorescence detection has also found some applications. Main characteristics, advantages and drawbacks of these methods will be comparatively discussed. Although at an early stage, some approaches for the assessment of the risk to mixtures of bisphenols, mainly based on the combination of chemical target analysis and toxicity evaluation, have been already applied and they will be here presented. Current knowledge gaps hindering a reliable assessment of human and environmental risk to mixtures of bisphenols and derivatives will be outlined. - Highlights: • Analytical methods for the (bio)monitoring of mixtures of bisphenols are reviewed. • LC and CG coupled to MS are the preferred techniques. • Method-dependent sample treatments are required to remove matrix

  5. Onondaga Lake: A Forsaken Superfund Site, or a Sampling Playground for Environmental Geochemistry Classes?

    Science.gov (United States)

    Karmosky, C. C.; Harpp, K. S.

    2004-05-01

    Onondaga Lake, in Syracuse, NY, is described by the EPA as one of the most polluted lakes in the US. High levels of heavy metal and semi-volatile organic contamination provide an excellent case study that serves as the cornerstone for an environmental geochemistry course at Colgate University. Our course is designed to teach students basic environmental analysis skills including experimental design, sample preparation, analytical instrumentation operation, data processing and statistical analysis, and preparation of a collaborative scientific paper. Participating students generally have some background in environmental geology, but rarely more than one semester of chemistry. The Onondaga Lake project is the focus of the course for approximately half the semester. At the outset of the project, students are presented with a driving question that is answered through a series of guided field and lab investigations, such as an assessment of the environmental consequences of a proposed marina along the lakefront. The students' first task is to delve into the lake's environmental history, including identification of contaminants, location of point and non-point pollution sources, and clean-up efforts. Students then participate in 2 field trips to the site. First, students learn the geography of the lake system, collect sediment and water samples, and observe mitigation efforts at the wastewater treatment plant. The second trip is 2-3 weeks later, after students have assessed further sampling needs. Identification and quantification of organic compounds are accomplished by GC-MS, and heavy metal contents are determined by ICP-MS. Students compile their results, perform statistical analyses, and collaboratively draw their conclusions regarding the impact of the proposed project. The final product is a single report written by the entire class, an exercise in organization, cooperation, and planning that is usually the most challenging, but ultimately the most rewarding

  6. Negative dielectrophoresis spectroscopy for rare analyte quantification in biological samples

    Science.gov (United States)

    Kirmani, Syed Abdul Mannan; Gudagunti, Fleming Dackson; Velmanickam, Logeeshan; Nawarathna, Dharmakeerthi; Lima, Ivan T., Jr.

    2017-03-01

    We propose the use of negative dielectrophoresis (DEP) spectroscopy as a technique to improve the detection limit of rare analytes in biological samples. We observe a significant dependence of the negative DEP force on functionalized polystyrene beads at the edges of interdigitated electrodes with respect to the frequency of the electric field. We measured this velocity of repulsion for 0% and 0.8% conjugation of avidin with biotin functionalized polystyrene beads with our automated software through real-time image processing that monitors the Rayleigh scattering from the beads. A significant difference in the velocity of the beads was observed in the presence of as little as 80 molecules of avidin per biotin functionalized bead. This technology can be applied in the detection and quantification of rare analytes that can be useful in the diagnosis and the treatment of diseases, such as cancer and myocardial infarction, with the use of polystyrene beads functionalized with antibodies for the target biomarkers.

  7. A new colorimetric chemosensors for Cu{sup 2+} and Cd{sup 2+} ions detection: Application in environmental water samples and analytical method validation

    Energy Technology Data Exchange (ETDEWEB)

    Tekuri, Venkatadri; Trivedi, Darshak R., E-mail: darshak_rtrivedi@yahoo.co.in

    2017-06-15

    A new heterocyclic thiophene-2-caboxylic acid hydrazide based chemosensor R1 to R4 were designed, synthesized and characterized by various spectroscopic techniques like FT-IR, UV-Vis, {sup 1}H NMR, {sup 13}C NMR, Mass and SC-XRD. The chemosensor R3 showed a significant color change from colorless to yellow in the presence of Cu{sup 2+} ions and chemosensor R4 showed a significant color change from colorless to yellow in the presence of Cd{sup 2+} ions over the other tested cations such as Cr{sup 3+}, Mn{sup 2+}, Fe{sup 2+}, Fe{sup 3+}, Co{sup 2+}, Ni{sup 2+}, Zn{sup 2+}, Ag{sup 2+}, Al{sup 3+}, Pb{sup 2+}, Hg{sup 2+}, K{sup +}, Ca{sup 2+} and Mg{sup 2+}. The high selective and sensitivity of R3 towards Cu{sup 2+} and R4 towards Cd{sup 2+} ions was confirmed by UV-Vis spectroscopic study. The R3 showed a red shift in the presence of Cu{sup 2+} ions by Δλ{sub max} 67 nm and R4 showed a red shift in the presence of Cd{sup 2+} ions by Δλ{sub max} 105 nm in the absorption spectrum. The binding stoichiometric ratio of the complex between R3 - Cu{sup 2+} and R4 - Cd{sup 2+} ions have been found to be 1:1 using the B-H plot. Under optimized experimental conditions, the R3 and R4 exhibits a dynamic linear absorption response range, from 0 to 50 μM for Cu{sup 2+} ions and 0 to 30 μM for Cd{sup 2+} ions, with the detection limit of 2.8 × 10{sup −6} M for Cu{sup 2+} and 2.0 × 10{sup −7} M for Cd{sup 2+} ions. The proposed analytical method for the quantitative determination of Cu{sup 2+} and Cd{sup 2+} ions was validated and successfully applied for the environmental samples with good precision and accuracy. - Highlights: • Detection of Cu{sup 2+} and Cd{sup 2+} ions has gained significance by virtue of its key role in biological and environmental science. • The R3 and R4 showed instantaneous color change from colorless to yellow in the presence of Cu{sup 2+} and Cd{sup 2+} ions respectively. • The proposed detection methods were validated and

  8. Separation/preconcentration of silver(I) and lead(II) in environmental samples on cellulose nitrate membrane filter prior to their flame atomic absorption spectrometric determinations

    International Nuclear Information System (INIS)

    Soylak, Mustafa; Cay, Rukiye Sungur

    2007-01-01

    An enrichment method for trace amounts of Ag(I) and Pb(II) has been established prior to their flame atomic absorption spectrometric determinations. The preconcentration/separation procedure is based on chelate formation of Ag(I) and Pb(II) with ammonium pyrrolidine dithiocarbamate (APDC) and on retention of the chelates on cellulose nitrate membrane filter. The influences of some analytical parameters including pH and amounts of reagent, etc. on the recoveries of analytes were investigated. The effects of interferic ions on the quantitative recoveries of analytes were also examined. The detection limits (k = 3, N = 11) were 4.6 μg L -1 for silver(I) and 15.3 μg L -1 for lead(II). The relative standard deviations (R.S.D.) of the determinations for analyte ions were below 3%. The method was applied to environmental samples for the determination of analyte ions with satisfactory results (recoveries >95%)

  9. Island Explorations: Discovering Effects of Environmental Research-Based Lab Activities on Analytical Chemistry Students

    Science.gov (United States)

    Tomasik, Janice Hall; LeCaptain, Dale; Murphy, Sarah; Martin, Mary; Knight, Rachel M.; Harke, Maureen A.; Burke, Ryan; Beck, Kara; Acevedo-Polakovich, I. David

    2014-01-01

    Motivating students in analytical chemistry can be challenging, in part because of the complexity and breadth of topics involved. Some methods that help encourage students and convey real-world relevancy of the material include incorporating environmental issues, research-based lab experiments, and service learning projects. In this paper, we…

  10. Reference materials for micro-analytical nuclear techniques

    International Nuclear Information System (INIS)

    Valkovic, V.; Zeisler, R.; Bernasconi, G.; Danesi, P.R.

    1994-01-01

    Direct application of many existing reference materials in micro-analytical procedures such as energy dispersive x-ray fluorescence (EDXRF), particle induced x-ray emission spectroscopy (PIXE) and ion probe techniques for the determination of trace elements is often impossible or difficult because: 1) other constituents present in large amounts interfere with the determination; 2) trace components are not sufficiently homogeneously distributed in the sample. Therefore specific natural-matrix reference materials containing very low levels of trace elements and having high degree of homogeneity are required for many micro-analytical procedures. In this report, selection of the types of environmental and biological materials which are suitable for micro-analytical techniques will be discussed. (author)

  11. Solid-phase extraction of polar pesticides from environmental water samples on graphitized carbon and Empore-activated carbon disks and on-line coupling to octadecyl-bonded silica analytical columns.

    Science.gov (United States)

    Slobodník, J; Oztezkizan, O; Lingeman, H; Brinkman, U A

    1996-10-25

    The suitability of Empore-activated carbon disks (EACD), Envi-Carb graphitized carbon black (GCB) and CPP-50 graphitized carbon for the trace enrichment of polar pesticides from water samples was studied by means of off-line and on-line solid-phase extraction (SPE). In the off-line procedure, 0.5-2 l samples spiked with a test mixture of oxamyl, methomyl and aldicarb sulfoxide were enriched on EnviCarb SPE cartridges or 47 mm diameter EACD and eluted with dichloromethane-methanol. After evaporation, a sample was injected onto a C18-bonded silica column and analysed by liquid chromatography with ultraviolet (LC-UV) detection. EACD performed better than EnviCarb cartridges in terms of breakthrough volumes (> 2 l for all test analytes), reproducibility (R.S.D. of recoveries, 4-8%, n = 3) and sampling speed (100 ml/min); detection limits in drinking water were 0.05-0.16 microgram/l. In the on-line experiments, 4.6 mm diameter pieces cut from original EACD and stacked onto each other in a 9 mm long precolumn, and EnviCarb and CPP-50 packed in 10 x 2.0 mm I.D. precolumn, were tested, and 50-200 ml spiked water samples were preconcentrated. Because of the peak broadening caused by the strong sorption of the analytes on carbon, the carbon-packed precolumns were eluted by a separate stream of 0.1 ml/min acetonitrile which was mixed with the gradient LC eluent in front of the C18 analytical column. The final on-line procedure was also applied for the less polar propoxur, carbaryl and methiocarb. EnviCarb could not be used due to its poor pressure resistance. CPP-50 provided less peak broadening than EACD: peak widths were 0.1-0.3 min and R.S.D. of peak heights 4-14% (n = 3). In terms of analyte trapping efficiency on-line SPE-LC-UV with a CPP-50 precolumn also showed better performance than when Bondesil C18/OH or polymeric PLRP-S was used, but chromatographic resolution was similar. With the CPP-50-based system, detection limits of the test compounds were 0.05-1 microgram

  12. Environmental radiation monitoring

    International Nuclear Information System (INIS)

    Watanabe, Isao

    2011-01-01

    The samples, pretreatment method, and measurement methods of 'Environmental radioactivity level by prefecture' of Ministry of Education, Culture, Sports, Science and Education (MEXT) is explained. It consists of 1), 'Environmental radioactivity level by prefecture' in normal period, 2) 'Strengthening of Monitoring of Environmental Radioactivity Level by Prefecture' of MEXT at emergency 3) strengthening of monitoring by Fukushima Daiichi nuclear accident, 4) radiation monitoring around the nuclear facility, 5) strengthening of monitoring by MEXT, and 6) quality of monitoring. The survey item and samples etc., of 'Environmental radioactivity level by prefecture', monitoring post, NaI (Tl) scintillation survey meter, sampling and pretreatment methods for radionuclide analysis in normal period, an example of germanium semiconductor detector, gamma ray spectrum of spaghetti from Italy by germanium semiconductor detector, flow chart of radionuclide analysis of fallout in normal period and emergency by germanium semiconductor detector, example of analytical method of radioactive strontium ( ion exchange method), outline of plutonium analytical method for emergency, sampling and pretreatment methods of radionuclides for strengthening, monitoring result around Fukushima Daiichi nuclear plant from June 23 to 24, 2011, change of air dose rate of monitoring post in Mito city from March 14 to 26, 2011, concentration of I-131 and Cs-137 in fallout in Hitachinaka city from March 19 to April 30, 2011, and change of concentration of I-131, Cs-134 and Cs-137 in tap water of Iitate village from March 20 to April 30, 2011, are illustrated. (S.Y.)

  13. o-TOF ICPMS analysis of environmental, food and biological samples

    International Nuclear Information System (INIS)

    Krejcova, A.; Cernohorsky, T.; Ludvikova, I.; Pouzar, M.; Capova, L.

    2009-01-01

    Full text: o-TOF ICPMS was used for inorganic analysis of environmental, food and biological samples. The method validity was proved by analysis of spiked samples, reference materials, by determination without/with internal standards and the standard addition technique. The technique was shown to be powerful, and reliable for analysis of the samples mentioned, and high sample throughput enables environmental or biological screening studies. Independent of the number of elements analyzed, complete analysis and whole mass spectra are gained from a small sample amount in a very short time. (author)

  14. Optimization of organic contaminant and toxicity testing analytical procedures for estimating the characteristics and environmental significance of natural gas processing plant waste sludges

    International Nuclear Information System (INIS)

    Novak, N.

    1990-10-01

    The Gas Plant Sludge Characterization Phase IIB program is a continuation of the Canadian Petroleum Association's (CPA) initiatives to characterize sludge generated at gas processing plants. The objectives of the Phase IIB project were to develop an effective procedure for screening waste sludges or centrifuge/leachate generated from sludge samples for volatile, solvent-soluble and water-soluble organics; verify the reproducibility of the three aquatic toxicity tests recommended as the battery of tests for determining the environmental significance of sludge centrifugates or leachates; assess the performance of two terrestrial toxicity tests in determining the environmental significance of whole sludge samples applied to soil; and to assess and discuss the reproducibility and cost-effectiveness of the sampling and analytical techniques proposed for the overall sludge characterization procedure. Conclusions and recommendations are provided for sludge collection, preparation and distribution, organic analyses, toxicity testing, project management, and procedure standardization. The three aquatic and two terrestrial toxicity tests proved effective in indicating the toxicity of complex mixtures. 27 refs., 3 figs., 59 tabs

  15. Chicago Clean Air, Clean Water Project: Environmental Monitoring for a Healthy, Sustainable Urban Future

    Energy Technology Data Exchange (ETDEWEB)

    none, none; Tuchman, Nancy [Institute of Environmental Sustainability (IES), Chicago, IL (United States)

    2015-11-11

    The U.S. Department of Energy awarded Loyola University Chicago and the Institute of Environmental Sustainability (IES) $486,000.00 for the proposal entitled “Chicago clean air, clean water project: Environmental monitoring for a healthy, sustainable urban future.” The project supported the purchase of analytical instruments for the development of an environmental analytical laboratory. The analytical laboratory is designed to support the testing of field water and soil samples for nutrients, industrial pollutants, heavy metals, and agricultural toxins, with special emphasis on testing Chicago regional soils and water affected by coal-based industry. Since the award was made in 2010, the IES has been launched (fall 2013), and the IES acquired a new state-of-the-art research and education facility on Loyola University Chicago’s Lakeshore campus. Two labs were included in the research and education facility. The second floor lab is the Ecology Laboratory where lab experiments and analyses are conducted on soil, plant, and water samples. The third floor lab is the Environmental Toxicology Lab where lab experiments on environmental toxins are conducted, as well as analytical tests conducted on water, soil, and plants. On the south end of the Environmental Toxicology Lab is the analytical instrumentation collection purchased from the present DOE grant, which is overseen by a full time Analytical Chemist (hired January 2016), who maintains the instruments, conducts analyses on samples, and helps to train faculty and undergraduate and graduate student researchers.

  16. Newly introduced sample preparation techniques: towards miniaturization.

    Science.gov (United States)

    Costa, Rosaria

    2014-01-01

    Sampling and sample preparation are of crucial importance in an analytical procedure, representing quite often a source of errors. The technique chosen for the isolation of analytes greatly affects the success of a chemical determination. On the other hand, growing concerns about environmental and human safety, along with the introduction of international regulations for quality control, have moved the interest of scientists towards specific needs. Newly introduced sample preparation techniques are challenged to meet new criteria: (i) miniaturization, (ii) higher sensitivity and selectivity, and (iii) automation. In this survey, the most recent techniques introduced in the field of sample preparation will be described and discussed, along with many examples of applications.

  17. Automated Clean Chemistry for Bulk Analysis of Environmental Swipe Samples - FY17 Year End Report

    Energy Technology Data Exchange (ETDEWEB)

    Ticknor, Brian W. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Metzger, Shalina C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); McBay, Eddy H. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Hexel, Cole R. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Tevepaugh, Kayron N. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Bostick, Debra A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-11-30

    Sample preparation methods for mass spectrometry are being automated using commercial-off-the-shelf (COTS) equipment to shorten lengthy and costly manual chemical purification procedures. This development addresses a serious need in the International Atomic Energy Agency’s Network of Analytical Laboratories (IAEA NWAL) to increase efficiency in the Bulk Analysis of Environmental Samples for Safeguards program with a method that allows unattended, overnight operation. In collaboration with Elemental Scientific Inc., the prepFAST-MC2 was designed based on COTS equipment. It was modified for uranium/plutonium separations using renewable columns packed with Eichrom TEVA and UTEVA resins, with a chemical separation method based on the Oak Ridge National Laboratory (ORNL) NWAL chemical procedure. The newly designed prepFAST-SR has had several upgrades compared with the original prepFAST-MC2. Both systems are currently installed in the Ultra-Trace Forensics Science Center at ORNL.

  18. Hanford Site Environmental Surveillance Master Sampling Schedule for Calendar Year 2006

    Energy Technology Data Exchange (ETDEWEB)

    Bisping, Lynn E.

    2006-01-27

    This document contains the calendar year 2006 schedules for the routine and non-routine collection of samples for the Surface Environmental Surveillance Project (SESP) and Drinking Water Monitoring Project. Each section includes sampling locations, sample types, and analyses to be performed. In some cases, samples are scheduled on a rotating basis and may not be collected in 2006 in which case the anticipated year for collection is provided. The project document package (PDP) for Surface Environmental Surveillance contains the milestone control log for the issuing of CY06 Environmental Surveillance Master Sampling Schedule WBS 4.2.3.21.3.03, milestone: RL00430306 (4830106-12).

  19. Optimization of pressurized liquid extraction (PLE) of dioxin-furans and dioxin-like PCBs from environmental samples.

    Science.gov (United States)

    Antunes, Pedro; Viana, Paula; Vinhas, Tereza; Capelo, J L; Rivera, J; Gaspar, Elvira M S M

    2008-05-30

    Pressurized liquid extraction (PLE) applying three extraction cycles, temperature and pressure, improved the efficiency of solvent extraction when compared with the classical Soxhlet extraction. Polychlorinated-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs) and dioxin-like PCBs (coplanar polychlorinated biphenyls (Co-PCBs)) in two Certified Reference Materials [DX-1 (sediment) and BCR 529 (soil)] and in two contaminated environmental samples (sediment and soil) were extracted by ASE and Soxhlet methods. Unlike data previously reported by other authors, results demonstrated that ASE using n-hexane as solvent and three extraction cycles, 12.4 MPa (1800 psi) and 150 degrees C achieves similar recovery results than the classical Soxhlet extraction for PCDFs and Co-PCBs, and better recovery results for PCDDs. ASE extraction, performed in less time and with less solvent proved to be, under optimized conditions, an excellent extraction technique for the simultaneous analysis of PCDD/PCDFs and Co-PCBs from environmental samples. Such fast analytical methodology, having the best cost-efficiency ratio, will improve the control and will provide more information about the occurrence of dioxins and the levels of toxicity and thereby will contribute to increase human health.

  20. Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples.

    Science.gov (United States)

    Artigues, Margalida; Abellà, Jordi; Colominas, Sergi

    2017-11-14

    Amperometric biosensors based on the use of glucose oxidase (GOx) are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan) onto highly ordered titanium dioxide nanotube arrays (TiO₂NTAs) has been evaluated. The GOx-Chitosan/TiO₂NTAs biosensor showed a sensitivity of 5.46 μA·mM -1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%), reproducibility (RSD = 2.5%), accuracy (95-105% recovery), and robustness (RSD = 3.3%). Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx-Chitosan/TiO₂NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated.

  1. UNOCAL Parachute Creek Shale Oil Program. Environmental Monitoring Plan - supplemental environmental. Volume 1. Trip 2 report. Rept. for 1988-90

    International Nuclear Information System (INIS)

    1991-01-01

    The Energy Security Act of 1980 established a program to provide financial assistance to private industry in the construction and operation of commercial-scale synthetic fuels plants. The Parachute Creek Shale Oil Program is one of four projects awarded financial assistance. The Program agreed to comply with existing environmental monitoring regulations and to develop an Environmental Monitoring Plan (EMP) incorporating supplemental monitoring in the areas of water, air, solid waste, and worker health and safety during the period 1985-1992. These activities are described in a series of quarterly and annual reports. The report contains results of three years of supplemental environmental sampling (Trial Trip, 1988; Trip 1, 1989; and Trip 2, 1990); Trip 2 sampling and analytical methods; quality assurance and quality control procedures; sampling and analytical methods; and corrected data from 1988 and 1989 gas and particulate concentrations

  2. Radiochemical separation of actinides from environmental samples for determination with DF-ICP-MS and alpha spectrometry

    International Nuclear Information System (INIS)

    Ayranov, M.; Kraehenbuehl, U.; Sahli, H.; Roellin, S.; Burger, M.

    2005-01-01

    The purpose of this study was to develop an optimised sample preparation method for the determination of Pu, Am, and Cm in environmental samples, soils, and sediments, and to compare the sensitivities of DF-ICP-MS, alpha spectrometry, and liquid scintillation alpha spectrometry. Borate fusion was used for sample material digestion. Two methods based on TOPO liquid-liquid extraction and combination of TEVA and TRU extraction chromatography showed highest yields of 92.7% for Pu, 86.8% for Am, and 87.6% for Cm. The detection limits were between 0.014-0.034 Bq/kg for 239 Pu, 0.014-0.093 Bq/kg for 240 Pu, and 0.011-1.20 Bq/kg for 241 Am. Analytical results for 238 Pu, 239 Pu, 240 Pu, 241 Pu and 241 Am and their isotope ratios in certified reference materials (IAEA-135 and IAEA-300) indicated very good accuracy of the methods proposed. (orig.)

  3. Analytical strategies for uranium determination in natural water and industrial effluents samples

    International Nuclear Information System (INIS)

    Santos, Juracir Silva

    2011-01-01

    The work was developed under the project 993/2007 - 'Development of analytical strategies for uranium determination in environmental and industrial samples - Environmental monitoring in the Caetite city, Bahia, Brazil' and made possible through a partnership established between Universidade Federal da Bahia and the Comissao Nacional de Energia Nuclear. Strategies were developed to uranium determination in natural water and effluents of uranium mine. The first one was a critical evaluation of the determination of uranium by inductively coupled plasma optical emission spectrometry (ICP OES) performed using factorial and Doehlert designs involving the factors: acid concentration, radio frequency power and nebuliser gas flow rate. Five emission lines were simultaneously studied (namely: 367.007, 385.464, 385.957, 386.592 and 409.013 nm), in the presence of HN0 3 , H 3 C 2 00H or HCI. The determinations in HN0 3 medium were the most sensitive. Among the factors studied, the gas flow rate was the most significant for the five emission lines. Calcium caused interference in the emission intensity for some lines and iron did not interfere (at least up to 10 mg L -1 ) in the five lines studied. The presence of 13 other elements did not affect the emission intensity of uranium for the lines chosen. The optimized method, using the line at 385.957 nm, allows the determination of uranium with limit of quantification of 30 μg L -1 and precision expressed as RSD lower than 2.2% for uranium concentrations of either 500 and 1000 μg L -1 . In second one, a highly sensitive flow-based procedure for uranium determination in natural waters is described. A 100-cm optical path flow cell based on a liquid-core waveguide (LCW) was exploited to increase sensitivity of the arsenazo 111 method, aiming to achieve the limits established by environmental regulations. The flow system was designed with solenoid micro-pumps in order to improve mixing and minimize reagent consumption, as well as

  4. Determination of bismuth in environmental samples by ICP-MS and basic examination of cell toxicity for their compounds

    International Nuclear Information System (INIS)

    Kobayashi, Jun; Matsukawa, Takehisa; Chiba, Momoko; Yokoyama, Kazuhito; Terada, Hiroshi; Sugiyama, Hideo

    2011-01-01

    We examined both bismuth content levels in some environmental water samples (tapwater, bottled drinking water and slag obtained by sewage disposal) by inductively coupled plasma mass spectrometry (ICP-MS) and cultured cell toxicity of their compounds by the MTT assay. For ICP-MS, the conditions examined were addition of internal standard (IS), apparatus condition, and determination range, etc. When we examined an IS, the advantage was not clear that the ICP-MS response of the IS candidate elements was very variable. However, the sample induction rate into ICP-MS is more changeable at any time. Since the correction of analytical results was enabled by the addition of IS, Tl-203 was selected for IS, and was used in this study. The determination lower limit was 11 ppt by using 10 ppb Tl. Bi was detected in a few environmental water samples at 20.4 ppt - 6.8 ppb (0.07-6.83 μg/g original slags), but Bi concentrations of most samples were lower than the determination limit. On the other hand, concerning cell toxicity, the subgallate and free gallic acid affected the lives of cultured cells. Especially, the toxicity of free gallic acid was higher. It has been understood that the toxicity is weakly adjusted by chelating with Bi. (author)

  5. The analytical calibration in (bio)imaging/mapping of the metallic elements in biological samples--definitions, nomenclature and strategies: state of the art.

    Science.gov (United States)

    Jurowski, Kamil; Buszewski, Bogusław; Piekoszewski, Wojciech

    2015-01-01

    Nowadays, studies related to the distribution of metallic elements in biological samples are one of the most important issues. There are many articles dedicated to specific analytical atomic spectrometry techniques used for mapping/(bio)imaging the metallic elements in various kinds of biological samples. However, in such literature, there is a lack of articles dedicated to reviewing calibration strategies, and their problems, nomenclature, definitions, ways and methods used to obtain quantitative distribution maps. The aim of this article was to characterize the analytical calibration in the (bio)imaging/mapping of the metallic elements in biological samples including (1) nomenclature; (2) definitions, and (3) selected and sophisticated, examples of calibration strategies with analytical calibration procedures applied in the different analytical methods currently used to study an element's distribution in biological samples/materials such as LA ICP-MS, SIMS, EDS, XRF and others. The main emphasis was placed on the procedures and methodology of the analytical calibration strategy. Additionally, the aim of this work is to systematize the nomenclature for the calibration terms: analytical calibration, analytical calibration method, analytical calibration procedure and analytical calibration strategy. The authors also want to popularize the division of calibration methods that are different than those hitherto used. This article is the first work in literature that refers to and emphasizes many different and complex aspects of analytical calibration problems in studies related to (bio)imaging/mapping metallic elements in different kinds of biological samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Environmental monitoring master sampling schedule: January--December 1989

    International Nuclear Information System (INIS)

    Bisping, L.E.

    1989-01-01

    Environmental monitoring of the Hanford Site is conducted by the Pacific Northwest Laboratory (PNL) for the US Department of Energy (DOE). This document contains the planned schedule for routine sample collection for calendar year 1989 for the Surface and Ground-Water Environmental Monitoring Projects. This schedule is subject to modification during the year in response to changes in Site operations, program requirements, and the nature of the observed results. Operational limitations such as weather, mechanical failures, sample availability, etc., may also require schedule modifications. Changes will be documented in the respective project files, but this plan will not be reissued. This schedule includes routine ground-water sampling performed by PNL for Westinghouse Hanford Company, but does not include samples that may be collected in 1989 to support special studies or special contractor projects, or for quality control. The sampling schedule for Site-wide chemical monitoring is not included here, because it varies each quarter as needed, based on past results and operating needs. This schedule does not include Resource Conservation and Recovery Act ground-water sampling performed by PNL for Hanford Site contractors, nor does it include sampling that may be done by other DOE Hanford contractors

  7. Thallium Analysis in Environmental Samples by Inductively Coupled Plasma Mass Spectrometry; Analisis de Talio en Muestras Ambientales por Espectrometria de Masas con Fuente de Plasma de Acoplamiento Inductivo

    Energy Technology Data Exchange (ETDEWEB)

    Higueras, I; Fernandez, M; Conde, E; Gajate, A

    2008-08-06

    Due to its high toxicity, thallium has been considered by the US Environmental Protection Agency as one of the priority pollutants to be controlled. While being a highly toxic element, thallium has been studied to a much lesser degree than other toxic elements, mainly because thallium is often undetected by classical analytical methods. Thallium is a rare and dispersed element that occurs mainly in sulfur-containing ores. Thus, it is a potential pollutant to surrounding environment, if Tl-rich mineral and/or their industrial wastes are not properly disposed. In this work an Inductively Coupled Plasma Mass Spectrometry analytical procedure has been developed in order to determine thallium in environmental solid samples and its application to the study of this element as a potential pollutant associated with natural and anthropogenic activities. The analytical procedure has been validated by the use of appropriate reference materials, and through the isotope dilution technique as a primary method of measurement. Finally, the developed procedure has been applied to several samples from a mining area, as one of the scenarios where thallium it is likely to occur. (Author) 87 refs.

  8. New developments in radiometrics and mass spectrometry methods for radionuclide analysis of environmental samples

    International Nuclear Information System (INIS)

    Povinec, P.P.; LaRosa, J.J.; Lee, S.H.; Wyse, E.

    2002-01-01

    The radionuclide levels observed at present in the environment are very low, therefore high sensitive analytical systems are required for carrying out environmental investigations. One very important recent development in analytical techniques for low-level activity measurements is the production of large volume HPGe detectors (up to 200% relative efficiency to 75 mm diameter x 75 mm long NaI (Tl) crystals). Their high efficiency and excellent energy resolution permit the analyses of various gamma-emitters in composite samples selectively and very often non-destructively (e.g. in sea sediments). However, this technique is restricted to gamma-emitters only (e.g. for 7 Be, 40 K, 54 Mn, 60 Co, 137 Cs, 210 Pb, etc.). Other radionuclides frequently found in the marine environment are the pure beta-emitters, like 3 H, 14 C, 32 Si, 32 P, 90 Sr, 241 Pu, etc., where mainly liquid scintillation counting has made great improvements in recent years. However, for some of these radionuclides mass spectrometry methods represent a real breakthrough in low-level counting, e.g. 3 He in-growth mass spectrometry for 3 H, or accelerator mass spectrometry (AMS) for 14 C

  9. Analytical procedures for determining Pb and Sr isotopic compositions in water samples by ID-TIMS

    Directory of Open Access Journals (Sweden)

    Veridiana Martins

    2008-01-01

    Full Text Available Few articles deal with lead and strontium isotopic analysis of water samples. The aim of this study was to define the chemical procedures for Pb and Sr isotopic analyses of groundwater samples from an urban sedimentary aquifer. Thirty lead and fourteen strontium isotopic analyses were performed to test different analytical procedures. Pb and Sr isotopic ratios as well as Sr concentration did not vary using different chemical procedures. However, the Pb concentrations were very dependent on the different procedures. Therefore, the choice of the best analytical procedure was based on the Pb results, which indicated a higher reproducibility from samples that had been filtered and acidified before the evaporation, had their residues totally dissolved, and were purified by ion chromatography using the Biorad® column. Our results showed no changes in Pb ratios with the storage time.

  10. Rapid isolation of plutonium in environmental solid samples using sequential injection anion exchange chromatography followed by detection with inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Qiao Jixin, E-mail: jixin.qiao@risoe.d [Radiation Research Division, Riso National Laboratory for Sustainable Energy, Technical University of Denmark, DK-4000 Roskilde (Denmark); Hou Xiaolin; Roos, Per [Radiation Research Division, Riso National Laboratory for Sustainable Energy, Technical University of Denmark, DK-4000 Roskilde (Denmark); Miro, Manuel [Department of Chemistry, Faculty of Sciences, University of the Balearic Islands, Carretera de Valldemossa km. 7.5, E-07122 Palma de Mallorca, Illes Balears (Spain)

    2011-01-31

    This paper reports an automated analytical method for rapid determination of plutonium isotopes ({sup 239}Pu and {sup 240}Pu) in environmental solid extracts. Anion exchange chromatographic columns were incorporated in a sequential injection (SI) system to undertake the automated separation of plutonium from matrix and interfering elements. The analytical results most distinctly demonstrated that the crosslinkage of the anion exchanger is a key parameter controlling the separation efficiency. AG 1-x4 type resin was selected as the most suitable sorbent material for analyte separation. Investigation of column size effect upon the separation efficiency revealed that small-sized (2 mL) columns sufficed to handle up to 50 g of environmental soil samples. Under the optimum conditions, chemical yields of plutonium exceeded 90% and the decontamination factors for uranium, thorium and lead ranged from 10{sup 3} to 10{sup 4}. The determination of plutonium isotopes in three standard/certified reference materials (IAEA-375 soil, IAEA-135 sediment and NIST-4359 seaweed) and two reference samples (Irish Sea sediment and Danish soil) revealed a good agreement with reference/certified values. The SI column-separation method is straightforward and less labor intensive as compared with batch-wise anion exchange chromatographic procedures. Besides, the automated method features low consumption of ion-exchanger and reagents for column washing and elution, with the consequent decrease in the generation of acidic waste, thus bearing green chemical credentials.

  11. Determination of plutonium isotopes (238Pu, 239Pu, 240Pu, 241Pu) in environmental samples using radiochemical separation combined with radiometric and mass spectrometric measurements.

    Science.gov (United States)

    Xu, Yihong; Qiao, Jixin; Hou, Xiaolin; Pan, Shaoming; Roos, Per

    2014-02-01

    This paper reports an analytical method for the determination of plutonium isotopes ((238)Pu, (239)Pu, (240)Pu, (241)Pu) in environmental samples using anion exchange chromatography in combination with extraction chromatography for chemical separation of Pu. Both radiometric methods (liquid scintillation counting and alpha spectrometry) and inductively coupled plasma mass spectrometry (ICP-MS) were applied for the measurement of plutonium isotopes. The decontamination factors for uranium were significantly improved up to 7.5 × 10(5) for 20 g soil compared to the level reported in the literature, this is critical for the measurement of plutonium isotopes using mass spectrometric technique. Although the chemical yield of Pu in the entire procedure is about 55%, the analytical results of IAEA soil 6 and IAEA-367 in this work are in a good agreement with the values reported in the literature or reference values, revealing that the developed method for plutonium determination in environmental samples is reliable. The measurement results of (239+240)Pu by alpha spectrometry agreed very well with the sum of (239)Pu and (240)Pu measured by ICP-MS. ICP-MS can not only measure (239)Pu and (240)Pu separately but also (241)Pu. However, it is impossible to measure (238)Pu using ICP-MS in environmental samples even a decontamination factor as high as 10(6) for uranium was obtained by chemical separation. © 2013 Elsevier B.V. All rights reserved.

  12. Environmental monitoring master sampling schedule, January--December 1990

    Energy Technology Data Exchange (ETDEWEB)

    Bisping, L.E.

    1990-01-01

    Environmental monitoring of the Hanford Site is conducted by the Pacific Northwest Laboratory (PNL) for the US Department of Energy (DOE). This document contains the planned schedule for routine sample collection for calendar year 1990 for the Environment Surveillance and Ground-Water Monitoring Projects. This schedule is subject to modification during the year in response to changes in Site operations, program requirements, and the nature of the observed results. Operational limitations such as weather, mechanical failures, sample availability, etc., may also require schedule modifications. Changes will be documented in the respective project files, but this plan will not be reissued. The purpose of these monitoring projects is to evaluate levels of radioactive and nonradioactive pollutants in the Hanford environs. This schedule includes ground-water sampling performed by PNL for environmental surveillance of the Hanford Site.

  13. Towards a Mobile Ecogenomic sensor: the Third Generation Environmental Sample Processor (3G-ESP).

    Science.gov (United States)

    Birch, J. M.; Pargett, D.; Jensen, S.; Roman, B.; Preston, C. M.; Ussler, W.; Yamahara, K.; Marin, R., III; Hobson, B.; Zhang, Y.; Ryan, J. P.; Scholin, C. A.

    2016-02-01

    Researchers are increasingly using one or more autonomous platforms to characterize ocean processes that change in both space and time. Conceptually, studying processes that change quickly both spatially and temporally seems relatively straightforward. One needs to sample in many locations synoptically over time, or follow a coherent water mass and sample it repeatedly. However, implementing either approach presents many challenges. For example, acquiring samples over days to weeks far from shore, without human intervention, requires multiple systems to work together seamlessly, and the level of autonomy, navigation and communications needed to conduct the work exposes the complexity of these requirements. We are addressing these challenges by developing a new generation of robotic systems that are primarily aimed at studies of microbial-mediated processes. As a step towards realizing this new capability, we have taken lessons learned from our second-generation Environmental Sample Processor (2G-ESP), a robotic microbiology "lab-in-a-can" and have re-engineered the system for use on a Tethys-class Long Range AUV (LRAUV). The new instrument is called the third-generation ESP (3G-ESP), and its integration with the LRAUV provides mobility and a persistent presence not seen before in microbial oceanography. The 3G-ESP autonomously filters a water sample and then either preserves that material for eventual return to a laboratory, or processes the sample in real-time for further downstream molecular analytical analyses. The 3G ESP modularizes hardware needed for the collection and preparation of a sample from subsequent molecular analyses by the use of self-contained "cartridges". Cartridges currently come in two forms: one for the preservation of a sample, and the other for onboard homogenization and handoff for downstream processing via one or more analytical devices. The 3G-ESP is designed as a stand-alone instrument, and thus could be deployed on a variety of

  14. Sensitive trace enrichment of environmental andiandrogen vinclozolin from natural waters and sediment samples using hollow-fiber liquid-phase microextraction.

    Science.gov (United States)

    Lambropoulou, Dimitra A; Albanis, Triantafyllos A

    2004-12-17

    The presence of vinclozolin in the environment as far as the endocrine disruption effects in biota are concerned has raised interest in the environmental fate of this compound. In this respect, the present study attempts to investigate the feasibility of applying a novel quantitative method, liquid-phase microextraction (LPME), so as to determine this environmental andiandrogen in environmental samples such as water and sediment samples. The technique involved the use of a small amount (3 microL) of organic solvent impregnated in a hollow fiber membrane, which was attached to the needle of a conventional GC syringe. The extracted samples were analyzed by gas chromatography coupled with electron-capture detection. Experimental LPME conditions such as extraction solvent, stirring rate, content of NaCl and pH were tested. Once LPME was optimized, the performance of the proposed technique was evaluated for the determination of vinclozolin in different types of natural water samples. The recovery of spiked water samples was from 80 to 99%. The procedure was adequate for quantification of vinclozolin in waters at levels of 0.010 to 50 microg/L (r> 0.994) with a detection limit of 0.001 microg/L (S/N= 3). Natural sediment samples from the Aliakmonas River area (Macedonia, Greece) spiked with the target andiandrogen compound were liquid-liquid extracted and analyzed by the methodology developed in this work. No significant interferences from the samples matrix were noticed, indicating that the reported methodology is an innovative tactic for sample preparation in sediment analysis, with a considerable improvement in the achieved detection limits. The results demonstrated that apart from analyte enrichment, the proposed LPME procedure also serves as clean-up method and could be successfully performed to determine trace amounts of vinclozolin in water and sediment samples.

  15. Coupling pervaporation to AAS for inorganic and organic mercury determination. A new approach to speciation of Hg in environmental samples.

    Science.gov (United States)

    Fernandez-Rivas, C; Muñoz-Olivas, R; Camara, C

    2001-12-01

    The design and development of a new approach for Hg speciation in environmental samples is described in detail. This method, consisting of the coupling of pervaporation and atomic absorption spectrometry, is based on a membrane phenomenon that combines the evaporation of volatile analytes and their diffusion through a polymeric membrane. It is proposed here as an alternative to gas chromatography for speciation of inorganic and organic Hg compounds, as the latter compounds are volatile and can be separated by applying the principles mentioned above. The interest of this method lies in its easy handling, low cost, and rapidity for the analysis of liquid and solid samples. This method has been applied to Hg speciation in a compost sample provided by a waste water treatment plant.

  16. Analytical results from salt batch 9 routine DSSHT and SEHT monthly samples

    Energy Technology Data Exchange (ETDEWEB)

    Peters, T. B. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2017-06-01

    Strip Effluent Hold Tank (SEHT) and Decontaminated Salt Solution Hold Tank (DSSHT) samples from several of the “microbatches” of Integrated Salt Disposition Project (ISDP) Salt Batch (“Macrobatch”) 9 have been analyzed for 238Pu, 90Sr, 137Cs, cations (Inductively Coupled Plasma Emission Spectroscopy - ICPES), and anions (Ion Chromatography Anions - IC-A). The analytical results from the current microbatch samples are similar to those from previous macrobatch samples. The Cs removal continues to be acceptable, with decontamination factors (DF) averaging 25700 (107% RSD). The bulk chemistry of the DSSHT and SEHT samples do not show any signs of unusual behavior, other than lacking the anticipated degree of dilution that is calculated to occur during Modular Caustic-Side Solvent Extraction Unit (MCU) processing.

  17. A soil sampling intercomparison exercise for the ALMERA network

    Energy Technology Data Exchange (ETDEWEB)

    Belli, Maria [Istituto Superiore per la Protezione e la Ricerca Ambientale (ISPRA), Via di Castel Romano 100, I-00128 Roma (Italy)], E-mail: maria.belli@apat.it; Zorzi, Paolo de [Istituto Superiore per la Protezione e la Ricerca Ambientale (ISPRA), Via di Castel Romano 100, I-00128 Roma (Italy)], E-mail: paolo.dezorzi@isprambiente.it; Sansone, Umberto [International Atomic Energy Agency (IAEA), Agency' s Laboratories Seibersdorf, A-2444 Seibersdorf (Austria)], E-mail: u.sansone@iaea.org; Shakhashiro, Abduhlghani [International Atomic Energy Agency (IAEA), Agency' s Laboratories Seibersdorf, A-2444 Seibersdorf (Austria)], E-mail: a.shakhashiro@iaea.org; Gondin da Fonseca, Adelaide [International Atomic Energy Agency (IAEA), Agency' s Laboratories Seibersdorf, A-2444 Seibersdorf (Austria)], E-mail: a.gondin-da-fonseca-azeredo@iaea.org; Trinkl, Alexander [International Atomic Energy Agency (IAEA), Agency' s Laboratories Seibersdorf, A-2444 Seibersdorf (Austria)], E-mail: a.trinkl@iaea.org; Benesch, Thomas [International Atomic Energy Agency (IAEA), Agency' s Laboratories Seibersdorf, A-2444 Seibersdorf (Austria)], E-mail: t.benesch@iaea.org

    2009-11-15

    Soil sampling and analysis for radionuclides after an accidental or routine release is a key factor for the dose calculation to members of the public, and for the establishment of possible countermeasures. The IAEA organized for selected laboratories of the ALMERA (Analytical Laboratories for the Measurement of Environmental Radioactivity) network a Soil Sampling Intercomparison Exercise (IAEA/SIE/01) with the objective of comparing soil sampling procedures used by different laboratories. The ALMERA network is a world-wide network of analytical laboratories located in IAEA member states capable of providing reliable and timely analysis of environmental samples in the event of an accidental or intentional release of radioactivity. Ten ALMERA laboratories were selected to participate in the sampling exercise. The soil sampling intercomparison exercise took place in November 2005 in an agricultural area qualified as a 'reference site', aimed at assessing the uncertainties associated with soil sampling in agricultural, semi-natural, urban and contaminated environments and suitable for performing sampling intercomparison. In this paper, the laboratories sampling performance were evaluated.

  18. A soil sampling intercomparison exercise for the ALMERA network

    International Nuclear Information System (INIS)

    Belli, Maria; Zorzi, Paolo de; Sansone, Umberto; Shakhashiro, Abduhlghani; Gondin da Fonseca, Adelaide; Trinkl, Alexander; Benesch, Thomas

    2009-01-01

    Soil sampling and analysis for radionuclides after an accidental or routine release is a key factor for the dose calculation to members of the public, and for the establishment of possible countermeasures. The IAEA organized for selected laboratories of the ALMERA (Analytical Laboratories for the Measurement of Environmental Radioactivity) network a Soil Sampling Intercomparison Exercise (IAEA/SIE/01) with the objective of comparing soil sampling procedures used by different laboratories. The ALMERA network is a world-wide network of analytical laboratories located in IAEA member states capable of providing reliable and timely analysis of environmental samples in the event of an accidental or intentional release of radioactivity. Ten ALMERA laboratories were selected to participate in the sampling exercise. The soil sampling intercomparison exercise took place in November 2005 in an agricultural area qualified as a 'reference site', aimed at assessing the uncertainties associated with soil sampling in agricultural, semi-natural, urban and contaminated environments and suitable for performing sampling intercomparison. In this paper, the laboratories sampling performance were evaluated.

  19. THE STUDY OF HEAVY METAL FROM ENVIRONMENTAL SAMPLES BY ATOMIC TECHNIQUES

    Directory of Open Access Journals (Sweden)

    Ion V. POPESCU

    2011-05-01

    Full Text Available Using the Atomic Absorption Spectrometry (AAS and Energy Dispersive X-ray spectrometry (EDXRF techniques we analyzed the contents of heavy metals ( Cd, Cr, Ni, Pb, Ti, Sr, Co, Bi from eight wild mushrooms and soil substrate samples (48 samples of eight fungal species and 32 underlying soil samples, collected from ten forest sites of Dambovița County Romania. It was determined that the elements, especially heavy metals, in soil were characteristic of the acidic soils of the Romanian forest lands and are influenced by industrial pollution. Analytical possibilities of AAS and EDXRF analytical techniques have been compared and the heavy metal transfer from substrate to mushrooms has been studied. The coefficient of accumulation of essential and heavy metals has been calculated as well. Heavy metal contents of all analyzed mushrooms were generally higher than previously reported in literature.

  20. Environmental sampling: Issues for the cut-off regime

    International Nuclear Information System (INIS)

    Fearey, B.L.

    1995-01-01

    The fissile material cut-off treaty (FMCT) initiative under the Conference on Disarmament mandate is envisioned to include certain aspects of environmental sampling and monitoring. One of the intents of this treaty is to bring certain non-NPT signatories (e.g., threshold states) under this treaty agreement along with the nuclear weapon states (NWSs). This paper provides a brief overview of some of the relevant issues that may be involved in the implementation and use of environmental monitoring for (1) verification of the cut-off regime declarations, (2) the detection of undeclared activities, and, (3) application in non-routine inspections. The intent is to provide backstopping information important for treaty negotiators. Specific issues addressed within this paper include signature sampling, differences in the proposed detection regime, potential signature integrators, specific examples and spoofing concerns. Many of these issues must be carefully considered and weighed in order to create a credibly verifiable inspection regime. Importantly, the cut-off treaty must enable nondiscriminatory implementation, while carefully assuring that nonproliferation treaty requirements are maintained (i.e., preventing unintentional release of critical weapons design information--potentially through environmental sampling and analysis)

  1. Environmental Monitoring Plan, Revision 6

    Energy Technology Data Exchange (ETDEWEB)

    Gallegos, G M; Bertoldo, N A; Blake, R G; Campbell, C G; Grayson, A R; Nelson, J C; Revelli, M A; Rosene, C A; Wegrecki, T; Williams, R A; Wilson, K R; Jones, H E

    2012-03-02

    The purpose of environmental monitoring is to promote the early identification of, and response to, potential adverse environmental impacts associated with Lawrence Livermore National Laboratory (LLNL) operations. Environmental monitoring supports the Integrated Safety Management System (ISMS), International Organization for Standardization (ISO) 14001 Environmental Management Systems standard, and U. S. Department of Energy (DOE) Order 458.1, Radiation Protection of the Public and the Environment. Specifically, environmental monitoring enables LLNL to detect, characterize, and respond to releases from LLNL activities; assess impacts; estimate dispersal patterns in the environment; characterize the pathways of exposure to members of the public; characterize the exposures and doses to individuals and to the population; and to evaluate the potential impacts to the biota in the vicinity of LLNL. Environmental monitoring is also a major component of compliance demonstration for permits and other regulatory requirements. The Environmental Monitoring Plan (EMP) addresses the sample collection and analytical work supporting environmental monitoring to ensure the following: (1) A consistent system for collecting, assessing, and documenting environmental data of known and documented quality; (2) A validated and consistent approach for sampling and analysis of samples to ensure laboratory data meets program-specific needs and requirements within the framework of a performance-based approach for analytical laboratory work; and (3) An integrated sampling approach to avoid duplicative data collection. LLNL prepares the EMP because it provides an organizational framework for ensuring that environmental monitoring work, which is integral to the implementation of LLNL's Environmental Management System, is conducted appropriately. Furthermore, the Environmental Monitoring Plan helps LLNL ensure compliance with DOE Order 231.1 Change 2, Environment, Safety and Health Reporting

  2. Sorption models and their application in environmental samples

    International Nuclear Information System (INIS)

    Kamel, Nariman H.M.

    2008-01-01

    Full text: Naturally occurring radioactive materials (NORM) were found in some environmental soils not high enough to pose problems for human health. The health may be affected by increasing of NORM at some environmental soils. Four soil samples obtained from certain coastal regions in Egypt. Naturally occurring radioactive materials (NORM) of the uranium ( 238 U) series, thorium ( 232 Th) series and the radioactive isotope of potassium ( 40 K) were measured. The soil samples were selected from the situations where the radionuclide concentrations are significantly higher than the average level of other sites. It were chemically analyzed for the uranium, silicon aluminum and iron. The cation exchange capacity (CEC) were determined, it was found lower in the presence of Fe-silicates suggested that Fe-hydroxide had precipitin at the exchangeable edge sites of the clay minerals. The pH of the solid particles at which the net total surface charge is zero was known as the point of zero charge (PZC). The PZC is very important in determining the affinity of the soil samples for different cations and anions. The aim of this work is to determine the natural radiological hazardous of radionuclide at four environmental coastal soil samples in Egypt. The point of zero surface charge was determined using titration tests. Sorption model was developed for this purpose. (author)

  3. Recent bibliography on analytical and sampling problems of a PWR primary coolant Suppl. 4

    International Nuclear Information System (INIS)

    Illy, H.

    1986-09-01

    The 4th supplement of a bibliographical series comprising the analytical and sampling problems of the primary coolant of PWR type reactors covers the literature from 1985 up to July 1986 (220 items). References are listed according to the following topics: boric acid; chloride, chlorine; general; hydrogen isotopes; iodine; iodide; noble gases; oxygen; other elements; radiation monitoring; reactor safety; sampling; water chemistry. (V.N.)

  4. Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples

    Directory of Open Access Journals (Sweden)

    Margalida Artigues

    2017-11-01

    Full Text Available Amperometric biosensors based on the use of glucose oxidase (GOx are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan onto highly ordered titanium dioxide nanotube arrays (TiO2NTAs has been evaluated. The GOx–Chitosan/TiO2NTAs biosensor showed a sensitivity of 5.46 μA·mM−1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%, reproducibility (RSD = 2.5%, accuracy (95–105% recovery, and robustness (RSD = 3.3%. Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx–Chitosan/TiO2NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated.

  5. Analytical Parameters of an Amperometric Glucose Biosensor for Fast Analysis in Food Samples

    Science.gov (United States)

    2017-01-01

    Amperometric biosensors based on the use of glucose oxidase (GOx) are able to combine the robustness of electrochemical techniques with the specificity of biological recognition processes. However, very little information can be found in literature about the fundamental analytical parameters of these sensors. In this work, the analytical behavior of an amperometric biosensor based on the immobilization of GOx using a hydrogel (Chitosan) onto highly ordered titanium dioxide nanotube arrays (TiO2NTAs) has been evaluated. The GOx–Chitosan/TiO2NTAs biosensor showed a sensitivity of 5.46 μA·mM−1 with a linear range from 0.3 to 1.5 mM; its fundamental analytical parameters were studied using a commercial soft drink. The obtained results proved sufficient repeatability (RSD = 1.9%), reproducibility (RSD = 2.5%), accuracy (95–105% recovery), and robustness (RSD = 3.3%). Furthermore, no significant interferences from fructose, ascorbic acid and citric acid were obtained. In addition, the storage stability was further examined, after 30 days, the GOx–Chitosan/TiO2NTAs biosensor retained 85% of its initial current response. Finally, the glucose content of different food samples was measured using the biosensor and compared with the respective HPLC value. In the worst scenario, a deviation smaller than 10% was obtained among the 20 samples evaluated. PMID:29135931

  6. Literature Review on Processing and Analytical Methods for ...

    Science.gov (United States)

    Report The purpose of this report was to survey the open literature to determine the current state of the science regarding the processing and analytical methods currently available for recovery of F. tularensis from water and soil matrices, and to determine what gaps remain in the collective knowledge concerning F. tularensis identification from environmental samples.

  7. A Review for the Analysis of Antidepressant, Antiepileptic and Quinolone Type Drugs in Pharmaceuticals and Environmental Samples.

    Science.gov (United States)

    Rani, Susheela; Malik, Ashok Kumar; Kaur, Ramandeep; Kaur, Ripneel

    2016-09-02

    The analysis of drugs in various biological fluids is an important criterion for the determination of the physiological performance of a drug. After sampling of the biological fluid, the next step in the analytical process is sample preparation. Sample preparation is essential for isolation of desired components from complex biological matrices and greatly influences their reliable and accurate determination. The complexity of biological fluids adds to the challenge of direct determination of the drug by chromatographic analysis, therefore demanding a sample preparation step that is often time consuming, tedious and frequently overlooked. However, direct online injection methods offer the advantage of reducing sample preparation steps and enabling effective pre-concentration and clean-up of biological fluids. These procedures can be automated and therefore reduce the requirements for handling potentially infectious biomaterial, improve reproducibility, and minimize sample manipulations and potential contamination. This review is focused on the discovery and development of high-performance liquid chromatography (HPLC) and gas chromatography (GC) with different detectors. The drugs covered in this review are antiepileptics, antidepressant (AD), and quinolones. The application of these methods for determination of these drugs in biological, environmental and pharmaceutical samples has also been discussed.

  8. [DOE method for evaluating environmental and waste management samples: Revision 1, Addendum 1

    Energy Technology Data Exchange (ETDEWEB)

    Goheen, S.C.

    1995-04-01

    The US Dapartment of Energy`s (DOE`s) environmental and waste management (EM) sampling and analysis activities require that large numbers of samples be analyzed for materials characterization, environmental surveillance, and site-remediation programs. The present document, DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods), is a supplemental resource for analyzing many of these samples.

  9. [DOE method for evaluating environmental and waste management samples: Revision 1, Addendum 1

    International Nuclear Information System (INIS)

    Goheen, S.C.

    1995-04-01

    The US Dapartment of Energy's (DOE's) environmental and waste management (EM) sampling and analysis activities require that large numbers of samples be analyzed for materials characterization, environmental surveillance, and site-remediation programs. The present document, DOE Methods for Evaluating Environmental and Waste Management Samples (DOE Methods), is a supplemental resource for analyzing many of these samples

  10. Enhanced bacterial affinity of PVDF membrane: its application as improved sea water sampling tool for environmental monitoring.

    Science.gov (United States)

    Kumar, Sweta Binod; Sharnagat, Preeti; Manna, Paramita; Bhattacharya, Amit; Haldar, Soumya

    2017-02-01

    Isolation of diversified bacteria from seawater is a major challenge in the field of environmental microbiology. In the present study, an attempt has been made to select specific membrane with improved property of attaching diversified bacteria. Initially, different concentrations (15, 18, and 20% W/W) of polysulfone (PSF) were used to check their affinity for the attachment of selected gram-positive (Bacillus subtilis) and gram-negative (Escherichia coli) bacteria. Among these, 20% W/W PSF showed maximum attachment. Therefore, membrane prepared with other materials such as polyvinylidene fluoride (PVDF) and polyether sulfone (PES) were used with the same concentration (20% W/W) to check their improved bacterial attachment property. Comparative study of bacterial attachment on three different membranes revealed that PVDF possessed the highest affinity towards both the groups of bacteria. This property was confirmed by different analytical methods viz. contact angle, atomic force microscopy, zeta potential, and flux study and further validated with seawater samples collected from seven sites of western coast and Lakshadweep island of India, using Biolog EcoPlate™. All the samples showed that bacterial richness and diversity was high in PVDF membrane in comparison to surrounding seawater samples. Interestingly, affinity for more diversified bacteria was reported to be higher in water sample with less turbidity and low bacteria load. This finding can facilitate the development of PVDF (20% W/W) membrane as a simple, cheap, and less labor intensive environmental sampling tool for the isolation of diversified bacteria from seawater sample wih different physiochemical properties. Graphical abstract ᅟ.

  11. An analysis of combined standard uncertainty for radiochemical measurements of environmental samples

    International Nuclear Information System (INIS)

    Berne, A.

    1996-01-01

    It is anticipated that future data acquisitions intended for use in radiological risk assessments will require the incorporation of uncertainty analysis. Often, only one aliquot of the sample is taken and a single determination is made. Under these circumstances, the total uncertainty is calculated using the open-quotes propagation of errorsclose quotes approach. However, there is no agreement in the radioanalytical community as to the exact equations to use. The Quality Assurance/Metrology Division of the Environmental Measurements Laboratory has developed a systematic process to compute uncertainties in constituent components of the analytical procedure, as well as the combined standard uncertainty (CSU). The equations for computation are presented here, with examples of their use. They have also been incorporated into a code for use in the spreadsheet application, QuattroPro trademark. Using the spreadsheet with appropriate inputs permits an analysis of the variations in the CSU as a function of several different variables. The relative importance of the open-quotes counting uncertaintyclose quotes can also be ascertained

  12. Mercury and gold concentrations of highly polluted environmental samples determined using prompt gamma-ray analysis and instrument neutron activation analysis

    Science.gov (United States)

    Osawa, Takahito; Hatsukawa, Yuichi; Appel, Peter W. U.; Matsue, Hideaki

    2011-04-01

    The authors have established a method of determining mercury and gold in severely polluted environmental samples using prompt gamma-ray analysis (PGA) and instrumental neutron activation analysis (INAA). Since large amounts of mercury are constantly being released into the environment by small-scale gold mining in many developing countries, the mercury concentration in tailings and water has to be determined to mitigate environmental pollution. Cold-vapor atomic absorption analysis, the most pervasive method of mercury analysis, is not suitable because tailings and water around mining facilities have extremely high mercury concentrations. On the other hand, PGA can determine high mercury concentrations in polluted samples as it has an appropriate level of sensitivity. Moreover, gold concentrations can be determined sequentially by using INAA after PGA. In conclusion, the analytical procedure established in this work using PGA and INAA is the best way to evaluate the degree of pollution and the tailing resource value. This method will significantly contribute to mitigating problems in the global environment.

  13. Mercury and gold concentrations of highly polluted environmental samples determined using prompt gamma-ray analysis and instrument neutron activation analysis

    International Nuclear Information System (INIS)

    Osawa, Takahito; Hatsukawa, Yuichi; Appel, Peter W.U.; Matsue, Hideaki

    2011-01-01

    The authors have established a method of determining mercury and gold in severely polluted environmental samples using prompt gamma-ray analysis (PGA) and instrumental neutron activation analysis (INAA). Since large amounts of mercury are constantly being released into the environment by small-scale gold mining in many developing countries, the mercury concentration in tailings and water has to be determined to mitigate environmental pollution. Cold-vapor atomic absorption analysis, the most pervasive method of mercury analysis, is not suitable because tailings and water around mining facilities have extremely high mercury concentrations. On the other hand, PGA can determine high mercury concentrations in polluted samples as it has an appropriate level of sensitivity. Moreover, gold concentrations can be determined sequentially by using INAA after PGA. In conclusion, the analytical procedure established in this work using PGA and INAA is the best way to evaluate the degree of pollution and the tailing resource value. This method will significantly contribute to mitigating problems in the global environment.

  14. A new measurement method for quantification and speciation of technetium-99 in sample at environmental concentrations

    International Nuclear Information System (INIS)

    Kasprzak, L.M.; Aubert, C.; Cossonnet, C.; Fattahi, M.

    2006-01-01

    Technetium-99 is a pure β- emitter and important long half-lived multi-valent radionuclide to be considered in radiation protection of the environment and the public. It a fission product of both 235 U and 239 Pu with approximately a 6% yield. The most stable and very mobile form of Tc is the pertechnetate anion (TcO 4 - ). Therefore, environmental monitoring requires the knowledge of the redox and chemical properties of this element in order to predict its behaviour and transfer in the environment. Given the extremely low concentration of 99 Tc in the environment (10 -10 M to 10 -12 M), its determination currently necessitates an enrichment and separation from the sample matrix prior to instrumental measurement. To this end, the development of a suitable analytical technique is required. The advantages of Capillary Electrophoresis (CE) as a powerful separation technique can be combined with the atomic specificity, multi-elemental character and extremely high sensitivity of an inductively coupled plasma mass spectrometer (ICP-MS) for trace metal-speciation studies in different fields of interest. However, the coupling of both commercially available instruments deserves particular attention if separative resolution, high analyte transport efficiency and sensitive detection are to be achieved. In, that technical vein, the interface itself may be considered as the 'key to success'. Several attempts to develop interfaces for CE-ICP-MS have been described over the last few years. However, the 99 Tc quantification by ICP-MS can be disturbed by isobaric overlaps 99 Ru and interferences induced by the matrix, including those associated with hydride formation ( 98 Mo 1 H (23.8%), 98 Ru 1 H (1.9%)). The aim of the present study was to develop a rapid and efficient method for the determination of 99 Tc in environmental samples by CE-ICP-MS without preliminary classical radiochemical separation to eliminate the interfering elements. In this paper, we describe the development

  15. Detection and Molecular Characterization of Gemycircularvirus from Environmental Samples in Brazil.

    Science.gov (United States)

    da Silva Assis, Matheus Ribeiro; Vieira, Carmen Baur; Fioretti, Julia Monassa; Rocha, Mônica Simões; de Almeida, Pedro Ivo Neves; Miagostovich, Marize Pereira; Fumian, Tulio Machado

    2016-12-01

    Gemycircularvirus (GemyCV) is a group of viruses which has been recently proposed as a new viral genus detected in fecal and environmental samples around the world. GemyCVs have been detected in human blood, brain tissue, cerebrospinal fluid, and stool sample. In the present study, we demonstrate for the first time, through molecular detection and characterization, the presence of GemyCVs in environmental samples from Brazil. Our results show a percentage of positivity ranging from 69 (25/36) to 97 % (35/36) in river water samples collected in Manaus, Amazon region, and wastewater from a wastewater treatment plant located in Rio de Janeiro, respectively, revealing GemyCVs as an important environmental contaminant.

  16. An overview of the Environmental Monitoring Computer Automation Project

    International Nuclear Information System (INIS)

    Johnson, S.M.; Lorenz, R.

    1992-01-01

    The Savannah River Site (SRS) was bulk to produce plutonium and tritium for national defense. As a result of site operations, routine and accidental releases of radionuclides have occurred. The effects these releases have on the k>cal population and environment are of concern to the Department of Energy (DOE) and SRS personnel. Each year, approximately 40,000 environmental samples are collected. The quality of the samples, analytical methods and results obtained are important to site personnel. The Environmental Monitoring Computer Automation Project (EMCAP) was developed to better manage scheduling, log-in, tracking, analytical results, and report generation. EMCAP can be viewed as a custom Laboratory Information Management System (LIMS) with the ability to schedule samples, generate reports, and query data. The purpose of this paper is to give an overview of the SRS environmental monitoring program, describe the development of EMCAP software and hardware, discuss the different software modules, show how EMCAP improved the Environmental Monitoring Section program, and examine the future of EMCAP at SRS

  17. Environmental Contaminants, Metabolites, Cells, Organ Tissues, and Water: All in a Day’s Work at the EPA Analytical Chemistry Research Core

    Science.gov (United States)

    The talk will highlight key aspects and results of analytical methods the EPA National Health and Environmental Effects Research Laboratory (NHEERL) Analytical Chemistry Research Core (ACRC) develops and uses to provide data on disposition, metabolism, and effects of environmenta...

  18. The procedures manual of the Environmental Measurements Laboratory. Volume 2, 28. edition

    Energy Technology Data Exchange (ETDEWEB)

    Chieco, N.A. [ed.

    1997-02-01

    This report contains environmental sampling and analytical chemistry procedures that are performed by the Environmental Measurements Laboratory. The purpose of environmental sampling and analysis is to obtain data that describe a particular site at a specific point in time from which an evaluation can be made as a basis for possible action.

  19. Analytical procedures for the determination of strontium radionuclides in environmental materials

    International Nuclear Information System (INIS)

    Harvey, B.R.; Ibbett, R.D.; Lovett, M.B.; Williams, K.J.

    1989-01-01

    As part of its statutory role in the authorisation, monitoring and research relating to radioactive wastes discharged into the aquatic environment, the Aquatic Environment Protection Division of the Directorate of Fisheries Research (DFR), Lowestoft routinely carries out analyses for a substantial number of radionuclides in a wide range of environmental materials. The Ministry of a Agriculture, Fisheries and Food has for many years required information about the concentrations of strontium radionuclides in waters, sediments and biological materials. There are not absolute standard methods for such radiochemical analysis; indeed none are required because methodology is continually developing. A very considerable amount of expertise has been developed in the analysis of radiostrontium at the Laboratory since the late 1950s, when detailed analysis first commenced, and the procedures described in this report have been developed and tested over a long period of time with a view to achieving the highest analytical quality. Full details of the practical, analytical and computational procedures, as currently used, are given in the Appendix. (author)

  20. Activities at Forschungszentrum Juelich in Safeguards Analytical Techniques and Measurements

    International Nuclear Information System (INIS)

    Duerr, M.; Knott, A.; Middendorp, R.; Niemeyer, I.; Kueppers, S.; Zoriy, M.; Froning, M.; Bosbach, D.

    2015-01-01

    The application of safeguards by the IAEA involves analytical measurements of samples taken during inspections. The development and advancement of analytical techniques with support from the Member States contributes to strengthened and more efficient verification of compliance with non-proliferation obligations. Since recently, a cooperation agreement has been established between Forschungszentrum Juelich and the IAEA in the field of analytical services. The current working areas of Forschungszentrum Juelich are: (i) Production of synthetic micro-particles as calibration standard and reference material for particle analysis, (ii) qualification of the Forschungszentrum Juelich as a member of the IAEA network of analytical laboratories for safeguards (NWAL), and (iii) analysis of impurities in nuclear material samples. With respect to the synthesis of particles, a dedicated setup for the production of uranium particles is being developed, which addresses the urgent need for material tailored for its use in quality assurance and quality control measures for particle analysis of environmental swipe samples. Furthermore, Forschungszentrum Juelich has been nominated as a candidate laboratory for membership in the NWAL network. To this end, analytical capabilities at Forschungszentrum Juelich have been joined to form an analytical service within a dedicated quality management system. Another activity is the establishment of analytical techniques for impurity analysis of uranium-oxide, mainly focusing on inductively coupled mass spectrometry. This contribution will present the activities at Forschungszentrum Juelich in the area of analytical measurements and techniques for nuclear verification. (author)

  1. Determination of Pu, Am and Cm in Environmental Samples

    Energy Technology Data Exchange (ETDEWEB)

    Lujaniene, G. [SRI Centre for Physical Sciences and Technology, Vilnius (Lithuania)

    2013-07-15

    The determination of actinides in the environmental samples at a lower detection limit is required for monitoring purposes and for environmental research. The method for Pu, Am and Cm measurements in soil and sediment samples provides high recoveries and good decontamination from interfering radionuclides. The main steps of the method involve digestion of the samples, separation of radionuclides from matrix using the TOPO /cyclohexane extraction and final purification using extraction Eichrom resins (TEVA, TRU). The accuracy and precision of Pu, Am and Cm analyses were tested using IAEA RM No 135, NIST SRM No 4350b, No 4357 and in intercomparison runs organized by the Riso National Laboratory, Denmark, and in the proficiency tests organized by National Physical Laboratory, UK. The method was applied for measurement of radionuclides in aerosol samples (ashes {approx}30 g), bottom sediments (50-80 g dr. wt) and soil (including Chernobyl soil) samples. (author)

  2. Microplastics in the environment: Challenges in analytical chemistry - A review.

    Science.gov (United States)

    Silva, Ana B; Bastos, Ana S; Justino, Celine I L; da Costa, João P; Duarte, Armando C; Rocha-Santos, Teresa A P

    2018-08-09

    Microplastics can be present in the environment as manufactured microplastics (known as primary microplastics) or resulting from the continuous weathering of plastic litter, which yields progressively smaller plastic fragments (known as secondary microplastics). Herein, we discuss the numerous issues associated with the analysis of microplastics, and to a less extent of nanoplastics, in environmental samples (water, sediments, and biological tissues), from their sampling and sample handling to their identification and quantification. The analytical quality control and quality assurance associated with the validation of analytical methods and use of reference materials for the quantification of microplastics are also discussed, as well as the current challenges within this field of research and possible routes to overcome such limitations. Copyright © 2018 Elsevier B.V. All rights reserved.

  3. Mobile laboratory-based environmental radioactivity analysis capability of the US Environmental Protection Agency

    International Nuclear Information System (INIS)

    Dempsey, G.; Poppell, S.

    1999-01-01

    This poster presentation will highlight the capability of the US Environmental Protection Agency, Office of Radiation and Indoor Air to process and analyze environmental and emergency response samples in mobile radiological laboratories. Philosophy of use, construction, analytical equipment, and procedures will be discussed in the poster presentation. Accompanying the poster presentation, EPA will also have a static display of its mobile laboratories at the meeting site. (author)

  4. Analysis of plant gums and saccharide materials in paint samples: comparison of GC-MS analytical procedures and databases.

    Science.gov (United States)

    Lluveras-Tenorio, Anna; Mazurek, Joy; Restivo, Annalaura; Colombini, Maria Perla; Bonaduce, Ilaria

    2012-10-10

    Saccharide materials have been used for centuries as binding media, to paint, write and illuminate manuscripts and to apply metallic leaf decorations. Although the technical literature often reports on the use of plant gums as binders, actually several other saccharide materials can be encountered in paint samples, not only as major binders, but also as additives. In the literature, there are a variety of analytical procedures that utilize GC-MS to characterize saccharide materials in paint samples, however the chromatographic profiles are often extremely different and it is impossible to compare them and reliably identify the paint binder. This paper presents a comparison between two different analytical procedures based on GC-MS for the analysis of saccharide materials in works-of-art. The research presented here evaluates the influence of the analytical procedure used, and how it impacts the sugar profiles obtained from the analysis of paint samples that contain saccharide materials. The procedures have been developed, optimised and systematically used to characterise plant gums at the Getty Conservation Institute in Los Angeles, USA (GCI) and the Department of Chemistry and Industrial Chemistry of the University of Pisa, Italy (DCCI). The main steps of the analytical procedures and their optimisation are discussed. The results presented highlight that the two methods give comparable sugar profiles, whether the samples analysed are simple raw materials, pigmented and unpigmented paint replicas, or paint samples collected from hundreds of centuries old polychrome art objects. A common database of sugar profiles of reference materials commonly found in paint samples was thus compiled. The database presents data also from those materials that only contain a minor saccharide fraction. This database highlights how many sources of saccharides can be found in a paint sample, representing an important step forward in the problem of identifying polysaccharide binders in

  5. How to take environmental samples for stable isotope analyses

    International Nuclear Information System (INIS)

    Rogers, K.M.

    2009-01-01

    It is possible to analyse a diverse range of samples for environmental investigations. The main types are soil/sediments, vegetation, fauna, shellfish, waste and water. Each type of samples requires different storage and collection methods. Outlined here are the preferred methods of collection to ensure maximum sample integrity and reliability. (author).

  6. How to take environmental samples for stable isotope analyses

    International Nuclear Information System (INIS)

    Rogers, K.M.

    2013-01-01

    It is possible to analyse a diverse range of samples for environmental investigations. The main types are soil/sediments, vegetation, fauna, shellfish, waste and water. Each type of samples requires different storage and collection methods. Outlined here are the preferred methods of collection to ensure maximum sample integrity and reliability. (author).

  7. How to take environmental samples for stable isotope analyses

    International Nuclear Information System (INIS)

    Rogers, K.M.

    2012-01-01

    It is possible to analyse a diverse range of samples for environmental investigations. The main types are soil/sediments, vegetation, fauna, shellfish, waste and water. Each type of samples requires different storage and collection methods. Outlined here are the preferred methods of collection to ensure maximum sample integrity and reliability. (author).

  8. How to take environmental samples for stable isotope analyses

    International Nuclear Information System (INIS)

    Rogers, K.M.

    2009-01-01

    It is possible to analyse a diverse range of samples for environmental investigations. The main types are soil/sediments, vegetation, fauna, shellfish, waste and water. Each type of samples requires different storage and collection methods. Outlined here are the preferred methods of collection to ensure maximum sample integrity and reliability. (author)

  9. Determination of Fe-55 and Ni-63 in Environmental Samples. Analytical Problems. Characteristic Limits. Automatized Calculation; Determinacion de 55{sup F}e y 63{sup N}i en Muestras Ambientales. Problemas Analiticos. Limites Caracteristicos. Calculo Automatizado

    Energy Technology Data Exchange (ETDEWEB)

    Gasco, C; Navarro, N; Gonzalez, P; Heras, M C; Gapan, M P; Alonso, C; Calderon, A; Sanchez, D; Morante, R; Fernandez, M; Gajate, A; Alvarez, A

    2008-08-06

    The Department of Vigilance Radiologica y Radiactividad Ambiental from CIEMAT has developed an appropriate analytical methodology for Fe-55 and Ni-63 sequential determination in environmental samples based on the procedure used by RIS0 Laboratories. The experimental results obtained in the mayor and minor elements behaviour (soil and air constituents) in the different types of resins used for separating Fe-55 and Ni-63 are showed in this report. The measuring method of both isotopes by scintillation counting has been optimized with Ultima Gold liquid with different concentrations of stable element Fe and Ni. The decontamination factors of different gamma-emitters are experimentally determined in this method with the presence of soil matrix. The Fe-55 and Ni-63 activity concentrations and their associated uncertainties have been calculated from the counting data and sample preparation. A computer application has been implemented in Visual Basic in excel sheets for: (I) obtaining the counting data from spectrometer and counts in each window, (II) representing graphically the background and sample spectrums, (III) determining the activity concentration and its associated uncertainty and (IV) calculating the characteristic limits using ISO 11929 (2007) with various confidence levels. (Author) 30 refs.

  10. Determination of the activity of the uranium isotopes U-234, U-235 and U-238 in environmental samples by alpha spectrometry

    International Nuclear Information System (INIS)

    Kromphorn, G.

    1996-02-01

    Different materials containing urandium are regularly investigated in the Laboratory for Environmental Radioactivity of the Physikalisch-Technische Bundesanstalt (PTB) with respect to the activity of the uranium isotopes ( 234 U, 235 U, and 238 U). Moreover for reasons of quality assurance, the PTB takes part in international comparisons where also uranium contents are to be determined in environmental samples and in the framework of which reference materials can be certified. Finally in national comparisons the PTB has the task to determine values of the specific activity for the different isotopes which can play the role of nominal (orientation) values. The single steps of uranium analyses are described after a compilation of the most important data of the uranium isotopes contained in natural uranium: The use of 232 U as tracer, the chemical separation analytics, the production of α-sources and the measuring methods. Analyses of a soil sample and a waste water sample with respect to their specific uranium activity have been chosen as examples of a practical application. (orig.) [de

  11. Least-squares resolution of gamma-ray spectra in environmental samples

    International Nuclear Information System (INIS)

    Kanipe, L.G.; Seale, S.K.; Liggett, W.S.

    1977-08-01

    The use of ALPHA-M, a least squares computer program for analyzing NaI (Tl) gamma spectra of environmental samples, is evaluated. Included is a comprehensive set of program instructions, listings, and flowcharts. Two other programs, GEN4 and SIMSPEC, are also described. GEN4 is used to create standard libraries for ALPHA-M, and SIMSPEC is used to simulate spectra for ALPHA-M analysis. Tests to evaluate the standard libraries selected for use in analyzing environmental samples are provided. An evaluation of the results of sample analyses is discussed

  12. AAS determination of total mercury content in environmental samples

    International Nuclear Information System (INIS)

    Moskalova, M.; Zemberyova, M.

    1997-01-01

    Two methods for determination of total mercury content in environmental samples soils, and sediments, were compared. Dissolution procedure of soils, sediments, and biological material under elevated pressure followed by determination of mercury by cold vapour atomic absorption spectrometry using a MHS-1 system and direct total mercury determination without any chemical pretreatment from soil samples using a Trace Mercury Analyzer TMA-254 were compared. TMA-254 was also applied for the determination of mercury in various further standard reference materials. Good agreement with certified values of environmental reference materials was obtained. (authors)

  13. Collection of analytes from microneedle patches.

    Science.gov (United States)

    Romanyuk, Andrey V; Zvezdin, Vasiliy N; Samant, Pradnya; Grenader, Mark I; Zemlyanova, Marina; Prausnitz, Mark R

    2014-11-04

    Clinical medicine and public health would benefit from simplified acquisition of biological samples from patients that can be easily obtained at point of care, in the field, and by patients themselves. Microneedle patches are designed to serve this need by collecting dermal interstitial fluid containing biomarkers without the dangers, pain, or expertise needed to collect blood. This study presents novel methods to collect biomarker analytes from microneedle patches for analysis by integration into conventional analytical laboratory microtubes and microplates. Microneedle patches were made out of cross-linked hydrogel composed of poly(methyl vinyl ether-alt-maleic acid) and poly(ethylene glycol) prepared by micromolding. Microneedle patches were shown to swell with water up to 50-fold in volume, depending on degree of polymer cross-linking, and to collect interstitial fluid from the skin of rats. To collect analytes from microneedle patches, the patches were mounted within the cap of microcentrifuge tubes or formed the top of V-bottom multiwell microplates, and fluid was collected in the bottom of the tubes under gentle centrifugation. In another method, microneedle patches were attached to form the bottom of multiwell microplates, thereby enabling in situ analysis. The simplicity of biological sample acquisition using microneedle patches coupled with the simplicity of analyte collection from microneedles patches integrated into conventional analytical equipment could broaden the reach of future screening, diagnosis, and monitoring of biomarkers in healthcare and environmental/workplace settings.

  14. Intercalibration of analytical methods on marine environmental samples. Results of MEDPOL II exercise for the intercomparison of trace element measurements on mussel tissue homogenate and marine sediment (MA-M-2/TM and SD-N-1/2/TM)

    International Nuclear Information System (INIS)

    1986-12-01

    Mussels and coastal sediments are often considered as pollution indicators of the marine environment. These intercalibration exercises were organised in order to check the analytical performances of environmental laboratories. The samples MA-M-2/TM of Mediterranean mussels and SD-N-1/2/TM of surface sediment from the Scheldt Estuary (North Sea) were analysed by 19 laboratories for determination of 15 elements: Ag, As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Sb, Se, V and Zn. The analytical methods of atomic absorption spectroscopy, neutron activation analysis and voltametry were used in this intercomparison. For the mussel MA-M-2/TM, 65% of the reported coefficients of variation lie between 0 and 10%, 25% are between 10 and 20%, 9% between 20 and 30% and only 1% higher than 30%. In the case of the sediment SD-N-1/2/TM, 90% of the reported coefficients of variation lie between 0 and 10% and the remaining 10% are between 10 and 20%. The total number of outliers is moderate (9.2% of all results in the case of MA-M-2/TM and 3.0% in the case of SD-N-1/2/TM)

  15. Integrated sampling and analysis unit for the determination of sexual pheromones in environmental air using fabric phase sorptive extraction and headspace-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Alcudia-León, M Carmen; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel; Kabir, Abuzar; Furton, Kenneth G

    2017-03-10

    This article presents a novel unit that integrates for the first time air sampling and preconcentration based on the use of fabric phase sorptive extraction principles. The determination of Tuta absoluta sexual pheromone traces in environmental air has been selected as analytical problem. For this aim, a novel laboratory-built unit made up of commercial brass elements as holder of the sol-gel coated fabric extracting phase has been designed and optimized. The performance of the integrated unit was evaluated analyzing environmental air sampled in tomato crops. The unit can work under sampling and analysis mode which eliminates any need for sorptive phase manipulation prior to instrumental analysis. In the sampling mode, the unit can be connected to a sampling pump to pass the air through the sorptive phase at a controlled flow-rate. In the analysis mode, it is placed in the gas chromatograph autosampler without any instrumental modification. It also diminishes the risk of cross contamination between sampling and analysis. The performance of the new unit has been evaluated using the main components of the sexual pheromone of Tuta absoluta [(3E,8Z,11Z)-tetradecatrien-1-yl acetate and (3E,8Z)-tetradecadien-1-yl acetate] as model analytes. The limits of detection for both compounds resulted to be 1.6μg and 0.8μg, respectively, while the precision (expressed as relative standard deviation) was better than 3.7%. Finally, the unit has been deployed in the field to analyze a number of real life samples, some of them were found positive. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Determination of Organophosphorous Pesticides in Environmental Water Samples Using Surface-Engineered C18 Functionalized Silica-Coated Core-Shell Magnetic Nanoparticles-Based Extraction Coupled with GC-MS/MS Analysis.

    Science.gov (United States)

    Srivastava, Neha; Kumari, Supriya; Nair, Kishore; Alam, Samsul; Raza, Syed K

    2017-05-01

    The present paper depicts a novel method based on magnetic SPE (MSPE) for the determination of organophosphorus pesticides (OPs) such as phorate, malathion, and chlorpyrifos in environmental water samples. In this study, C18 functionalized silica-coated core-shell iron oxide magnetic nanoparticles (MNPs) were used as a surface-engineered magnetic sorbent for the selective extraction of pesticides from aqueous samples, followed by GC-MS and GC-tandem MS analysis for confirmative determination of the analytes. Various important method parameters, including quantity of MNP adsorbent, volume of sample, effective time for extraction, nature of the desorbing solvent, and pH of the aqueous sample, were investigated and optimized to obtain maximum method performance. Under the optimized instrumental analysis conditions, good linearity (r2 value ≥0.994) was achieved at the concentration range of 0.5-500 μg/L. Recoveries were in the range of 79.2-96.3 and 80.4-97.5% in selective-ion monitoring and multiple reaction monitoring (MRM) modes, respectively, at the spiking concentrations of 1, 5, and 10 μg/L. MRM mode showed better sensitivity, selectivity, and low-level detection (0.5 μg/L) of analytes. The novel MSPE method is a simple, cheap, rapid, and eco-friendly method for the determination of OPs in environmental water samples.

  17. The importance of sound methodology in environmental DNA sampling

    Science.gov (United States)

    T. M. Wilcox; K. J. Carim; M. K. Young; K. S. McKelvey; T. W. Franklin; M. K. Schwartz

    2018-01-01

    Environmental DNA (eDNA) sampling - which enables inferences of species’ presence from genetic material in the environment - is a powerful tool for sampling rare fishes. Numerous studies have demonstrated that eDNA sampling generally provides greater probabilities of detection than traditional techniques (e.g., Thomsen et al. 2012; McKelvey et al. 2016; Valentini et al...

  18. Fallout Concentration Various Environmental Samples in Indonesia

    International Nuclear Information System (INIS)

    Sutarman

    2001-01-01

    The testing of nuclear weapons have been carried out by the advanced countries, such as United States, Russian Federation, United Kingdom, France, China, India and Pakistan, since about 1945 until 1998. Nuclear weapons tests were conducted at various locations, on and above the earth's surface or underground or on and under the ocean's surface. Nuclear explosions caused the radionuclides of fission product, such as 131 l, 89 Sr, 90 Sr, 134 Cs, 137 Cs, and 239 Pu released to the atmospheric layer. In the atmospheric layer, the long-lived radionuclides, i.e, 90 Sr dan 137 Cs will be distributed into the environment as the fallout radionuclides, and deposited in the various environmental samples (soil, water, and biota). In general, at several locations in Indonesia the 90 Sr and 137 Cs in the various environmental samples still can be detected. The data of measurement results of 90 Sr and 137 Cs concentrations were generally lower than that from some countries in the northern hemisphere. (author)

  19. Hanford Site Environmental Surveillance Master Sampling Schedule for Calendar Year 2010

    Energy Technology Data Exchange (ETDEWEB)

    Bisping, Lynn E.

    2010-01-08

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by Pacific Northwest National Laboratory for the U.S. Department of Energy (DOE). Sampling is conducted to evaluate levels of radioactive and nonradioactive pollutants in the Hanford Site environs per regulatory requirements. This document contains the calendar year 2010 schedule for the routine collection of samples for the Surface Environmental Surveillance Project and the Drinking Water Monitoring Project. Each section includes sampling locations, sampling frequencies, sample types, and analyses to be performed. In some cases, samples are scheduled on a rotating basis. If a sample will not be collected in 2010, the anticipated year for collection is provided. Maps showing approximate sampling locations are included for media scheduled for collection in 2010.

  20. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

    International Nuclear Information System (INIS)

    Montaser, A.

    1993-01-01

    In this research, new high-temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. During the period January 1993--December 1993, emphasis was placed on (a) analytical investigations of atmospheric-pressure helium inductively coupled plasma (He ICP) that are suitable for atomization, excitation, and ionization of elements possessing high excitation and ionization energies; (b) simulation and computer modeling of plasma sources to predict their structure and fundamental and analytical properties without incurring the enormous cost of experimental studies; (c) spectrosopic imaging and diagnostic studies of high-temperature plasmas; (d) fundamental studies of He ICP discharges and argon-nitrogen plasma by high-resolution Fourier transform spectrometry; and (e) fundamental and analytical investigation of new, low-cost devices as sample introduction systems for atomic spectrometry and examination of new diagnostic techniques for probing aerosols. Only the most important achievements are included in this report to illustrate progress and obstacles. Detailed descriptions of the authors' investigations are outlined in the reprints and preprints that accompany this report. The technical progress expected next year is briefly described at the end of this report

  1. Analytical methodologies for the determination of benzodiazepines in biological samples.

    Science.gov (United States)

    Persona, Karolina; Madej, Katarzyna; Knihnicki, Paweł; Piekoszewski, Wojciech

    2015-09-10

    Benzodiazepine drugs belong to important and most widely used medicaments. They demonstrate such therapeutic properties as anxiolytic, sedative, somnifacient, anticonvulsant, diastolic and muscle relaxant effects. However, despite the fact that benzodiazepines possess high therapeutic index and are considered to be relatively safe, their use can be dangerous when: (1) co-administered with alcohol, (2) co-administered with other medicaments like sedatives, antidepressants, neuroleptics or morphine like substances, (3) driving under their influence, (4) using benzodiazepines non-therapeutically as drugs of abuse or in drug-facilitated crimes. For these reasons benzodiazepines are still studied and determined in a variety of biological materials. In this article, sample preparation techniques which have been applied in analysis of benzodiazepine drugs in biological samples have been reviewed and presented. The next part of the article is focused on a review of analytical methods which have been employed for pharmacological, toxicological or forensic study of this group of drugs in the biological matrices. The review was preceded by a description of the physicochemical properties of the selected benzodiazepines and two, very often coexisting in the same analyzed samples, sedative-hypnotic drugs. Copyright © 2015. Published by Elsevier B.V.

  2. Wet-digestion of environmental sample using silver-mediated electrochemical method

    International Nuclear Information System (INIS)

    Kuwabara, Jun

    2010-01-01

    An application of silver-mediated electrochemical method to environmental samples as the effective digestion method for iodine analysis was tried. Usual digestion method for 129 I in many type of environmental sample is combustion method using quartz glass tube. Chemical yield of iodine on the combustion method reduce depending on the type of sample. The silver-mediated electrochemical method is expected to achieve very low loss of iodine. In this study, dried kombu (Laminaria) sample was tried to digest with electrochemical cell. At the case of 1g of sample, digestion was completed for about 24 hours under the electric condition of <10V and <2A. After the digestion, oxidized species of iodine was reduced to iodide by adding sodium sulfite. And then the precipitate of silver iodide was obtained. (author)

  3. Hanford Environmental Information System (HEIS)

    International Nuclear Information System (INIS)

    1994-01-01

    The purpose of the Soil subject area of the Hanford Environmental Information System (HEIS) is to manage the data acquired from soil samples, both geologic and surface, and sediment samples. Stored in the Soil subject area are data relevant to the soil samples, laboratory analytical results, and field measurements. The two major types of data make up the Soil subject area are data concerning the samples and data about the chemical and/or radiologic analyses of soil samples

  4. Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites

    International Nuclear Information System (INIS)

    2012-01-01

    This plan incorporates U.S. Department of Energy (DOE) Office of Legacy Management (LM) standard operating procedures (SOPs) into environmental monitoring activities and will be implemented at all sites managed by LM. This document provides detailed procedures for the field sampling teams so that samples are collected in a consistent and technically defensible manner. Site-specific plans (e.g., long-term surveillance and maintenance plans, environmental monitoring plans) document background information and establish the basis for sampling and monitoring activities. Information will be included in site-specific tabbed sections to this plan, which identify sample locations, sample frequencies, types of samples, field measurements, and associated analytes for each site. Additionally, within each tabbed section, program directives will be included, when developed, to establish additional site-specific requirements to modify or clarify requirements in this plan as they apply to the corresponding site. A flowchart detailing project tasks required to accomplish routine sampling is displayed in Figure 1. LM environmental procedures are contained in the Environmental Procedures Catalog (LMS/PRO/S04325), which incorporates American Society for Testing and Materials (ASTM), DOE, and U.S. Environmental Protection Agency (EPA) guidance. Specific procedures used for groundwater and surface water monitoring are included in Appendix A. If other environmental media are monitored, SOPs used for air, soil/sediment, and biota monitoring can be found in the site-specific tabbed sections in Appendix D or in site-specific documents. The procedures in the Environmental Procedures Catalog are intended as general guidance and require additional detail from planning documents in order to be complete; the following sections fulfill that function and specify additional procedural requirements to form SOPs. Routine revision of this Sampling and Analysis Plan will be conducted annually at the

  5. Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites

    Energy Technology Data Exchange (ETDEWEB)

    None

    2012-10-24

    This plan incorporates U.S. Department of Energy (DOE) Office of Legacy Management (LM) standard operating procedures (SOPs) into environmental monitoring activities and will be implemented at all sites managed by LM. This document provides detailed procedures for the field sampling teams so that samples are collected in a consistent and technically defensible manner. Site-specific plans (e.g., long-term surveillance and maintenance plans, environmental monitoring plans) document background information and establish the basis for sampling and monitoring activities. Information will be included in site-specific tabbed sections to this plan, which identify sample locations, sample frequencies, types of samples, field measurements, and associated analytes for each site. Additionally, within each tabbed section, program directives will be included, when developed, to establish additional site-specific requirements to modify or clarify requirements in this plan as they apply to the corresponding site. A flowchart detailing project tasks required to accomplish routine sampling is displayed in Figure 1. LM environmental procedures are contained in the Environmental Procedures Catalog (LMS/PRO/S04325), which incorporates American Society for Testing and Materials (ASTM), DOE, and U.S. Environmental Protection Agency (EPA) guidance. Specific procedures used for groundwater and surface water monitoring are included in Appendix A. If other environmental media are monitored, SOPs used for air, soil/sediment, and biota monitoring can be found in the site-specific tabbed sections in Appendix D or in site-specific documents. The procedures in the Environmental Procedures Catalog are intended as general guidance and require additional detail from planning documents in order to be complete; the following sections fulfill that function and specify additional procedural requirements to form SOPs. Routine revision of this Sampling and Analysis Plan will be conducted annually at the

  6. Applied research of environmental monitoring using instrumental neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Chung, Young Sam; Moon, Jong Hwa; Chung, Young Ju

    1997-08-01

    This technical report is written as a guide book for applied research of environmental monitoring using Instrumental Neutron Activation Analysis. The contents are as followings; sampling and sample preparation as a airborne particulate matter, analytical methodologies, data evaluation and interpretation, basic statistical methods of data analysis applied in environmental pollution studies. (author). 23 refs., 7 tabs., 9 figs.

  7. Multi-analyte approach for the determination of ng L-1 levels of steroid hormones in unidentified aqueous samples

    International Nuclear Information System (INIS)

    Noppe, H.; Verheyden, K.; Gillis, W.; Courtheyn, D.; Vanthemsche, P.; De Brabander, H.F.

    2007-01-01

    Since the 1970s, many analytical methods for the detection of illegal growth promoters, such as thyreostats, anabolics, β-agonists and corticosteroids have been developed for a wide range of matrices of animal origin, including meat, fat, organ tissue, urine and faeces. The aim of this study was to develop an analytical method for the determination of ng L -1 levels of estrogens, gestagens, androgens (EGAs) and corticosteroids in aqueous preparations (i.e. drinking water, drinking water supplements), commercially available on the 'black' market. For this, extraction was performed with Bakerbond C 18 speedisk, a technique commonly used in environmental analysis. After fractionation, four fractions were collected using a methanol:water gradient program. Gas chromatography coupled to electron impact multiple mass spectrometry (GC-EI-MS 2 ) screening for the EGAs was carried out on the derivatized extracts. For the detection of corticosteroids, gas chromatography coupled to negative chemical ionization mass spectrometry (GC-NCI-MS) was used after oxidation of the extracts. Confirmation was done by liquid chromatography coupled to electrospray ionization multiple mass spectrometry (LC-ESI-MS 2 ). The combined use of GC and LC coupled to MS enabled the identification and quantification of anabolics and corticosteroids at the low ng L -1 level. This study demonstrated the occurrence of both androgens and corticosteroids in different commercial aqueous samples

  8. Sample Preparation Methodologies for In Situ Liquid and Gaseous Cell Analytical Transmission Electron Microscopy of Electropolished Specimens.

    Science.gov (United States)

    Zhong, Xiang Li; Schilling, Sibylle; Zaluzec, Nestor J; Burke, M Grace

    2016-12-01

    In recent years, an increasing number of studies utilizing in situ liquid and/or gaseous cell scanning/transmission electron microscopy (S/TEM) have been reported. Because of the difficulty in the preparation of suitable specimens, these environmental S/TEM studies have been generally limited to studies of nanoscale structured materials such as nanoparticles, nanowires, or sputtered thin films. In this paper, we present two methodologies which have been developed to facilitate the preparation of electron-transparent samples from conventional bulk metals and alloys for in situ liquid/gaseous cell S/TEM experiments. These methods take advantage of combining sequential electrochemical jet polishing followed by focused ion beam extraction techniques to create large electron-transparent areas for site-specific observation. As an example, we illustrate the application of this methodology for the preparation of in situ specimens from a cold-rolled Type 304 austenitic stainless steel sample, which was subsequently examined in both 1 atm of air as well as fully immersed in a H2O environment in the S/TEM followed by hyperspectral imaging. These preparation techniques can be successfully applied as a general procedure for a wide range of metals and alloys, and are suitable for a variety of in situ analytical S/TEM studies in both aqueous and gaseous environments.

  9. Hanford Site Environmental Surveillance Master Sampling Schedule for Calendar Year 2009

    Energy Technology Data Exchange (ETDEWEB)

    Bisping, Lynn E.

    2009-01-20

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest National Laboratory for the U.S. Department of Energy. Sampling is conducted to evaluate levels of radioactive and nonradioactive pollutants in the Hanford environs, as required in DOE Order 450.1 and DOE Order 5400.5. This document contains the calendar year 2009 schedule for the routine collection of samples for the Surface Environmental Surveillance Project and Drinking Water Monitoring Project. Each section includes sampling locations, sampling frequencies, sample types, and analyses to be performed. In some cases, samples are scheduled on a rotating basis. If a sample will not be collected in 2009, the anticipated year for collection is provided. Maps showing approximate sampling locations are included for media scheduled for collection in 2009.

  10. Sampling methodology and PCB analysis

    International Nuclear Information System (INIS)

    Dominelli, N.

    1995-01-01

    As a class of compounds PCBs are extremely stable and resist chemical and biological decomposition. Diluted solutions exposed to a range of environmental conditions will undergo some preferential degradation and the resulting mixture may differ considerably from the original PCB used as insulating fluid in electrical equipment. The structure of mixtures of PCBs (synthetic compounds prepared by direct chlorination of biphenyl with chlorine gas) is extremely complex and presents a formidable analytical problem, further complicated by the presence of PCBs as contaminants in oils to soils to water. This paper provides some guidance into sampling and analytical procedures; it also points out various potential problems encountered during these processes. The guidelines provided deal with sample collection, storage and handling, sample stability, laboratory analysis (usually gas chromatography), determination of PCB concentration, calculation of total PCB content, and quality assurance. 1 fig

  11. Marine anthropogenic radiotracers in the Southern Hemisphere: New sampling and analytical strategies

    Science.gov (United States)

    Levy, I.; Povinec, P. P.; Aoyama, M.; Hirose, K.; Sanchez-Cabeza, J. A.; Comanducci, J.-F.; Gastaud, J.; Eriksson, M.; Hamajima, Y.; Kim, C. S.; Komura, K.; Osvath, I.; Roos, P.; Yim, S. A.

    2011-04-01

    The Japan Agency for Marine Earth Science and Technology conducted in 2003-2004 the Blue Earth Global Expedition (BEAGLE2003) around the Southern Hemisphere Oceans, which was a rare opportunity to collect many seawater samples for anthropogenic radionuclide studies. We describe here sampling and analytical methodologies based on radiochemical separations of Cs and Pu from seawater, as well as radiometric and mass spectrometry measurements. Several laboratories took part in radionuclide analyses using different techniques. The intercomparison exercises and analyses of certified reference materials showed a reasonable agreement between the participating laboratories. The obtained data on the distribution of 137Cs and plutonium isotopes in seawater represent the most comprehensive results available for the Southern Hemisphere Oceans.

  12. Joint sampling programme-Verification of data obtained in environmental monitoring

    Energy Technology Data Exchange (ETDEWEB)

    Lauria, D.C. [Instituto de Radioprotecao e Dosimetria, Comissao Nacional de Energia Nuclear, Av. Salvador Allende s/no., CEP 22780-160, Rio de Janeiro, RJ (Brazil)], E-mail: dejanira@ird.gov.br; Martins, N.S.F.; Vasconcellos, M.L.H.; Zenaro, R.; Peres, S.S.; Pires do Rio, M.A. [Instituto de Radioprotecao e Dosimetria, Comissao Nacional de Energia Nuclear, Av. Salvador Allende s/no., CEP 22780-160, Rio de Janeiro, RJ (Brazil)

    2008-11-15

    The objective of the Environmental Radiological Monitoring Control programme carried out by the Institute of Radiation Protection and Dosimetry (IRD) in Brazil is to verify the licensee's compliance with the requirements for environmental monitoring of Brazilian facilities. The Joint Sampling Programme (JSP) is just one part of the control programme. In order to verify that the data reported by the licensees is representative and legitimate, this programme verifies sampling procedures, accuracy and precision of the data and the changes in the environmental conditions. This paper discusses the main findings of this programme that allowed IRD to optimize its available resources to control the monitoring of the eight facilities in Brazil.

  13. Environmental Measurements Laboratory annual report, calendar year 1980

    International Nuclear Information System (INIS)

    Volchok, H.L.

    1981-05-01

    The 1980 Annual Report is presented as a series of abstracts, organized by broad programmatic headings under the five technical Laboratory Divisions and one Branch. In addition, a short section appears at the end of the report describing the organization, staff, outside activities and our publications and presentations for the year. Research performaed by the Environmental Studies Division is reported under the following categories: high altitude sampling program, deposition and surface air, and the biosphere. Measurement methods research and air quality field studies are reported by the Aerosol Studies Division. The Radiation Physics Division reported research on radiation transport theory, radiation dosimetry, environmental radioactivity, and the assessment of non-nuclear energy technologies. Research in the Analytical Chemistry Division is reported on quality assurance, analytical support of research projects, analytical development for research projects, and programmatic research. The Instrumentation Division reported research on the development of instrumentation in various categories. The Applied Mathematics Branch reported results of programs for aerosol studies, analytical chemistry, environmental studies, and radiation physics

  14. Macro elemental analysis of food samples by nuclear analytical technique

    Science.gov (United States)

    Syahfitri, W. Y. N.; Kurniawati, S.; Adventini, N.; Damastuti, E.; Lestiani, D. D.

    2017-06-01

    Energy-dispersive X-ray fluorescence (EDXRF) spectrometry is a non-destructive, rapid, multi elemental, accurate, and environment friendly analysis compared with other detection methods. Thus, EDXRF spectrometry is applicable for food inspection. The macro elements calcium and potassium constitute important nutrients required by the human body for optimal physiological functions. Therefore, the determination of Ca and K content in various foods needs to be done. The aim of this work is to demonstrate the applicability of EDXRF for food analysis. The analytical performance of non-destructive EDXRF was compared with other analytical techniques; neutron activation analysis and atomic absorption spectrometry. Comparison of methods performed as cross checking results of the analysis and to overcome the limitations of the three methods. Analysis results showed that Ca found in food using EDXRF and AAS were not significantly different with p-value 0.9687, whereas p-value of K between EDXRF and NAA is 0.6575. The correlation between those results was also examined. The Pearson correlations for Ca and K were 0.9871 and 0.9558, respectively. Method validation using SRM NIST 1548a Typical Diet was also applied. The results showed good agreement between methods; therefore EDXRF method can be used as an alternative method for the determination of Ca and K in food samples.

  15. PFAS methods and guidance for sampling and analyzing water and other environmental media (Technical Brief)

    Science.gov (United States)

    EPA's methods for analyzing PFAS in environmental media are in various stages of development. This fact sheet summarizes EPA's analytical methods development for groundwater, surface water, wastewater, and solids, including soils, sediments, and biosolids

  16. Sampling in practice

    DEFF Research Database (Denmark)

    Esbensen, Kim Harry; Petersen, Lars

    2005-01-01

    A basic knowledge of the Theory of Sampling (TOS) and a set of only eight sampling unit operations is all the practical sampler needs to ensure representativeness of samples extracted from all kinds of lots: production batches, - truckloads, - barrels, sub-division in the laboratory, sampling...... in nature and in the field (environmental sampling, forestry, geology, biology), from raw materials or manufactory processes etc. We here can only give a brief introduction to the Fundamental Sampling Principle (FSP) and these eight Sampling Unit Operations (SUO’s). Always respecting FSP and invoking only...... the necessary SUO’s (dependent on the practical situation) is the only prerequisite needed for eliminating all sampling bias and simultaneously minimizing sampling variance, and this is in addition a sure guarantee for making the final analytical results trustworthy. No reliable conclusions can be made unless...

  17. Study of comparison between neutron activation analysis and the other analytical methods

    International Nuclear Information System (INIS)

    Nagatsuka, Sumiko

    1986-01-01

    The neutron activation analysis (NAA) is compared with other analytical methods based on various data. It is concluded that NAA is most frequently used for the analysis of NBS environmental standard samples. NAA is suitable for the analysis of trace elements contained in environmental samples since non-destructive quantitative determination can be carried out simultaneously for different elements. NAA and XRF are the only methods which can be used for analyzing oil samples. This also indicates the usefulness of non-destructive techniques. In any standard sample, NAA can achieve a high accuracy for more than 90 % of the elements contained. On the other hand, the accuracy varies depending on the type of sample in the case of the other analytical methods examined. Regarding the prescision, NAA for any standard sample is the smallest in the proportion of the number of elements determined with C.V. (coefficient of variation) of less than 10 % to the total number of elements contained. However, the total number of elements which can be determined by NAA with C.V. of less than 10 % is greater than that by any of the other four methods examined. It should be noticed that there are some elements which can be determined only by NAA. (Nogami, K.)

  18. Application of ICP-MS in Environmental Sampling Analysis for Safeguards

    International Nuclear Information System (INIS)

    Eko Pudjadi; Petrus Zacharias; Budi Prayitno

    2004-01-01

    Environmental samples measured by ICP-MS were analyzed for safeguards. There are two isotopes in environmental sampling that is used to find out the origin of nuclear materials and verify undeclared nuclear activities. Uranium isotopes are 234 U, 235 U, 236 U and 238 U and Plutonium isotopes are 239 Pu, 240 Pu, 241 Pu and 242 Pu. Uranium isotopes are used to verify an existing of nuclear power plants, enrichment plants or reprocessing plants. Plutonium isotopes are used to clarify global fallout from nuclear weapon testing and accident of nuclear facility or military purposes. The high sensitivity of ICP-MS can detect the isotopic fingerprint and trace elements in ppb concentration; ICP-MS has been applied to measure 235 U isotopic ratio and 240 Pu/ 239 Pu isotopic ratios. The sensitivity of ICP-MS is high precision and low operational cost in environmental sampling and can be considered in nuclear power design based on safeguards for development countries. (author)

  19. Environmental report 1993

    International Nuclear Information System (INIS)

    Wilt, G.C.; Gallegos, G.M.; Tate, P.J.; Balke, B.K.

    1994-01-01

    Lawrence Livermore National Laboratory (LLNL), a US Department of Energy (DOE) facility operated by the University of California, serves as a national resource of scientific, technical, and engineering capability with a special focus on national security. Over the years, the Laboratory's mission has been broadened to encompass such areas as strategic defense, energy, the environment, biomedicine, the economy, and education. The Laboratory carries out this mission in compliance with local, state, and federal environmental regulatory requirements and takes measures to ensure that its operations do not adversely affect the environment or public health. It does so with the support of the Environmental Protection Department, which is responsible for environmental monitoring, environmental restoration, hazardous waste management, and ensuring environmental compliance. During 1993, the Environmental Protection Department conducted sampling of air, sewage effluent, ground water, surface water, soil, vegetation and foodstuffs, and took measurements of environmental radiation. It performed more than 190,000 analyses of environmental samples. The analytical results are summarized along with evaluations of the impact of radioactive and nonradioactive materials, a discussion of the effects of LLNL operations on the environment, and a summary of the activities undertaken to comply with local, state, and federal environmental laws

  20. Environmental report 1993

    Energy Technology Data Exchange (ETDEWEB)

    Wilt, G.C. [ed.; Gallegos, G.M.; Tate, P.J.; Balke, B.K. [and others

    1994-09-01

    Lawrence Livermore National Laboratory (LLNL), a US Department of Energy (DOE) facility operated by the University of California, serves as a national resource of scientific, technical, and engineering capability with a special focus on national security. Over the years, the Laboratory`s mission has been broadened to encompass such areas as strategic defense, energy, the environment, biomedicine, the economy, and education. The Laboratory carries out this mission in compliance with local, state, and federal environmental regulatory requirements and takes measures to ensure that its operations do not adversely affect the environment or public health. It does so with the support of the Environmental Protection Department, which is responsible for environmental monitoring, environmental restoration, hazardous waste management, and ensuring environmental compliance. During 1993, the Environmental Protection Department conducted sampling of air, sewage effluent, ground water, surface water, soil, vegetation and foodstuffs, and took measurements of environmental radiation. It performed more than 190,000 analyses of environmental samples. The analytical results are summarized along with evaluations of the impact of radioactive and nonradioactive materials, a discussion of the effects of LLNL operations on the environment, and a summary of the activities undertaken to comply with local, state, and federal environmental laws.

  1. Gamma-ray self-attenuation corrections in environmental samples

    International Nuclear Information System (INIS)

    Robu, E.; Giovani, C.

    2009-01-01

    Gamma-spectrometry is a commonly used technique in environmental radioactivity monitoring. Frequently the bulk samples that should be measured differ with respect to composition and density from the reference sample used for efficiency calibration. Correction factors should be applied in these cases for activity measurement. Linear attenuation coefficients and self-absorption correction factors have been evaluated for soil, grass and liquid sources with different densities and geometries.(authors)

  2. Synthetic and Virtual Environmental Media (SAVEM)

    International Nuclear Information System (INIS)

    Booth, F. H. K.; Decker, K. M.; Bath, R. J.; Bottrell, D. W.; Wright, K. L.

    2002-01-01

    The Synthetic and Virtual Environmental Media (SAVEM) Program, developed at the DOE Environmental Measurements Laboratory, responds directly to issues of improved data quality, increased regulatory confidence, analytical laboratory waste minimization, pollution prevention, worker safety/radiation exposure risk reduction, and environmental stewardship. The SAVEM radiochemistry information analysis system uses digitally generated spectra to accurately model gamma-ray emission characteristics of radiological samples. A digital virtual sample can be specified that has the characteristics of any environmental media such as soil, sediment, or vegetation, and which exhibits the spectral characteristics of more than 2,000 gamma-emitting nuclides. The SAVEM system can duplicate the characteristics of 2,361 individual radionuclides with 47,902 gamma lines

  3. Sampling and Analysis Plan for Supplemental Environmental Project: Aquatic Life Surveys

    Energy Technology Data Exchange (ETDEWEB)

    Berryhill, Jesse Tobias [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Gaukler, Shannon Marie [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-09-26

    As part of a settlement agreement for nuclear waste incidents in 2014, several supplemental environment projects (SEPs) were initiated at Los Alamos National Laboratory (LANL or the Laboratory) between the U.S. Department of Energy and the state of New Mexico. One SEP from this agreement consists of performing aquatic life surveys and will be used to assess the applicability of using generic ambient water-quality criteria (AWQC) for aquatic life. AWQC are generic criteria developed by the U.S. Environmental Protection Agency (EPA) to cover a broad range of aquatic species and are not unique to a specific region or state. AWQC are established by a composition of toxicity data, called species sensitivity distributions (SSDs), and are determined by LC50 (lethal concentration of 50% of the organisms studied) acute toxicity experiments for chemicals of interest. It is of interest to determine whether aquatic species inhabiting waters on the Pajarito Plateau are adequately protected using the current generic AWQC. The focus of this study will determine which aquatic species are present in ephemeral, intermittent, and perennial waters within LANL boundaries and from reference waters adjacent to LANL. If the species identified from these waters do not generally represent species used in the SSDs, then SSDs may need to be modified and AWQC may need to be updated. This sampling and analysis plan details the sampling methodology, surveillance locations, temporal scheduling, and analytical approaches that will be used to complete aquatic life surveys. A significant portion of this sampling and analysis plan was formalized by referring to Appendix E: SEP Aquatic Life Surveys DQO (Data Quality Objectives).

  4. Infrared characterization of environmental samples by pulsed photothermal spectroscopy

    International Nuclear Information System (INIS)

    Seidel, W.; Foerstendorf, H.; Heise, K.H.; Nicolai, R.; Schamlott, A.; Ortega, J.M.; Glotin, F.; Prazeres, R.

    2004-01-01

    Low concentration of toxic radioactive metals in environmental samples often limits the interpretation of results of infrared studies investigating the interaction processes between the metal ions and environmental compartments. For the first time, we could show that photothermal infrared spectroscopy performed with a pulsed free electron laser can provide reliable infrared spectra throughout a distinct spectral range of interest. In this model investigation, we provide vibrational absorption spectra of a rare earth metal salt dissolved in a KBr matrix and a natural calcite sample obtained by photothermal beam deflection (PTBD) technique and FT-IR (Fourier-transform infrared) spectroscopy, respectively. General agreement was found between all spectra of the different recording techniques. Spectral deviations were observed with samples containing low concentration of the rare earth metal salt indicating a lower detection limit of the photothermal method as compared to conventional FT-IR spectroscopy. (authors)

  5. Hanford Site surface environmental surveillance

    International Nuclear Information System (INIS)

    Dirkes, R.L.

    1998-01-01

    Environmental surveillance of the Hanford Site and the surrounding region is conducted to demonstrate compliance with environmental regulations, confirm adherence to US Department of Energy (DOE) environmental protection policies, support DOE environmental management decisions, and provide information to the public. The Surface Environmental Surveillance Project (SESP) is a multimedia environmental monitoring program conducted to measure the concentrations of radionuclides and chemical contaminants in the environment and assess the integrated effects of these contaminants on the environment and the public. The monitoring program includes sampling air, surface water, sediments, soil, natural vegetation, agricultural products, fish, and wildlife. Functional elements inherent in the operation of the SESP include project management, quality assurance/control, training, records management, environmental sampling network design and implementation, sample collection, sample analysis, data management, data review and evaluation, exposure assessment, and reporting. The SESP focuses on those contaminant/media combinations calculated to have the highest potential for contributing to off-site exposure. Results of the SESP indicate that contaminant concentrations in the Hanford environs are very low, generally below environmental standards, at or below analytical detection levels, and indicative of environmental levels. However, areas of elevated contaminant concentrations have been identified at Hanford. The extent of these areas is generally limited to past operating areas and waste disposal sites

  6. Qualitative and quantitative analysis of environmental samples by laser-induced breakdown spectrometry

    International Nuclear Information System (INIS)

    Zorov, N B; Popov, A M; Zaytsev, S M; Labutin, T A

    2015-01-01

    The key achievements in the determination of trace amounts of components in environmental samples (soils, ores, natural waters, etc.) by laser-induced breakdown spectrometry are considered. Unique capabilities of this method make it suitable for rapid analysis of metals and alloys, glasses, polymers, objects of cultural heritage, archaeological and various environmental samples. The key advantages of the method that account for its high efficiency are demonstrated, in particular, a small amount of analyzed material, the absence of sample preparation, the possibility of local and remote analysis of either one or several elements. The use of chemometrics in laser-induced breakdown spectrometry for qualitative sample classification is described in detail. Various approaches to improving the figures of merit of quantitative analysis of environmental samples are discussed. The achieved limits of detection for most elements in geochemical samples are critically evaluated. The bibliography includes 302 references

  7. Analysis procedure for americium in environmental samples

    International Nuclear Information System (INIS)

    Holloway, R.W.; Hayes, D.W.

    1982-01-01

    Several methods for the analysis of 241 Am in environmental samples were evaluated and a preferred method was selected. This method was modified and used to determine the 241 Am content in sediments, biota, and water. The advantages and limitations of the method are discussed. The method is also suitable for 244 Cm analysis

  8. A new measurement method for quantification and speciation of technetium-99 in sample at environmental concentrations

    Energy Technology Data Exchange (ETDEWEB)

    Kasprzak, L.M. [IRSN/DEI/STEME/LMRE, ORSAY, F-91400 (France); SUBATECH, EMN-IN2P3/CNRS-Universit Nantes, F-44307 (France); Aubert, C.; Cossonnet, C. [IRSN/DEI/STEME/LMRE, ORSAY, F-91400 (France); Fattahi, M. [SUBATECH, EMN-IN2P3/CNRS-Universit Nantes, F-44307 (France)

    2006-07-01

    Technetium-99 is a pure {beta}- emitter and important long half-lived multi-valent radionuclide to be considered in radiation protection of the environment and the public. It a fission product of both {sup 235}U and {sup 239}Pu with approximately a 6% yield. The most stable and very mobile form of Tc is the pertechnetate anion (TcO{sub 4}{sup -}). Therefore, environmental monitoring requires the knowledge of the redox and chemical properties of this element in order to predict its behaviour and transfer in the environment. Given the extremely low concentration of {sup 99}Tc in the environment (10{sup -10} M to 10{sup -12} M), its determination currently necessitates an enrichment and separation from the sample matrix prior to instrumental measurement. To this end, the development of a suitable analytical technique is required. The advantages of Capillary Electrophoresis (CE) as a powerful separation technique can be combined with the atomic specificity, multi-elemental character and extremely high sensitivity of an inductively coupled plasma mass spectrometer (ICP-MS) for trace metal-speciation studies in different fields of interest. However, the coupling of both commercially available instruments deserves particular attention if separative resolution, high analyte transport efficiency and sensitive detection are to be achieved. In, that technical vein, the interface itself may be considered as the 'key to success'. Several attempts to develop interfaces for CE-ICP-MS have been described over the last few years. However, the {sup 99}Tc quantification by ICP-MS can be disturbed by isobaric overlaps {sup 99}Ru and interferences induced by the matrix, including those associated with hydride formation ({sup 98}Mo{sup 1}H (23.8%), {sup 98}Ru{sup 1}H (1.9%)). The aim of the present study was to develop a rapid and efficient method for the determination of {sup 99}Tc in environmental samples by CE-ICP-MS without preliminary classical radiochemical separation to

  9. Hanford Sampling Quality Management Plan (HSQMP)

    International Nuclear Information System (INIS)

    Hyatt, J.E.

    1995-06-01

    HSQMP establishes quality requirements in response to DOE Order 5700. 6C and to 10 Code of Federal Regulations 830.120. HSQMP is designed to meet the needs of Richland Operations Office for controlling the quality of services provided by sampling operations. It is issued through the Analytical Services Program of the Waste Programs Division. This document describes the Environmental Sampling and Analysis Program activities considered to represent the best management activities necessary to achieve a sampling program with adequate control

  10. Organically bound tritium analysis in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Baglan, N. [CEA/DAM/DIF, Arpajon (France); Kim, S.B. [AECL, Chalk River Laboratories, Chalk River, ON (Canada); Cossonnet, C. [IRSN/PRP-ENV/STEME/LMRE, Orsay (France); Croudace, I.W.; Warwick, P.E. [GAU-Radioanalytical, University of Southampton, Southampton (United Kingdom); Fournier, M. [IRSN/DG/DMQ, Fontenay-aux-Roses (France); Galeriu, D. [IFIN-HH, Horia-Hulubei, Inst. Phys. and Nucl. Eng., Bucharest (Romania); Momoshima, N. [Kyushu University, Radioisotope Ctr., Fukuoka (Japan); Ansoborlo, E. [CEA/DEN/DRCP/CETAMA, Bagnols-sur-Ceze (France)

    2015-03-15

    Organically bound tritium (OBT) has become of increased interest within the last decade, with a focus on its behaviour and also its analysis, which are important to assess tritium distribution in the environment. In contrast, there are no certified reference materials and no standard analytical method through the international organization related to OBT. In order to resolve this issue, an OBT international working group was created in May 2012. Over 20 labs from around the world participated and submitted their results for the first intercomparison exercise results on potato (Sep 2013). The samples, specially-prepared potatoes, were provided in March 2013 to each participant. Technical information and results from this first exercise are discussed here for all the labs which have realised the five replicates necessary to allow a reliable statistical treatment. The results are encouraging as the increased number of participating labs did not degrade the observed dispersion of the results for a similar activity level. Therefore, the results do not seem to depend on the analytical procedure used. From this work an optimised procedure can start to be developed to deal with OBT analysis and will guide subsequent planned OBT trials by the international group.

  11. Capability of environmental sampling to detect undeclared cask openings

    Energy Technology Data Exchange (ETDEWEB)

    Beckstead, L.W.; Efurd, D.W.; Hemberger, P.H.; Abhold, M.E.; Eccleston, G.W.

    1997-12-01

    The goal of this study is to determine the signatures that would allow monitors to detect diversion of nuclear fuel (by a diverter) from a storage area such as a geological repository. Due to the complexity of operations surrounding disposal of spent nuclear fuel in a geologic repository, there are several places that a diversion of fuel could take place. After the canister that contains the fuel rods is breached, the diverter would require a hot cell to process or repackage the fuel. A reference repository and possible diversion scenarios are discussed. When a canister is breached, or during reprocessing to extract nuclear weapons material (primarily Pu), several important isotopes or signatures including tritium, {sup 85}Kr, and {sup 129}I are released to the surrounding environment and have the potential for analysis. Estimates of release concentrations of the key signatures from the repository under a hypothetical diversion scenario are presented and discussed. Gas analysis data collected from above-ground storage casks at Idaho National Engineering and Environmental Laboratory (INEEL) Test Area North (TAN) are included and discussed in the report. In addition, LANL participated in gas sampling of one TAN cask, the Castor V/21, in July 1997. Results of xenon analysis from the cask gas sample are presented and discussed. The importance of global fallout and recent commercial reprocessing activities and their effects on repository monitoring are discussed. Monitoring and instrumental equipment for analysis of the key signature isotopes are discussed along with limits of detection. A key factor in determining if diversion activities are in progress at a repository is the timeliness of detection and analysis of the signatures. Once a clandestine operation is suspected, analytical data should be collected as quickly as possible to support any evidence of diversion.

  12. Capability of environmental sampling to detect undeclared cask openings

    International Nuclear Information System (INIS)

    Beckstead, L.W.; Efurd, D.W.; Hemberger, P.H.; Abhold, M.E.; Eccleston, G.W.

    1997-01-01

    The goal of this study is to determine the signatures that would allow monitors to detect diversion of nuclear fuel (by a diverter) from a storage area such as a geological repository. Due to the complexity of operations surrounding disposal of spent nuclear fuel in a geologic repository, there are several places that a diversion of fuel could take place. After the canister that contains the fuel rods is breached, the diverter would require a hot cell to process or repackage the fuel. A reference repository and possible diversion scenarios are discussed. When a canister is breached, or during reprocessing to extract nuclear weapons material (primarily Pu), several important isotopes or signatures including tritium, 85 Kr, and 129 I are released to the surrounding environment and have the potential for analysis. Estimates of release concentrations of the key signatures from the repository under a hypothetical diversion scenario are presented and discussed. Gas analysis data collected from above-ground storage casks at Idaho National Engineering and Environmental Laboratory (INEEL) Test Area North (TAN) are included and discussed in the report. In addition, LANL participated in gas sampling of one TAN cask, the Castor V/21, in July 1997. Results of xenon analysis from the cask gas sample are presented and discussed. The importance of global fallout and recent commercial reprocessing activities and their effects on repository monitoring are discussed. Monitoring and instrumental equipment for analysis of the key signature isotopes are discussed along with limits of detection. A key factor in determining if diversion activities are in progress at a repository is the timeliness of detection and analysis of the signatures. Once a clandestine operation is suspected, analytical data should be collected as quickly as possible to support any evidence of diversion

  13. Sampling and Analytical Method for Alpha-Dicarbonyl Flavoring Compounds via Derivatization with o-Phenylenediamine and Analysis Using GC-NPD

    Directory of Open Access Journals (Sweden)

    Stephanie M. Pendergrass

    2016-01-01

    Full Text Available A novel methodology is described for the sampling and analysis of diacetyl, 2,3-pentanedione, 2,3-hexanedione, and 2,3-heptanedione. These analytes were collected on o-phenylenediamine-treated silica gel tubes and quantitatively recovered as the corresponding quinoxaline derivatives. After derivatization, the sorbent was desorbed in 3 mL of ethanol solvent and analyzed using gas chromatography/nitrogen-phosphorous detection (GC/NPD. The limits of detection (LOD achieved for each analyte were determined to be in the range of 5–10 nanograms/sample. Evaluation of the on-tube derivatization procedure indicated that it is unaffected by humidities ranging from 20% to 80% and that the derivatization procedure was quantitative for analyte concentrations ranging from 0.1 μg to approximately 500 μg per sample. Storage stability studies indicated that the derivatives were stable for 30 days when stored at both ambient and refrigerated temperatures. Additional studies showed that the quinoxaline derivatives were quantitatively recovered when sampling up to a total volume of 72 L at a sampling rate of 50 cc/min. This method will be important to evaluate and monitor worker exposures in the food and flavoring industry. Samples can be collected over an 8-hour shift with up to 288 L total volume collected regardless of time, sampling rate, and/or the effects of humidity.

  14. Total Decomposition of Environmental Radionuclide Samples with a Microwave Oven

    International Nuclear Information System (INIS)

    Ramon Garcia, Bernd Kahn

    1998-01-01

    Closed-vessel microwave assisted acid decomposition was investigated as an alternative to traditional methods of sample dissolution/decomposition. This technique, used in analytical chemistry, has some potential advantages over other procedures. It requires less reagents, it is faster, and it has the potential of achieving total dissolution because of higher temperatures and pressures

  15. Radiological analyses of Marshall Islands environmental samples, 1974--1976

    International Nuclear Information System (INIS)

    Greenhouse, N.A.; Miltenberger, R.P.; Cua, F.T.

    1977-01-01

    Results are reported from the radiological analysis of environmental samples collected in the Marshall Islands during 1974 through 1976. Most of the samples were collected on or near the Bikini Atoll and included plants, soil, fish, catchment water, and sediments, with emphasis on local marine and terrestrial food items. Data are presented from γ spectral analysis and the content of 90 Sr and transuranic elements in the samples

  16. Measurements of plutonium in environmental samples

    International Nuclear Information System (INIS)

    D'Alberti, F.; Risposi, L.

    1996-01-01

    Within the activities connected with the start up of the PETRA Laboratory (Processo per l'Estrazione di Terre Rare ed Attinidi, i.e. process for extraction of rare earths and actinides), the Radiation Protection Unit of the J.R.C.-Ispra has carried out a well planned set of experimental measurements aimed at evaluating the zero point of the isotopes of plutonium in environmental samples by alfa spectrometry. After the International Moratorium in 1963, no release of plutonium has occurred in the environment apart from the burn up of SNAP 9A satellite in April 1964. Since then the plutonium concentration in air and in fallout samples has been continuously decreasing requiring, therefore, optimization of both instrumentation and experimental measurement procedures in order to obtain better sensibilities. In this work, the experimental methodology followed at the J.R.C.-Ispra for measurements of plutonium concentration in air, deposition and soil is described and the plutonium behaviour in these samples is reported and discussed starting from 1961

  17. Measurements of plutonium in environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    D' Alberti, F; Risposi, L [Instituto di Fisica Applicata, University of Milan, Milan (Italy)

    1996-01-01

    Within the activities connected with the start up of the PETRA Laboratory (Processo per l'Estrazione di Terre Rare ed Attinidi, i.e. process for extraction of rare earths and actinides), the Radiation Protection Unit of the J.R.C.-Ispra has carried out a well planned set of experimental measurements aimed at evaluating the zero point of the isotopes of plutonium in environmental samples by alfa spectrometry. After the International Moratorium in 1963, no release of plutonium has occurred in the environment apart from the burn up of SNAP 9A satellite in April 1964. Since then the plutonium concentration in air and in fallout samples has been continuously decreasing requiring, therefore, optimization of both instrumentation and experimental measurement procedures in order to obtain better sensibilities. In this work, the experimental methodology followed at the J.R.C.-Ispra for measurements of plutonium concentration in air, deposition and soil is described and the plutonium behaviour in these samples is reported and discussed starting from 1961.

  18. Determination of chemical form of iodine with IC-ICP-MS system and its application to the environmental samples

    International Nuclear Information System (INIS)

    Yoshida, S.; Katou, S.; Sekimoto, H.; Muramatsu, Y.

    2005-01-01

    Iodine-129 is one of the important radionuclides possibly released into the environment from nuclear weapons testing and from the nuclear facilities such as nuclear fuel reprocessing plants. Because of its long half-life (1.57 x 10 7 y), knowing its long-term behavior in the environment is a major concern. As I-129 is expected to act together with stable iodine (I-127) in the environment after long time, the biogeochemical cycling of stable iodine in the environment can be used for the reliable safety assessment of I-129. Chemical form is the one of the important factors controlling the 'iodine behavior in the environment. Iodide (I - ) and iodate (IO 3 - ) are known to be the major chemical form in the aqueous solution. However, the information on the chemical form of iodine in the environmental sample is limited because of lack of reliable analytical technique for trace level of iodine in the environment. In this study, the analytical system by using ion chromatograph (IC) followed by inductively coupled plasma mass spectrometry (ICP-MS) was developed for the separate determination of I - and IO 3 - in the aqueous solution. The IC with anion exchange column (EXCELPAK ICS-A23) was used for the separation of I - and IO 3 - with 30 mM (NH 4 ) 2 CO 3 as eluent. Separated iodine was determined with ICP-MS on line. with the detection limit 0.1 - 1 μg/L. The total iodine concentration was also measured by the direct determination with ICP-MS. The iodine in the several environmental samples such as irrigation water in paddy field was successfully determined with information of chemical form. In incubation experiment with flooded soil, the change of the chemical form of iodine in the soil solution with change of Eh was observed. Detailed data will be discussed in the presentation.

  19. Abstracts of the 1. Brazilian Meeting on Analytical Chemistry

    International Nuclear Information System (INIS)

    Curtius, A.J.

    1982-01-01

    Abstracts from experimental studies on analytical chemistry are presented. Several techniques have been used, such as: neutron activation analysis, potentiometry, optical emission spectroscopy, alpha and gamma spectroscopy, atomic absorption spectrophotometry, radiometric analysis, fission track detection, complexometry and others. Samples analysed are of various kinds: environmental materials (soil, water, air), rocks, coal, lanthanide complexes, polycarbonates and synthetic quartz. (C.L.B.) [pt

  20. ICP-MS applications for the analysis of geological materials and environmental samples

    International Nuclear Information System (INIS)

    Bendl, J.

    1997-01-01

    This work deals with applications of inductively coupled plasma - mass spectrometry applications for the analysis of geological materials and environmental samples. There are instrumentation, calibration, alternatives of sample introduction, interferences, trace elements analysis, rare earth elements and uranium and thorium, precious metals, isotopic analysis and environmental analysis discussed

  1. Aplikasi Analytical Hierarchy Process Pada Pemilihan Metode Analisis Zat Organik Dalam Air

    Directory of Open Access Journals (Sweden)

    Dino Rimantho

    2016-07-01

    Full Text Available Water is one of the food products analyzed in water chemistry and environmental laboratories. One of the parameters analyzed are organic substances. The number of samples that were not comparable with the analytical skills can cause delays in test results. Analytical Hierarchy Process applied to evaluate the analytical methods used. Alternative methods tested include titrimetric method, spectrophotometry, and total organic carbon (TOC. Respondents consisted of deputy technical manager, laboratory coordinator, and two senior analysts. Alternative results obtained are methods of TOC. Proposed improvements alternative analytical method based on the results obtained, the method of the TOC with a 10-15 minute analysis time and use of CRM to the validity of the analysis results.

  2. Hanford transuranic analytical capability

    International Nuclear Information System (INIS)

    McVey, C.B.

    1995-01-01

    With the current DOE focus on ER/WM programs, an increase in the quantity of waste samples that requires detailed analysis is forecasted. One of the prime areas of growth is the demand for DOE environmental protocol analyses of TRU waste samples. Currently there is no laboratory capacity to support analysis of TRU waste samples in excess of 200 nCi/gm. This study recommends that an interim solution be undertaken to provide these services. By adding two glove boxes in room 11A of 222S the interim waste analytical needs can be met for a period of four to five years or until a front end facility is erected at or near the 222-S facility. The yearly average of samples is projected to be approximately 600 samples. The figure has changed significantly due to budget changes and has been downgraded from 10,000 samples to the 600 level. Until these budget and sample projection changes become firmer, a long term option is not recommended at this time. A revision to this document is recommended by March 1996 to review the long term option and sample projections

  3. A practical method for determining γ-ray full-energy peak efficiency considering coincidence-summing and self-absorption corrections for the measurement of environmental samples after the Fukushima reactor accident

    Energy Technology Data Exchange (ETDEWEB)

    Shizuma, Kiyoshi, E-mail: shizuma@hiroshima-u.ac.jp [Graduate School of Engineering, Hiroshima University, Higashi-Hiroshima 739-8527 (Japan); Oba, Yurika; Takada, Momo [Graduate School of Integrated Arts and Sciences, Hiroshima University, Higashi-Hiroshima 739-8521 (Japan)

    2016-09-15

    A method for determining the γ-ray full-energy peak efficiency at positions close to three Ge detectors and at the well port of a well-type detector was developed for measuring environmental volume samples containing {sup 137}Cs, {sup 134}Cs and {sup 40}K. The efficiency was estimated by considering two correction factors: coincidence-summing and self-absorption corrections. The coincidence-summing correction for a cascade transition nuclide was estimated by an experimental method involving measuring a sample at the far and close positions of a detector. The derived coincidence-summing correction factors were compared with those of analytical and Monte Carlo simulation methods and good agreements were obtained. Differences in the matrix of the calibration source and the environmental sample resulted in an increase or decrease of the full-energy peak counts due to the self-absorption of γ-rays in the sample. The correction factor was derived as a function of the densities of several matrix materials. The present method was applied to the measurement of environmental samples and also low-level radioactivity measurements of water samples using the well-type detector.

  4. Trace determination of 10 beta-lactam antibiotics in environmental and food samples by capillary liquid chromatography.

    Science.gov (United States)

    Bailón-Pérez, M I; García-Campaña, A M; del Olmo-Iruela, M; Gámiz-Gracia, L; Cruces-Blanco, C

    2009-11-20

    A sensitive and reliable method using capillary HPLC with UV-diode array detection (DAD) has been developed and validated for the trace determination of residues of 10 beta-lactam antibiotics of human and veterinary use, in milk, chicken meat and environmental water samples. The analytes included ampicillin, amoxicillin, penicillin V, penicillin G, cloxacillin, oxacillin, dicloxacillin, nafcillin, piperacillin and clavulanic acid. Legal levels are regulated by the EU Council regulation 2377/90 in animal edible tissues for these compounds. For food analysis, a solid-phase extraction (SPE) procedure consisting in a tandem of Oasis HLB and Alumina N cartridges was applied for off-line preconcentration and cleanup. For water analysis, the first step was only necessary. The limits of detection for the studied compounds were between 0.04-0.06 microg l(-1) for water samples and 0.80-1.40 microg l(-1) (or microg kg(-1)) in the case of foods derived from animals. Average recoveries for fortified samples at different concentration levels ranged between 82.9% and 98.2%, with relative standard deviations (RSDs) lower than 9%. The method showed the advantages of capillary HPLC for the detection of these widely applied antibiotics in different samples at very low concentration levels.

  5. Final Report on the Analytical Results for Tank Farm Samples in Support of Salt Dissolution Evaluation

    International Nuclear Information System (INIS)

    Hobbs, D.T.

    1996-01-01

    Recent processing of dilute solutions through the 2H-Evaporator system caused dissolution of salt in Tank 38H, the concentrate receipt tank. This report documents analytical results for samples taken from this evaporator system

  6. Hydrophilic-lipophilic balanced magnetic nanoparticles: preparation and application in magnetic solid-phase extraction of organochlorine pesticides and triazine herbicides in environmental water samples.

    Science.gov (United States)

    He, Zeying; Wang, Peng; Liu, Donghui; Zhou, Zhiqiang

    2014-09-01

    In this study, a novel hydrophilic-lipophilic balanced magnetic nanoparticle, magnetic poly(divinylbenzene-co-N-vinylpyrrolidone) (HLB-MPNP) was successfully synthesized and applied for the extraction and determination of triazine and organochlorine pesticides in environmental water samples. The specific ratio of two monomers, hydrophilic N-vinylpyrrolidone and lipophilic divinylbenzene, endowed the magnetic nanoparticles with hydrophilic-lipophilic balanced character, which made it capable of extracting both polar and nonpolar analytes. The experimental parameters affecting extraction efficiency, including desorption conditions, sample pH, sample volume and extraction time were investigated and optimized. Under the optimum conditions, good linearity was obtained in the range of 0.20-10 μg L(-1) for triazine herbicides and 5.0-100 ng L(-1) for organochlorine pesticides, with correlation coefficients ranging from 0.994 to 0.999. The limits of determination were between 0.048 and 0.081 μg L(-1) for triazine herbicides and 0.39 and 3.26 ng L(-1) for organochlorine pesticides. The proposed method was successfully applied in the analysis of triazine and organochlorine pesticides in environmental water samples (ground, river and reservoir). Copyright © 2014 Elsevier B.V. All rights reserved.

  7. Hanford Site Environmental Surveillance Master Sampling Schedule for Calendar Year 2005

    Energy Technology Data Exchange (ETDEWEB)

    Bisping, Lynn E.

    2005-01-19

    Environmental surveillance of the Hanford Site and surrounding areas is conducted by the Pacific Northwest National Laboratory (PNNL) for the U.S. Department of Energy (DOE). Sampling is conducted to evaluate levels of radioactive and nonradioactive pollutants in the Hanford environs. This document contains the calendar year 2005 schedules for the routine and non-routine collection of samples for the Surface Environmental Surveillance Project (SESP) and Drinking Water Monitoring Project.

  8. Radiation Target Area Sample Environmental Chamber (RTASEC), Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Payload Systems Inc. proposes the Radiation Target Area Sample Environmental Chamber (RTASEC) as an innovative approach enabling radiobiologists to investigate the...

  9. Recent bibliography on analytical and sampling problems of a PWR primary coolant Suppl. 3

    International Nuclear Information System (INIS)

    Illy, H.

    1985-03-01

    The present supplement to the bibliography on analytical and sampling problems of PWR primary coolant covers the literature published in 1984 and includes some references overlooked in the previous volumes dealing with the publications of the last 10 years. References are devided into topics characterized by the following headlines: boric acid; chloride; chlorine; carbon dioxide; general; gas analysis; hydrogen isotopes; iodine; iodide; nitrogen; noble gases and radium; ammonia; ammonium; oxygen; other elements; radiation monitoring; reactor safety; sampling; water chemistry. Under a given subject bibliographical information is listed in alphabetical order of the authors. (V.N.)

  10. Instrumental neutron activation analysis of environmental samples from a region with prevalence of population disabilities in the North Gondar, Ethiopia

    Czech Academy of Sciences Publication Activity Database

    Bitewlign, T. A.; Chaubey, A. K.; Beyene, G. A.; Melikegnaw, T. H.; Mizera, Jiří; Kameník, Jan; Krausová, Ivana; Kučera, Jan

    2017-01-01

    Roč. 311, č. 3 (2017), s. 2047-2059 ISSN 0236-5731 R&D Projects: GA ČR(CZ) GBP108/12/G108; GA MŠk LM2015056 Institutional support: RVO:61389005 ; RVO:67985891 Keywords : INAA * Noth Gondar * Ethiopia * environmental pollution * health problems * rare earth elements Subject RIV: CB - Analytical Chemistry , Separation; DD - Geochemistry (USMH-B) OBOR OECD: Analytical chemistry ; Environmental sciences (social aspects to be 5.7) (USMH-B) Impact factor: 1.282, year: 2016

  11. The uses of neutron capture γ-rays in environmental pollution measurements

    International Nuclear Information System (INIS)

    Abdel-Haleem, A.S.; Abdel-Samad, M.A.; Zaghloul, R.A.; Hassan, A.M.

    1996-01-01

    A neutron capture γ-ray spectroscopy facility using an isotopic neutron source, 252 Cf, has been installed and used for investigation of some environmental samples. The facility is designed and calibrated for measurement of the prompt γ-ray spectra due to thermal neutron capture. Qualitative analysis studies of some local environmental samples have been carried out using some developed analytical programs. The experimental results of the environmental pollutant analysis are discussed. (author)

  12. Measuring myokines with cardiovascular functions: pre-analytical variables affecting the analytical output.

    Science.gov (United States)

    Lombardi, Giovanni; Sansoni, Veronica; Banfi, Giuseppe

    2017-08-01

    In the last few years, a growing number of molecules have been associated to an endocrine function of the skeletal muscle. Circulating myokine levels, in turn, have been associated with several pathophysiological conditions including the cardiovascular ones. However, data from different studies are often not completely comparable or even discordant. This would be due, at least in part, to the whole set of situations related to the preparation of the patient prior to blood sampling, blood sampling procedure, processing and/or store. This entire process constitutes the pre-analytical phase. The importance of the pre-analytical phase is often not considered. However, in routine diagnostics, the 70% of the errors are in this phase. Moreover, errors during the pre-analytical phase are carried over in the analytical phase and affects the final output. In research, for example, when samples are collected over a long time and by different laboratories, a standardized procedure for sample collecting and the correct procedure for sample storage are acknowledged. In this review, we discuss the pre-analytical variables potentially affecting the measurement of myokines with cardiovascular functions.

  13. Examining environmental drivers of spatial variability in aflatoxin ...

    African Journals Online (AJOL)

    Examining environmental drivers of spatial variability in aflatoxin accumulation in Kenyan maize: potential utility in risk prediction models. ... however, because of high sampling cost and lack of affordable and accurate analytical methods.

  14. Arsenic, Antimony, Chromium, and Thallium Speciation in Water and Sediment Samples with the LC-ICP-MS Technique

    Directory of Open Access Journals (Sweden)

    Magdalena Jabłońska-Czapla

    2015-01-01

    Full Text Available Chemical speciation is a very important subject in the environmental protection, toxicology, and chemical analytics due to the fact that toxicity, availability, and reactivity of trace elements depend on the chemical forms in which these elements occur. Research on low analyte levels, particularly in complex matrix samples, requires more and more advanced and sophisticated analytical methods and techniques. The latest trends in this field concern the so-called hyphenated techniques. Arsenic, antimony, chromium, and (underestimated thallium attract the closest attention of toxicologists and analysts. The properties of those elements depend on the oxidation state in which they occur. The aim of the following paper is to answer the question why the speciation analytics is so important. The paper also provides numerous examples of the hyphenated technique usage (e.g., the LC-ICP-MS application in the speciation analysis of chromium, antimony, arsenic, or thallium in water and bottom sediment samples. An important issue addressed is the preparation of environmental samples for speciation analysis.

  15. Development of Radioanalytical and Microanalytical Procedures for the Determination of Actinides in Environmental Samples

    International Nuclear Information System (INIS)

    Macsik, Zsuzsanna; Vajda, Nora; Bene, Balazs; Varga, Zsolt

    2008-01-01

    A radio-analytical procedure has been developed for the simultaneous determination of actinides in swipe samples by alpha-spectrometry after the separation of the actinides by extraction chromatography. The procedure is based on the complete decomposition of the sample by destruction with microwave digestion or ashing in furnace. Actinides are separated on an extraction chromatographic column filled with TRU resin (product of Eichrom Industries Inc.). Alpha sources prepared from the separated fractions of americium, plutonium, thorium and uranium are counted by alpha spectrometry. Micro-analytical procedure is being developed for the location and identification of individual particles containing fissile material using solid state nuclear track detectors. The parameters of alpha and fission track detection have been optimized and a procedure has been elaborated to locate the particles on the sample by defining the coordinates of the tracks created by the particles on the track detector. Development of a procedure is planned to separate the located particles using micromanipulator and these particles will be examined individually by different micro- and radio-analytical techniques. (authors)

  16. Development of Radioanalytical and Microanalytical Procedures for the Determination of Actinides in Environmental Samples

    Energy Technology Data Exchange (ETDEWEB)

    Macsik, Zsuzsanna [Institute of Nuclear Techniques, Moegyetem rakpart 9, H-1111 Budapest (Hungary); Vajda, Nora [RadAnal Ltd., Bimbo ut 119/a, H-1026 Budapest (Hungary); Bene, Balazs [National Institute of Standards and Technology, Gaithersburg, MD 20899 (United States); Varga, Zsolt [Institute of Isotopes, Konkoly-Thege M. ut 29-33, H-1121 Budapest (Hungary)

    2008-07-01

    A radio-analytical procedure has been developed for the simultaneous determination of actinides in swipe samples by alpha-spectrometry after the separation of the actinides by extraction chromatography. The procedure is based on the complete decomposition of the sample by destruction with microwave digestion or ashing in furnace. Actinides are separated on an extraction chromatographic column filled with TRU resin (product of Eichrom Industries Inc.). Alpha sources prepared from the separated fractions of americium, plutonium, thorium and uranium are counted by alpha spectrometry. Micro-analytical procedure is being developed for the location and identification of individual particles containing fissile material using solid state nuclear track detectors. The parameters of alpha and fission track detection have been optimized and a procedure has been elaborated to locate the particles on the sample by defining the coordinates of the tracks created by the particles on the track detector. Development of a procedure is planned to separate the located particles using micromanipulator and these particles will be examined individually by different micro- and radio-analytical techniques. (authors)

  17. Validation of an advanced analytical procedure applied to the measurement of environmental radioactivity.

    Science.gov (United States)

    Thanh, Tran Thien; Vuong, Le Quang; Ho, Phan Long; Chuong, Huynh Dinh; Nguyen, Vo Hoang; Tao, Chau Van

    2018-04-01

    In this work, an advanced analytical procedure was applied to calculate radioactivity in spiked water samples in a close geometry gamma spectroscopy. It included MCNP-CP code in order to calculate the coincidence summing correction factor (CSF). The CSF results were validated by a deterministic method using ETNA code for both p-type HPGe detectors. It showed that a good agreement for both codes. Finally, the validity of the developed procedure was confirmed by a proficiency test to calculate the activities of various radionuclides. The results of the radioactivity measurement with both detectors using the advanced analytical procedure were received the ''Accepted'' statuses following the proficiency test. Copyright © 2018 Elsevier Ltd. All rights reserved.

  18. The application of x-ray fluorescence and diffraction to the characterization of environmental assessment samples

    International Nuclear Information System (INIS)

    Censullo, A.C.; Briden, F.E.

    1982-01-01

    Some of the results of tests on environmental assessment samples are reported on. The utility of the J.W. Criss fundamental parameters computer program is evaluated for samples in which only one standard per element was used and where the standard matrix did not strictly resemble the unknown matrix. The environmental significance of a sample is dependent not only on its elemental composition, but also on the species or phases which the elements comprise. X-ray powder diffraction may be used to advantage for speciation. Multi-phase environmental assessment samples are amenable to XRD interpretation. Some results of the application of the Joint Committee on Power Diffraction Standards computer interpretatin of typical environmental samples are discussed. They were shown to contribute to the specification of the complex samples that are encountered in environmental assessments

  19. ENVIRONMENTAL EVALUATION FOR UTILIZATION OF ASH IN SOIL STABILIZATION

    Energy Technology Data Exchange (ETDEWEB)

    David J. Hassett; Loreal V. Heebink

    2001-08-01

    The Minnesota Pollution Control Agency (MPCA) approved the use of coal ash in soil stabilization, indicating that environmental data needed to be generated. The overall project goal is to evaluate the potential for release of constituents into the environment from ash used in soil stabilization projects. Supporting objectives are: (1) To ensure sample integrity through implementation of a sample collection, preservation, and storage protocol to avoid analyte concentration or loss. (2) To evaluate the potential of each component (ash, soil, water) of the stabilized soil to contribute to environmental release of analytes of interest. (3) To use laboratory leaching methods to evaluate the potential for release of constituents to the environment. (4) To facilitate collection of and to evaluate samples from a field runoff demonstration effort. The results of this study indicated limited mobility of the coal combustion fly ash constituents in laboratory tests and the field runoff samples. The results presented support previous work showing little to negligible impact on water quality. This and past work indicates that soil stabilization is an environmentally beneficial CCB utilization application as encouraged by the U.S. Environmental Protection Agency. This project addressed the regulatory-driven environmental aspect of fly ash use for soil stabilization, but the demonstrated engineering performance and economic advantages also indicate that the use of CCBs in soil stabilization can and should become an accepted engineering option.

  20. Recommendations for sampling for prevention of hazards in civil defense. On analytics of chemical, biological and radioactive contaminations. Brief instruction for the CBRN (chemical, biological, radioactive, nuclear) sampling

    International Nuclear Information System (INIS)

    Bachmann, Udo; Biederbick, Walter; Derakshani, Nahid

    2010-01-01

    The recommendation for sampling for prevention of hazards in civil defense is describing the analytics of chemical, biological and radioactive contaminations and includes detail information on the sampling, protocol preparation and documentation procedures. The volume includes a separate brief instruction for the CBRN (chemical, biological, radioactive, nuclear) sampling.

  1. Hanford environmental analytical methods: Methods as of March 1990. Volume 3, Appendix A2-I

    Energy Technology Data Exchange (ETDEWEB)

    Goheen, S.C.; McCulloch, M.; Daniel, J.L.

    1993-05-01

    This paper from the analytical laboratories at Hanford describes the method used to measure pH of single-shell tank core samples. Sludge or solid samples are mixed with deionized water. The pH electrode used combines both a sensor and reference electrode in one unit. The meter amplifies the input signal from the electrode and displays the pH visually.

  2. Osmium in environmental samples from Northeast Sweden

    International Nuclear Information System (INIS)

    Rodushkin, Ilia; Engstroem, Emma; Soerlin, Dieke; Ponter, Christer; Baxter, Douglas C.

    2007-01-01

    Osmium (Os) concentrations and 187 Os/ 188 Os isotope abundance ratios are presented for sedimentary materials, soils, humus, plants, mushrooms, mosses and lichens collected in the vicinity of the town of Lulea, Northeast Sweden, the data for biological specimens being the first reported. Contributions from sampling and varying exposure time to the observed environmental variability were evaluated. Sedimentary materials (from both fresh and brackish water) are most elevated in radiogenic 187 Os, followed by inorganic soil horizons, mushrooms and humus. The Os isotopic compositions of plants, mosses and lichens are much less radiogenic, with mean 187 Os/ 188 Os lying within a relatively narrow 0.3-0.6 range. Significant temporal variations in Os concentrations and isotopic compositions of plant samples are attributed to integrative uptake of airborne Os with non-radiogenic composition. Measured Os concentrations in biological matrices increase in the order: small shrub leaves (blueberry and lingonberry) ≤ spruce needles ≤ mushrooms ≤ tree leaves ≤ pine needles 4 ) in the environment. Though the Os content of samples from Northeast Sweden does not differ significantly from matrix-matched international reference materials (not certified for Os) of abiotic origin, the estimates of gaseous OsO 4 concentrations are roughly an order of magnitude higher than have been reported for particle-bound Os in other studies. The pronounced spatial variations between relatively closely situated sites in mean 187 Os/ 188 Os ratios for samples of the same species (presumably with the same dominating uptake mechanism) point to the presence of different local Os sources. This study therefore demonstrates that emissions of Os from automobile catalytic converters are not the only source of contemporary environmental contamination

  3. Determination of uranium and its isotopic ratios in environmental samples

    International Nuclear Information System (INIS)

    Flues Szeles, M.S.M.

    1990-01-01

    A method for the determination of uranium and its isotopic ratios ( sup(235)U/ sup(238)U and sup(234U/ sup(238)U) is established in the present work. The method can be applied in environmental monitoring programs of uranium enrichment facilities. The proposed method is based on the alpha spectrometry technique which is applied after a purification of the sample by using an ionic exchange resin. The total yield achieved was (91 + 5)% with a precision of 5%, an accuracy of 8% and a lower limit of detection of 7,9 x 10 sup(-4)Bq. The uranium determination in samples containing high concentration of iron, which is an interfering element present in environmental samples, particularly in soil and sediment, was also studied. The results obtained by using artificial samples containing iron and uranium in the ratio 1000:1, were considered satisfactory. (author)

  4. Bee pollen as a bioindicator of environmental pesticide contamination.

    Science.gov (United States)

    de Oliveira, Renata Cabrera; Queiroz, Sonia Claudia do Nascimento; da Luz, Cynthia Fernandes Pinto; Porto, Rafael Silveira; Rath, Susanne

    2016-11-01

    Honeybees and bee products are potential bioindicators of the presence of contaminants in the environment, enabling monitoring of large areas due to the long distances travelled by bees. This work evaluates the use of bee pollen as a bioindicator of environmental contamination by pesticides. A GC-MS/MS analytical method for multiresidue determination of 26 different pesticides in pollen was developed and validated in accordance with the recommendations of the European Union SANCO guide. Environmental monitoring was conducted using the analysis of 145 pollen samples collected from ten beehives in the experimental apiary of Embrapa in Jaguariúna (São Paulo State, Brazil). Bioallethrin and pendimethalin were identified in four and eighteen samples, respectively, at concentrations below the LOQ of the method (25 ng g(-1)). Passive sampling with polyurethane foam discs was used as a control, and no pesticides were found. The detection of pesticide residues in seven samples (33%) from commercial apiaries in Ribeirão Preto (São Paulo State) confirmed the efficiency of the analytical method and the need for environmental monitoring for the presence of pesticide residues. The results demonstrated the potential of bee pollen as a bioindicator of environmental contamination by pesticides. Copyright © 2016 Elsevier Ltd. All rights reserved.

  5. A prequalifying program for evaluating the analytical performance of commercial laboratories

    International Nuclear Information System (INIS)

    Reith, C.C.; Bishop, C.T.

    1987-01-01

    Soil and water samples were spiked with known activities of radionuclides and sent to seven commercial laboratories that had expressed an interest in analyzing environmental samples for the Waste Isolation Pilot Plant (WIPP). This Prequalifying Program was part of the selection process for an analytical subcontractor for a three-year program of baseline radiological surveillance around the WIPP site. Both media were spiked at three different activity levels with several transuranic radionuclides, as well as tritium, fission products, and activation products. Laboratory performance was evaluated by calculating relative error for each radionuclide in each sample, assigning grade values, and compiling grades into report cards for each candidate. Results for the five laboratories completing the Prequalifying Program were pooled to reveal differing degrees of difficulty among the treatments and radionuclides. Interlaboratory comparisons revealed systematic errors in the performance of one candidate. The final report cards contained clear differences among overall grades for the five laboratories, enabling analytical performance to be used as a quantitative criterion in the selection of an analytical subcontractor. (author)

  6. A study on aluminum determination in environmental samples by Neutron Activation Analysis

    International Nuclear Information System (INIS)

    Noyori, Amanda

    2017-01-01

    Aluminum determinations are of great interest since this element is toxic to humans and it is widely distributed in the environment. Besides, the determinations of this element by conventional analytical methods present difficulties due to sample contamination during the analyses. Neutron activation analysis (NAA) for Al determination presents advantages of fast analyses and of high sensitivity. However, NAA of Al does present problems of P and Si nuclear reaction interferences. Aluminum is determined by measuring 28 Al, formed in the reaction 27 Al (n, γ) 28 Al, the same radioisotope formed in reactions 31 P (n, α) 28 Al and 28 Si (n, p) 28 Al. The purpose of this study was to determine Al in environmental samples by NAA correcting these interferences using correction factors, and determining P and Si concentrations in the samples. In this study, certified reference materials and biomonitor samples (tree barks and lichen) were analyzed. Experimental procedure consisted of irradiating an aliquot of the sample at the IEA-R1 nuclear research reactor together with Al standard, followed by gamma ray spectrometry. Phosphorus was determined by measuring beta radiation of 32 P using a Geiger-Müller counter. Silicon was determined by epithermal neutron activation analysis and measuring 29 Al formed in the reaction 29 Si (n, p) 29 Al. Results obtained in the determination of Al, P and Si in the certified reference materials showed good precision and accuracy with |Z-score| ≤ 2. Aluminum results in the biomonitor samples varied from to 253 to 15783 μg g -1 . In the case of P its concentrations varied from 283 to 1946 μg g -1 . Silicon determinations in biomonitors varied from 0.11 to 7.8 %. The interference contribution rates in the analyses of the biomonitor samples were of the order of 2.0 % and this contribution depends on the relation between concentrations of interfering elements and of Al in the sample. Detection limit values of Al in the biomonitor analyses

  7. Sampling and monitoring for the mine life cycle

    Science.gov (United States)

    McLemore, Virginia T.; Smith, Kathleen S.; Russell, Carol C.

    2014-01-01

    Sampling and Monitoring for the Mine Life Cycle provides an overview of sampling for environmental purposes and monitoring of environmentally relevant variables at mining sites. It focuses on environmental sampling and monitoring of surface water, and also considers groundwater, process water streams, rock, soil, and other media including air and biological organisms. The handbook includes an appendix of technical summaries written by subject-matter experts that describe field measurements, collection methods, and analytical techniques and procedures relevant to environmental sampling and monitoring.The sixth of a series of handbooks on technologies for management of metal mine and metallurgical process drainage, this handbook supplements and enhances current literature and provides an awareness of the critical components and complexities involved in environmental sampling and monitoring at the mine site. It differs from most information sources by providing an approach to address all types of mining influenced water and other sampling media throughout the mine life cycle.Sampling and Monitoring for the Mine Life Cycle is organized into a main text and six appendices that are an integral part of the handbook. Sidebars and illustrations are included to provide additional detail about important concepts, to present examples and brief case studies, and to suggest resources for further information. Extensive references are included.

  8. Portable sample preparation and analysis system for micron and sub-micron particle characterization using light scattering and absorption spectroscopy

    Science.gov (United States)

    Stark, Peter C [Los Alamos, NM; Zurek, Eduardo [Barranquilla, CO; Wheat, Jeffrey V [Fort Walton Beach, FL; Dunbar, John M [Santa Fe, NM; Olivares, Jose A [Los Alamos, NM; Garcia-Rubio, Luis H [Temple Terrace, FL; Ward, Michael D [Los Alamos, NM

    2011-07-26

    There is provided a method and device for remote sampling, preparation and optical interrogation of a sample using light scattering and light absorption methods. The portable device is a filtration-based device that removes interfering background particle material from the sample matrix by segregating or filtering the chosen analyte from the sample solution or matrix while allowing the interfering background particles to be pumped out of the device. The segregated analyte is then suspended in a diluent for analysis. The device is capable of calculating an initial concentration of the analyte, as well as diluting the analyte such that reliable optical measurements can be made. Suitable analytes include cells, microorganisms, bioparticles, pathogens and diseases. Sample matrixes include biological fluids such as blood and urine, as well as environmental samples including waste water.

  9. Ames Laboratory Site Environmental Report, Calendar year 1992

    International Nuclear Information System (INIS)

    1992-01-01

    The summarized data and conclusions from the Ames Laboratory environmental monitoring program are presented in this Annual Site Environmental Report. Pollution awareness and waste minimization programs and plans implemented in 1990 are continuing to date. Ames Laboratory (AL) is responsible for a small chemical burial site, located on ISU property. The site was used for the disposal of chemical and metal slags from thorium and uranium production. Samples of water from existing test wells, and upstream and downstream sites on the nearby Squaw Creek, have not detected migration of the buried materials off site. Surface, hand auger and deep boring soil samples have been collected from the site. The analytical results are pending, Six new monitoring wells have been installed and sampled. Analytical results are pending. Ames Laboratory is responsible for an area contaminated by diesel fuel that leaked from an underground storage tank (UST) in 1970. The tank was removed that year. Soil borings and groundwater have been analyzed for contamination and a preliminary assessment written. Nine small inactive waste sites have been identified for characterization. The NEPA review for this work resulted in a CX determination. The work plans were approved by AL and CH. A subcontractor has surveyed and sampled the sites. Analytical results are pending

  10. Application of analytic hierarchy process in mine environmental assesment-take Fuxin mines as example

    International Nuclear Information System (INIS)

    Kong Zhizhao; Jiang Xue; Dong Shuangfa; Zhao Zhao

    2012-01-01

    We taking mine environmental assessment work by analytic hierarchy process on the basis of results of remote sensing investigation in Fuxin Mines. Putting forward an assessing system consist of index, method and levels. This system makes the levels by weight percent calculated by judging matrixes. Taking Hebei Mines as an example test the system. It shows that the result by the system is credible and is reasonable. This provides a significant data for the second-mines-plan of Liaoning Province. (authors)

  11. Optimized Analytical Method to Determine Gallic and Picric Acids in Pyrotechnic Samples by Using HPLC/UV (Reverse Phase)

    International Nuclear Information System (INIS)

    Garcia Alonso, S.; Perez Pastor, R. M.

    2013-01-01

    A study on the optimization and development of a chromatographic method for the determination of gallic and picric acids in pyrotechnic samples is presented. In order to achieve this, both analytical conditions by HPLC with diode detection and extraction step of a selected sample were studied. (Author)

  12. Innovative technology summary report: Road Transportable Analytical Laboratory (RTAL)

    International Nuclear Information System (INIS)

    1998-10-01

    The Road Transportable Analytical Laboratory (RTAL) has been used in support of US Department of Energy (DOE) site and waste characterization and remediation planning at Fernald Environmental Management Project (FEMP) and is being considered for implementation at other DOE sites, including the Paducah Gaseous Diffusion Plant. The RTAL laboratory system consists of a set of individual laboratory modules deployable independently or as an interconnected group to meet each DOE site's specific analysis needs. The prototype RTAL, deployed at FEMP Operable Unit 1 Waste Pits, has been designed to be synergistic with existing analytical laboratory capabilities, thereby reducing the occurrence of unplanned rush samples that are disruptive to efficient laboratory operations

  13. Participation of the IPEN/CNEN/SP Environmental Diagnostic Division on programs of laboratory intercomparisons in environmental samples

    International Nuclear Information System (INIS)

    Cotrim, Marycel Barboza; Sato, Ivone Mulako; Salvador, Vera Lucia R.; Dantas, Elizabeth Sonoda Keiko; Cantagallo, Maria Ines; Lemes, Marcos Jose L.; Scapin, Marcos Antonio; Sisti, Cristina; Silveira, Elias Santana; Furusawa, Helio Akira; Pires, Maria Aparecida Faustino

    2003-01-01

    The present work presents the participation of the Environmental Diagnostic Division Laboratories (MQA) at the intercomparison national and international laboratories, (PI/SABESP - Interlaboratory Sao Paulo, Brazil, Program; Program for Interlaboratorial Analytic Quality Control of Metals in Water (CBM/COMETRO); Programa para La Calidad de las Mediciones Quimicas (PCQM/INTI) - Argentine, and the Commission d'Etablissement des Methodes d'Analyse, France (CETAMA/CEA). Those essay providers have using statistical tests such as the t-Student, Zscore and Cochran and Grubbs for the data evaluations. The obtained results are presented involving the analytical such as atomic absorption spectrometry: flame, graphite oven and hydride generation (AAS), emission spectrometry with induced plasma (ICP-OES), X-ray fluorescence WD-XRFS), ion chromatography and voltametry (VRA). The elements such as B, Al, K, Mg, Ca, Cr, Fe, Co, Cu, Zn and Pb, and the anions such as Cl-, NO 3 - , SO 4 2- and F - , were determined at trace level (mgL -1 ), and the elements such as Cr, As, Cd, Pb e Hg, at the trace level (μgL -1 ) in water matrices. The evaluation of analytical results, in the period 1997 to 2002, demonstrate a continuous improvement evidencing the importance of Laboratories participation at those type of exercises

  14. Bio- and chemiluminescence imaging in analytical chemistry

    International Nuclear Information System (INIS)

    Roda, Aldo; Guardigli, Massimo; Pasini, Patrizia; Mirasoli, Mara; Michelini, Elisa; Musiani, Monica

    2005-01-01

    Bio- and chemiluminescence imaging techniques combine the high sensitivity of bio- and chemiluminescence detection with the ability of current light imaging devices to localize and quantify light emission down to the single-photon level. These techniques have been successfully exploited for the development of sensitive analytical methods relying on the evaluation of the spatial distribution of the light emitted from a target sample. In this paper, we report on recent applications of bio- and chemiluminescence imaging for in vitro and in vivo assays, including: quantitative assays performed in various analytical formats, such as microtiter plates, microarrays and miniaturized analytical devices, used in the pharmaceutical, clinical, diagnostic and environmental fields; luminescence imaging microscopy based on enzymatic, immunohistochemical and in situ hybridization reactions for the localization of metabolites, enzymes, antigens and gene sequences in cells and tissues; whole-body luminescence imaging in live animals for evaluating biological and pathological processes and for pharmacological studies

  15. Green analytical chemistry introduction to chloropropanols determination at no economic and analytical performance costs?

    Science.gov (United States)

    Jędrkiewicz, Renata; Orłowski, Aleksander; Namieśnik, Jacek; Tobiszewski, Marek

    2016-01-15

    In this study we perform ranking of analytical procedures for 3-monochloropropane-1,2-diol determination in soy sauces by PROMETHEE method. Multicriteria decision analysis was performed for three different scenarios - metrological, economic and environmental, by application of different weights to decision making criteria. All three scenarios indicate capillary electrophoresis-based procedure as the most preferable. Apart from that the details of ranking results differ for these three scenarios. The second run of rankings was done for scenarios that include metrological, economic and environmental criteria only, neglecting others. These results show that green analytical chemistry-based selection correlates with economic, while there is no correlation with metrological ones. This is an implication that green analytical chemistry can be brought into laboratories without analytical performance costs and it is even supported by economic reasons. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Environmental research organizations and climate change policy analytical capacity : an assessment of the Canadian case

    International Nuclear Information System (INIS)

    Howlett, M.; Oliphant, S.

    2010-01-01

    Climate change is a topic of increasing interest to contemporary decision makers. In order for governments to make informed decisions in climate change mitigation and adaptation efforts, environmental policy makers require strong research and analytical capabilities to design and implement effective policies to deal with wide-ranging and complex policy issues. This articles presented a 7-criteria model of policy analytical capacity (PAC) and applied it to 3 prominent Canadian environmental policy research organizations. The 2 governmental organizations examined in this study were Environment Canada and the British Columbia Ministry of the Environment, while the non-government organization was the David Suzuki Foundation. Following the 7 principles that determine the PAC of an organization, each case study examined the education/training of the organization's employees; the types and mix of policy analysis techniques used by the organization; the culture and structure of decision making in the organization; the nature and source of demand for the organization's research; and the organization's access to necessary data and information to conduct work at a high level of competence. Interview data provided information on the status of each organizations' current research capacity and the effect this has on overall government policy-making capability in the face of climate change challenges. 75 refs.

  17. Environmental report 1994. Volume No. 2

    International Nuclear Information System (INIS)

    Rath, K.S.; Harrach, R.J.; Gallegos, G.M.; Failor, R.A.; Christofferson, E.

    1995-01-01

    This volume 2 of the Lawrence Livermore National Laboratory's (LLNL's) annual Environmental Report 1994 is a detailed data report that provides individual data points, where applicable, along with some summary data and more detailed accounts of sample collection and analytical methods. Six chapters have information on monitoring of air, surface water, groundwater, soil and sediment, vegetation and foodstuffs, and environmental radiation; two other chapters cover compliance sel-monitoring and quality assurance

  18. Analytical method comparisons for the accurate determination of PCBs in sediments

    Energy Technology Data Exchange (ETDEWEB)

    Numata, M.; Yarita, T.; Aoyagi, Y.; Yamazaki, M.; Takatsu, A. [National Metrology Institute of Japan, Tsukuba (Japan)

    2004-09-15

    National Metrology Institute of Japan in National Institute of Advanced Industrial Science and Technology (NMIJ/AIST) has been developing several matrix reference materials, for example, sediments, water and biological tissues, for the determinations of heavy metals and organometallic compounds. The matrix compositions of those certified reference materials (CRMs) are similar to compositions of actual samples, and those are useful for validating analytical procedures. ''Primary methods of measurements'' are essential to obtain accurate and SI-traceable certified values in the reference materials, because the methods have the highest quality of measurement. However, inappropriate analytical operations, such as incomplete extraction of analytes or crosscontamination during analytical procedures, will cause error of analytical results, even if one of the primary methods, isotope-dilution, is utilized. To avoid possible procedural bias for the certification of reference materials, we employ more than two analytical methods which have been optimized beforehand. Because the accurate determination of trace POPs in the environment is important to evaluate their risk, reliable CRMs are required by environmental chemists. Therefore, we have also been preparing matrix CRMs for the determination of POPs. To establish accurate analytical procedures for the certification of POPs, extraction is one of the critical steps as described above. In general, conventional extraction techniques for the determination of POPs, such as Soxhlet extraction (SOX) and saponification (SAP), have been characterized well, and introduced as official methods for environmental analysis. On the other hand, emerging techniques, such as microwave-assisted extraction (MAE), pressurized fluid extraction (PFE) and supercritical fluid extraction (SFE), give higher recovery yields of analytes with relatively short extraction time and small amount of solvent, by reasons of the high

  19. A pirólise como técnica analítica Pyrolysis as an analytical technique

    Directory of Open Access Journals (Sweden)

    Flaviano Oliveira Silvério

    2008-01-01

    Full Text Available In this paper historical aspects of analytical pyrolysis, the equipment used, the fundamentals and the mechanisms of pyrolysis of different polymeric materials are discussed. The latest work on analytical pyrolysis applied to various types of synthetic and natural samples is reviewed. Current applications of this technique that are discussed include identification of microorganisms, analysis of trace compounds by forensic laboratories, investigation of food and agricultural products, study of the chemical composition of wood, authentication and conservation of artworks, and the study of environmental and geochemical samples.

  20. Use of immunomagnetic separation for the detection of Desulfovibrio vulgaris from environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Chakraborty, R.; Hazen, T.C.; Joyner, D.C.; Kusel, K.; Singer, M.E.; Sitte, J.; Torok, T.

    2011-04-15

    Immunomagnetic separation (IMS) has proved highly efficient for recovering microorganisms from heterogeneous samples. Current investigation targeted the separation of viable cells of the sulfate-reducing bacterium, Desulfovibrio vulgaris. Streptavidin-coupled paramagnetic beads and biotin labeled antibodies raised against surface antigens of this microorganism were used to capture D. vulgaris cells in both bioreactor grown laboratory samples and from extremely low-biomass environmental soil and subsurface drilling samples. Initial studies on detection, recovery efficiency and viability for IMS were performed with laboratory grown D. vulgaris cells using various cell densities. Efficiency of cell isolation and recovery (i.e., release of the microbial cells from the beads following separation) was followed by microscopic imaging and acridine orange direct counts (AODC). Excellent recovery efficiency encouraged the use of IMS to capture Desulfovibrio spp. cells from low-biomass environmental samples. The environmental samples were obtained from a radionuclide-contaminated site in Germany and the chromium (VI)-contaminated Hanford site, an ongoing bioremediation project of the U.S. Department of Energy. Field deployable IMS technology may greatly facilitate environmental sampling and bioremediation process monitoring and enable transcriptomics and proteomics/metabolomics-based studies directly on cells collected from the field.

  1. Rapid and simultaneous determination of neptunium and plutonium isotopes in environmental samples by extraction chromatography using sequential injection analysis and ICP-MS

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per

    2010-01-01

    plutonium and neptunium in three reference materials were in agreement with the recommended or literature values at the 0.05 significance level. The developed method is suitable for the analysis of up to 10 g of soil and 20 g of seaweed samples. The extraction chromatographic separation within the SI system......This paper reports an automated analytical method for rapid and simultaneous determination of plutonium isotopes (239Pu and 240Pu) and neptunium (237Np) in environmental samples. An extraction chromatographic column packed with TrisKem TEVA® resin was incorporated in a sequential injection (SI...... for a single sample takes less than 1.5 h. As compared to batchwise procedures, the developed method significantly improves the analysis efficiency, reduces the labor intensity and expedites the simultaneous determination of plutonium and neptunium as demanded in emergency actions....

  2. [Detection of Cryptospordium spp. in environmental water samples by FTA-PCR].

    Science.gov (United States)

    Zhang, Xiao-Ping; Zhu, Qian; He, Yan-Yan; Jiang, Li; Jiang, Shou-Fu

    2011-02-01

    To establish a FTA-polymeras chain reaction (FTA-PCR) method in detection of Cryptospordium spp. in different sources of water. The semi automated immunomagnetic separation (IMS) of Cryptospordium oocysts in environmental water samples was performed firstly, and then genomic DNA of Cryptospordium oocysts was extracted by FTA filters disk. Oligonucleotide primers were designed based on the DNA fragment of the 18 S rRNA gene from C. parvum. Plate DNA was amplified with primers in PCR. The control DNA samples from Toxoplasma gondii,Sarcocystis suihominis, Echinococcus granulosus, and Clonorchis sinensis were amplified simultaneously. All PCR products were detected by agar electrophoresis dyed with ethidium bromide. The 446 bp fragment of DNA was detected in all samples of C. parvum, C. andersoni, and C. baileyi, while it was not detected in control groups in laboratory. No positive samples were found from 10 samples collected from tape water in 5 districts of Shanghai City by FTA-PCR. Nine positive samples were detected totally from 70 different environmental water samples, there were 0 out of 15 samples from the source of tape water, 2 out of 25 from the Huangpu River, 5 out of 15 from rivers around the animal farmers, 1 out of 9 from output water of contaminating water treatment factory, 1 out of 6 from the out gate of living contaminating water. The 446 bp fragment was detected from all the amplified positive water samples. FTA-PCR is an efficient method for gene detection of Cryptospordium oocysts, which could be used in detection of environmental water samples. The contamination degree of Cryptospordium oocysts in the river water around animal farms is high.

  3. Stability of purgeable VOCs in water samples during pre-analytical holding: Part 1, Analysis by a commercial laboratory

    Energy Technology Data Exchange (ETDEWEB)

    West, O.R.; Bayne, C.K.; Siegrist, R.L.; Holden, W.L.; Scarborough, S.S. [Oak Ridge National Lab., TN (United States); Bottrell, D.W. [USDOE, Washington, DC (United States)

    1996-10-01

    This study was undertaken to examine the hypothesis that prevalent and priority purgeable VOCs in properly preserved water samples are stable for at least 28 days. (VOCs are considered stable if concentrations do not change by more than 10%.) Surface water was spiked with 44 purgeable VOCs. Results showed that the measurement of 35 out of 44 purgeable VOCs in properly preserved water samples (4 C, 250 mg NaHSO{sub 4}, no headspace in 40 mL VOC vials with 0.010-in. Teflon-lined silicone septum caps) will not be affected by sample storage for 28 days. Larger changes (>10%) and low practical reporting times were observed for a few analytes, e.g. acrolein, CS{sub 2}, vinyl acetate, etc.; these also involve other analytical problems. Advantages of a 28-day (compared to 14-day) holding time are pointed out.

  4. User's and reference guide to the INEL RML/analytical radiochemistry sample tracking database version 1.00

    International Nuclear Information System (INIS)

    Femec, D.A.

    1995-09-01

    This report discusses the sample tracking database in use at the Idaho National Engineering Laboratory (INEL) by the Radiation Measurements Laboratory (RML) and Analytical Radiochemistry. The database was designed in-house to meet the specific needs of the RML and Analytical Radiochemistry. The report consists of two parts, a user's guide and a reference guide. The user's guide presents some of the fundamentals needed by anyone who will be using the database via its user interface. The reference guide describes the design of both the database and the user interface. Briefly mentioned in the reference guide are the code-generating tools, CREATE-SCHEMA and BUILD-SCREEN, written to automatically generate code for the database and its user interface. The appendices contain the input files used by the these tools to create code for the sample tracking database. The output files generated by these tools are also included in the appendices

  5. Glycan characterization of the NIST RM monoclonal antibody using a total analytical solution: From sample preparation to data analysis.

    Science.gov (United States)

    Hilliard, Mark; Alley, William R; McManus, Ciara A; Yu, Ying Qing; Hallinan, Sinead; Gebler, John; Rudd, Pauline M

    Glycosylation is an important attribute of biopharmaceutical products to monitor from development through production. However, glycosylation analysis has traditionally been a time-consuming process with long sample preparation protocols and manual interpretation of the data. To address the challenges associated with glycan analysis, we developed a streamlined analytical solution that covers the entire process from sample preparation to data analysis. In this communication, we describe the complete analytical solution that begins with a simplified and fast N-linked glycan sample preparation protocol that can be completed in less than 1 hr. The sample preparation includes labelling with RapiFluor-MS tag to improve both fluorescence (FLR) and mass spectral (MS) sensitivities. Following HILIC-UPLC/FLR/MS analyses, the data are processed and a library search based on glucose units has been included to expedite the task of structural assignment. We then applied this total analytical solution to characterize the glycosylation of the NIST Reference Material mAb 8761. For this glycoprotein, we confidently identified 35 N-linked glycans and all three major classes, high mannose, complex, and hybrid, were present. The majority of the glycans were neutral and fucosylated; glycans featuring N-glycolylneuraminic acid and those with two galactoses connected via an α1,3-linkage were also identified.

  6. Recent bibliography on analytical and sampling problems of a PWR primary coolant Pt. 1

    International Nuclear Information System (INIS)

    Illy, H.

    1981-12-01

    The first bibliography on analytical and sampling problems of a PWR primary coolant (KFKI Report-1980-48) was published in 1980 and it covered the literature published in the previous 8-10 years. The present supplement reviews the subsequent literature up till December 1981. It also includes some references overlooked in the first volume. The serial numbers are continued from the first bibliography. (author)

  7. Osmium in environmental samples from Northeast Sweden

    Energy Technology Data Exchange (ETDEWEB)

    Rodushkin, Ilia [Division of Applied Geology, Lulea University of Technology, S-971 87 Lulea (Sweden); ALS Laboratory Group, ALS Analytica AB, Aurorum 10, S-977 75 Lulea (Sweden)], E-mail: ilia.rodushkin@alsglobal.com; Engstroem, Emma [Division of Applied Geology, Lulea University of Technology, S-971 87 Lulea (Sweden); Soerlin, Dieke; Ponter, Christer; Baxter, Douglas C. [ALS Laboratory Group, ALS Analytica AB, Aurorum 10, S-977 75 Lulea (Sweden)

    2007-11-01

    Osmium (Os) concentrations and {sup 187}Os/{sup 188}Os isotope abundance ratios are presented for sedimentary materials, soils, humus, plants, mushrooms, mosses and lichens collected in the vicinity of the town of Lulea, Northeast Sweden, the data for biological specimens being the first reported. Contributions from sampling and varying exposure time to the observed environmental variability were evaluated. Sedimentary materials (from both fresh and brackish water) are most elevated in radiogenic {sup 187}Os, followed by inorganic soil horizons, mushrooms and humus. The Os isotopic compositions of plants, mosses and lichens are much less radiogenic, with mean {sup 187}Os/{sup 188}Os lying within a relatively narrow 0.3-0.6 range. Significant temporal variations in Os concentrations and isotopic compositions of plant samples are attributed to integrative uptake of airborne Os with non-radiogenic composition. Measured Os concentrations in biological matrices increase in the order: small shrub leaves (blueberry and lingonberry) {<=} spruce needles {<=} mushrooms {<=} tree leaves {<=} pine needles < mosses << lichens. The concentrations found in three different species of plant were used to provide the first estimates of gaseous osmium tetroxide (OsO{sub 4}) in the environment. Though the Os content of samples from Northeast Sweden does not differ significantly from matrix-matched international reference materials (not certified for Os) of abiotic origin, the estimates of gaseous OsO{sub 4} concentrations are roughly an order of magnitude higher than have been reported for particle-bound Os in other studies. The pronounced spatial variations between relatively closely situated sites in mean {sup 187}Os/{sup 188}Os ratios for samples of the same species (presumably with the same dominating uptake mechanism) point to the presence of different local Os sources. This study therefore demonstrates that emissions of Os from automobile catalytic converters are not the only

  8. 8. Latin American Symposium on Environmental and Sanitary Analytical Chemistry: abstracts

    International Nuclear Information System (INIS)

    2009-01-01

    The rapid changes and development of world economy, incidental to continued growth in consumption of industrial goods, continue presenting biological and biochemical interactions unsuspected or underestimated. This has imposed increasing challenges in the study of the effects on human health and environmental, vital issues that affect all citizens of the planet and the biota in general, but have not yet been sufficiently studied or well understood. Stringent criteria are needed to determine the impacts on health, long-term, of technical and chemical inventions today. This movement has received support from consumers and politicians, in the case of the European Union, the largest common market in the world. Large employers already know that it is necessary to develop the new green technology and its controls, if they are to survive in the global economy of a future that is next. The countries of the great region of Latin America have presented a specific weight very noticeable on the world community and have not been independent of the process generalized and they also correspond to scientifically scrutinize the environmental interactive phenomena to deal with possible negative consequences, give solutions and options satisfactory to their leaders and its population. The scientific program included new techniques, qualitative and quantitative, applied to the determination of substances and microorganisms in organisms and ecosystems. The evaluation of the effects of pollution on the environment has been focused so, as the development of standards for pollution control and various activities related to the study and solution of environmental problems facing the area. Abstracts of oral presentations and posters that were presented at the 8th Latin American Symposium on Environmental Analytical Chemistry and Health were included in this compendium. (author) [es

  9. Environmental Monitoring Plan, Revision 5

    Energy Technology Data Exchange (ETDEWEB)

    Gallegos, G M; Blake, R G; Bertoldo, N A; Campbell, C G; Coty, J; Folks, K; Grayson, A R; Jones, H E; Nelson, J C; Revelli, M A; Wegrecki, T; Williams, R A; Wilson, K

    2010-01-27

    The purpose of environmental monitoring is to promote the early identification of, and response to, potential adverse environmental impacts associated with Lawrence Livermore National Laboratory (LLNL) operations. Environmental monitoring supports the Integrated Safety Management System (ISMS), International Organization for Standardization (ISO) 14001 Environmental Management Systems standard, and U. S. Department of Energy (DOE) Order 450.1A, Environmental Protection Program. Specifically, in conformance with DOE Order 450.1A, Attachment 1, paragraph 1(b)(5), environmental monitoring enables LLNL to detect, characterize, and respond to releases from LLNL activities; assess impacts; estimate dispersal patterns in the environment; characterize the pathways of exposure to members of the public; characterize the exposures and doses to individuals and to the population; and to evaluate the potential impacts to the biota in the vicinity of LLNL. Environmental monitoring also serves to demonstrate compliance with permits and other regulatory requirements. The Environmental Monitoring Plan (EMP) addresses the sample collection and analytical work supporting environmental monitoring to ensure the following: (1) A consistent system for collecting, assessing, and documenting environmental data of known and documented quality. (2) A validated and consistent approach for sampling and analysis of samples to ensure laboratory data meets program-specific needs and requirements within the framework of a performance-based approach for analytical laboratory work. (3) An integrated sampling approach to avoid duplicative data collection. Until its cancellation in January 2003, DOE Order 5400.1 required the preparation of an environmental monitoring plan. Neither DOE Order 450.1A nor the ISO 14001 standard are as prescriptive as DOE Order 5400.1, in that neither expressly requires an EMP. However, LLNL continues to prepare the EMP because it provides an organizational framework for

  10. Visualizing data for environmental analysis

    International Nuclear Information System (INIS)

    Benson, J.

    1997-01-01

    The Environmental Restoration Project at Los Alamos National Laboratory (LANL) has over 11,000 sampling locations in a 44 square mile area. The sample analyses contain raw analytical chemistry values for over 2,300 analytes and compounds used to define and remediate contaminated areas at LANL. The data consist of 2.5 million records in an oracle database. Maps are often used to visualize the data. Problems arise when a client specifies a particular kind of map without fully understanding the limitations of the data or the map. The ability of maps to convey information is dependent on many factors, though all maps are data dependent. The quantity, spatial distribution, and numerical range of the data can limit use with certain kinds of maps. To address these issues and educate the clients, several types of statistical maps (e.g., choropleth, isarithm, and graduated symbol such as bubble and spike) used for environmental analysis were chosen to show the advantages, disadvantages, and data limitations of each. By examining both the complexity of the analytical data and the limitations of the map type, it is possible to consider how reality has been transformed through the map, and if that transformation accurately conveys the information present

  11. Visualizing data for environmental analysis

    Energy Technology Data Exchange (ETDEWEB)

    Benson, J.

    1997-04-01

    The Environmental Restoration Project at Los Alamos National Laboratory (LANL) has over 11,000 sampling locations in a 44 square mile area. The sample analyses contain raw analytical chemistry values for over 2,300 analytes and compounds used to define and remediate contaminated areas at LANL. The data consist of 2.5 million records in an oracle database. Maps are often used to visualize the data. Problems arise when a client specifies a particular kind of map without fully understanding the limitations of the data or the map. The ability of maps to convey information is dependent on many factors, though all maps are data dependent. The quantity, spatial distribution, and numerical range of the data can limit use with certain kinds of maps. To address these issues and educate the clients, several types of statistical maps (e.g., choropleth, isarithm, and graduated symbol such as bubble and spike) used for environmental analysis were chosen to show the advantages, disadvantages, and data limitations of each. By examining both the complexity of the analytical data and the limitations of the map type, it is possible to consider how reality has been transformed through the map, and if that transformation accurately conveys the information present.

  12. Applications of nuclear analytical techniques to environmental studies

    International Nuclear Information System (INIS)

    Freitas, M.C.; Marques, A.P.; Reis, M.A.; Pacheco, A.M.G.; Barros, L.I.C.

    2001-01-01

    A few examples of application of nuclear-analytical techniques to biological monitors - natives and transplants - are given herein. Parmelia sulcata Taylor transplants were set up in a heavily industrialized area of Portugal - the Setubal peninsula, about 50 km south of Lisbon - where indigenous lichens are rare. The whole area was 10x15 km around an oil-fired power station, and a 2.5x2.5 km grid was used. In north-western Portugal, native thalli of the same epiphytes (Parmelia spp., mostly Parmelia sulcata Taylor) and bark from olive trees (Olea europaea) were sampled across an area of 50x50 km, using a 10x10 km grid. This area is densely populated and features a blend of rural, urban-industrial and coastal environments, together with the country's second-largest metro area (Porto). All biomonitors have been analyzed by INAA and PIXE. Results were put through nonparametric tests and factor analysis for trend significance and emission sources, respectively

  13. An Optimized Method for Quantification of Pathogenic Leptospira in Environmental Water Samples.

    Science.gov (United States)

    Riediger, Irina N; Hoffmaster, Alex R; Casanovas-Massana, Arnau; Biondo, Alexander W; Ko, Albert I; Stoddard, Robyn A

    2016-01-01

    Leptospirosis is a zoonotic disease usually acquired by contact with water contaminated with urine of infected animals. However, few molecular methods have been used to monitor or quantify pathogenic Leptospira in environmental water samples. Here we optimized a DNA extraction method for the quantification of leptospires using a previously described Taqman-based qPCR method targeting lipL32, a gene unique to and highly conserved in pathogenic Leptospira. QIAamp DNA mini, MO BIO PowerWater DNA and PowerSoil DNA Isolation kits were evaluated to extract DNA from sewage, pond, river and ultrapure water samples spiked with leptospires. Performance of each kit varied with sample type. Sample processing methods were further evaluated and optimized using the PowerSoil DNA kit due to its performance on turbid water samples and reproducibility. Centrifugation speeds, water volumes and use of Escherichia coli as a carrier were compared to improve DNA recovery. All matrices showed a strong linearity in a range of concentrations from 106 to 10° leptospires/mL and lower limits of detection ranging from Leptospira in environmental waters (river, pond and sewage) which consists of the concentration of 40 mL samples by centrifugation at 15,000×g for 20 minutes at 4°C, followed by DNA extraction with the PowerSoil DNA Isolation kit. Although the method described herein needs to be validated in environmental studies, it potentially provides the opportunity for effective, timely and sensitive assessment of environmental leptospiral burden.

  14. Superhydrophobic analyte concentration utilizing colloid-pillar array SERS substrates.

    Science.gov (United States)

    Wallace, Ryan A; Charlton, Jennifer J; Kirchner, Teresa B; Lavrik, Nickolay V; Datskos, Panos G; Sepaniak, Michael J

    2014-12-02

    The ability to detect a few molecules present in a large sample is of great interest for the detection of trace components in both medicinal and environmental samples. Surface enhanced Raman spectroscopy (SERS) is a technique that can be utilized to detect molecules at very low absolute numbers. However, detection at trace concentration levels in real samples requires properly designed delivery and detection systems. The following work involves superhydrophobic surfaces that have as a framework deterministic or stochastic silicon pillar arrays formed by lithographic or metal dewetting protocols, respectively. In order to generate the necessary plasmonic substrate for SERS detection, simple and flow stable Ag colloid was added to the functionalized pillar array system via soaking. Native pillars and pillars with hydrophobic modification are used. The pillars provide a means to concentrate analyte via superhydrophobic droplet evaporation effects. A ≥ 100-fold concentration of analyte was estimated, with a limit of detection of 2.9 × 10(-12) M for mitoxantrone dihydrochloride. Additionally, analytes were delivered to the surface via a multiplex approach in order to demonstrate an ability to control droplet size and placement for scaled-up uses in real world applications. Finally, a concentration process involving transport and sequestration based on surface treatment selective wicking is demonstrated.

  15. A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

    Science.gov (United States)

    Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

    2013-01-01

    A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

  16. Radionuclides concentration in marine environmental samples along the coast of Vietnam

    International Nuclear Information System (INIS)

    Nguyen Trong Ngo; Nguyen Thanh Binh; Nguyen Van Phuc; Le Nhu Sieu; Truong Y; Mai Thi Huong; Nguyen Thi Linh; Nguyen Mong Sinh; Phan Son Hai; Le Ngoc Chung; Dang Duc Nhan; Nguyen Quang Long; Nguyen Hao Quang; Tran Tuyet Mai

    2009-01-01

    Studies on radioactivity inventories in environmental samples are necessary as they will serve as baseline data for assessing any environmental impact usage of nuclear-based activities. Approximately 700 data on 238 U, 232 Th, 226 Ra, 90 Sr, 137 Cs, 239,240 Pu activity concentrations in 150 samples i.e. sea water, sediment, fish, mollusc, crustaceans, oyster and weeds samples collected from 7 various locations in Vietnam (Hai Phong, Nghe An, Khanh Hoa, Ninh Thuan, Binh Thuan, Vung Tau, Tien Giang) throughout 1999-2008 are summarised and presented in this paper. Generally, the levels of artificial radionuclides in the studied marine environmental samples are lower as compared to other Asia-Pacific countries while naturally occurred radionuclides activity concentrations obtained were found to be in accordance with respective data from other studies within Pacific region. The radionuclides bioaccumulation factors studied in Red laver and oyster were mostly found to be high; therefore, further reinvestigation should be done for these biota that will be used as bio-fingerprint indicators in monitoring the marine environment from nuclear-based pollutions. The data set obtained from this study is available to the Asia-Pacific Marine Radioactivity Database. (author)

  17. Extraction of fullerenes from environmental matrices as affected by solvent characteristics and analyte concentration.

    Science.gov (United States)

    Place, Benjamin J; Kleber, Markus; Field, Jennifer A

    2013-03-01

    Fullerenes possess unique chemical properties that make the isolation of these compounds from heterogeneous environmental matrices difficult. For example, previous reports indicate that toluene-based extraction techniques vary in their ability to extract C60, especially from highly carbonaceous solid matrices. Here, we examined the effects of (i) solvent type (toluene alone versus an 80:20 v/v mixture of toluene and 1-methylnaphthalene) and (ii) analyte concentration on the extraction efficiency of an isotopically labeled surrogate compound, (13)C60. The toluene/1-methylnaphthalene mixture increased fullerene extraction efficiency from carbon lampblack by a factor of five, but was not significantly different from 100% toluene when applied to wood stove soot or montmorillonite. Recovery of the (13)C60 surrogate declined with decreasing analyte concentration. The usefulness of isotopically labeled surrogate is demonstrated and the study provides a quantitative assessment regarding the dependence of fullerene extraction efficiencies on the geochemical characteristics of solid matrices. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Analytical quality control service programme, intercomparison runs, certified reference materials, reference materials 1987-88

    International Nuclear Information System (INIS)

    1986-12-01

    The purpose of the Analytical Quality Control Services (AQCS) programme provided by the IAEA, is to assist laboratories engaged in the analysis of nuclear, environmental, biological, and materials of marine origin for radionuclide, major, minor and trace elements, as well as stable isotopes using atomic and nuclear analytical techniques, to check the quality of their work. The tables give details of the intercomparison samples and reference materials distributed by the IAEA in the period 1987 to 1988. 2 tabs

  19. An analytical method for trifluoroacetic Acid in water and air samples using headspace gas chromatographic determination of the methyl ester.

    Science.gov (United States)

    Zehavi, D; Seiber, J N

    1996-10-01

    An analytical method has been developed for the determination of trace levels of trifluoroacetic acid (TFA), an atmospheric breakdown product of several of the hydrofluorocarbon (HFC) and hydrochlorofluorocarbon (HCFC) replacements for the chlorofluorocarbon (CFC) refrigerants, in water and air. TFA is derivatized to the volatile methyl trifluoroacetate (MTFA) and determined by automated headspace gas chromatography (HSGC) with electron-capture detection or manual HSGC using GC/MS in the selected ion monitoring (SIM) mode. The method is based on the reaction of an aqueous sample containing TFA with dimethyl sulfate (DMS) in concentrated sulfuric acid in a sealed headspace vial under conditions favoring distribution of MTFA to the vapor phase. Water samples are prepared by evaporative concentration, during which TFA is retained as the anion, followed by extraction with diethyl ether of the acidified sample and then back-extraction of TFA (as the anion) in aqueous bicarbonate solution. The extraction step is required for samples with a relatively high background of other salts and organic materials. Air samples are collected in sodium bicarbonate-glycerin-coated glass denuder tubes and prepared by rinsing the denuder contents with water to form an aqueous sample for derivatization and analysis. Recoveries of TFA from spiked water, with and without evaporative concentration, and from spiked air were quantitative, with estimated detection limits of 10 ng/mL (unconcentrated) and 25 pg/mL (concentrated 250 mL:1 mL) for water and 1 ng/m(3) (72 h at 5 L/min) for air. Several environmental air, fogwater, rainwater, and surface water samples were successfully analyzed; many showed the presence of TFA.

  20. An overview of sample preparation procedures for LC-MS multiclass antibiotic determination in environmental and food samples.

    Science.gov (United States)

    Moreno-Bondi, María Cruz; Marazuela, María Dolores; Herranz, Sonia; Rodriguez, Erika

    2009-10-01

    Antibiotics are a class of pharmaceuticals that are of great interest due to the large volumes of these substances that are consumed in both human and veterinary medicine, and due to their status as the agents responsible for bacterial resistance. They can be present in foodstuffs and in environmental samples as multicomponent chemical mixtures that exhibit a wide range of mechanisms of action. Moreover, they can be transformed into different metabolites by the action of microorganisms, as well as by other physical or chemical means, resulting in mixtures with higher ecotoxicities and risks to human health than those of the individual compounds. Therefore, there is growing interest in the availability of multiclass methods for the analysis of antimicrobial mixtures in environmental and food samples at very low concentrations. Liquid chromatography (LC) has become the technique of choice for multiclass analysis, especially when coupled to mass spectrometry (LC-MS) and tandem MS (LC-MS(2)). However, due to the complexity of the matrix, in most cases an extraction step for sample clean-up and preconcentration is required before analysis in order to achieve the required sensitivities. This paper reviews the most recent developments and applications of multiclass antimicrobial determination in environmental and food matrices, emphasizing the practical aspects of sample preparation for the simultaneous extraction of antimicrobials from the selected samples. Future trends in the application of LC-MS-based techniques to multiclass antibiotic analysis are also presented.