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Sample records for preparing soil samples

  1. Preparation and application of radioactive soil samples for intercomparison

    International Nuclear Information System (INIS)

    Gao Zequan; Li Zhou; Li Pengxiang; Wang Ruijun; Ren Xiaona

    2014-01-01

    This article summarized the preparation process and intercomparison results of the simulated environmental radioactive soil samples. The components of the matrix were: SiO 2 , Al 2 O 3 , Fe 2 O 3 , MgO, CaO, NaCl, KCl and TiO 2 . All of the components were milled, oven-dried, sieved and then blended together. The homogeneity test was according to GB 15000. 5-1994, and no significant differences were observed. The 3 H analysis soils were spiked natural soils with the moisture content of 15%. Eight laboratories attended this intercomparison. The results proves that the preparation of the simulated soils were suitable for the inter-laboratories comparison. (authors)

  2. Soil sample preparation using microwave digestion for uranium analysis

    International Nuclear Information System (INIS)

    Mohagheghi, Amir H.; Preston, Rose; Akbarzadeh, Mansoor; Bakthiar, Steven

    2000-01-01

    A new sample preparation procedure has been developed for digestion of soil samples for uranium analysis. The technique employs a microwave oven digestion system to digest the sample and to prepare it for separation chemistry and analysis. The method significantly reduces the volume of acids used, eliminates a large fraction of acid vapor emissions, and speeds up the analysis time. The samples are analyzed by four separate techniques: Gamma Spectrometry, Alpha Spectroscopy using the open digestion method, Kinetic Phosphorescence Analysis (KPA) using open digestion, and KPA by Microwave digestion technique. The results for various analytical methods are compared and used to confirm the validity of the new procedure. The details of the preparation technique along with its benefits are discussed

  3. Atomic absorption determination of metals in soils using ultrasonic sample preparation

    International Nuclear Information System (INIS)

    Chmilenko, F.A.; Smityuk, N.M.; Baklanov, A.N.

    2002-01-01

    It was shown that ultrasonic treatment accelerates sample preparation of soil extracts from chernozem into different solvents by a factor of 6 to 60. These extracts are used for the atomic absorption determination of soluble species of Cd, Co, Cr, Cu, Ni, Pb, and Zn. The optimum ultrasound parameters (frequency, intensity, and treatment time) were found for preparing soil extracts containing analytes in concentrations required in agrochemical procedures. Different extractants used to extract soluble heavy metals from soils of an ordinary chernozem type in agrochemical procedures using ultrasonic treatment were classified in accordance with the element nature [ru

  4. Review of sample preparation techniques for the analysis of pesticide residues in soil.

    Science.gov (United States)

    Tadeo, José L; Pérez, Rosa Ana; Albero, Beatriz; García-Valcárcel, Ana I; Sánchez-Brunete, Consuelo

    2012-01-01

    This paper reviews the sample preparation techniques used for the analysis of pesticides in soil. The present status and recent advances made during the last 5 years in these methods are discussed. The analysis of pesticide residues in soil requires the extraction of analytes from this matrix, followed by a cleanup procedure, when necessary, prior to their instrumental determination. The optimization of sample preparation is a very important part of the method development that can reduce the analysis time, the amount of solvent, and the size of samples. This review considers all aspects of sample preparation, including extraction and cleanup. Classical extraction techniques, such as shaking, Soxhlet, and ultrasonic-assisted extraction, and modern techniques like pressurized liquid extraction, microwave-assisted extraction, solid-phase microextraction and QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) are reviewed. The different cleanup strategies applied for the purification of soil extracts are also discussed. In addition, the application of these techniques to environmental studies is considered.

  5. Soil and Water – What is Detectable through Microbiological Sample Preparation Techniques

    Science.gov (United States)

    The concerns of a potential terrorist’s use of biological agents in soil and ground water are articulated by comparisons to major illnesses in this Country involving contaminated drinking water sources. Objectives are focused on the importance of sample preparation in the rapid, ...

  6. Miniaturized Sample Preparation and Rapid Detection of Arsenite in Contaminated Soil Using a Smartphone

    Directory of Open Access Journals (Sweden)

    Mohd Farhan Siddiqui

    2018-03-01

    Full Text Available Conventional methods for analyzing heavy metal contamination in soil and water generally require laboratory equipped instruments, complex procedures, skilled personnel and a significant amount of time. With the advancement in computing and multitasking performances, smartphone-based sensors potentially allow the transition of the laboratory-based analytical processes to field applicable, simple methods. In the present work, we demonstrate the novel miniaturized setup for simultaneous sample preparation and smartphone-based optical sensing of arsenic As(III in the contaminated soil. Colorimetric detection protocol utilizing aptamers, gold nanoparticles and NaCl have been optimized and tested on the PDMS-chip to obtain the high sensitivity with the limit of detection of 0.71 ppm (in the sample and a correlation coefficient of 0.98. The performance of the device is further demonstrated through the comparative analysis of arsenic-spiked soil samples with standard laboratory method, and a good agreement with a correlation coefficient of 0.9917 and the average difference of 0.37 ppm, are experimentally achieved. With the android application on the device to run the experiment, the whole process from sample preparation to detection is completed within 3 hours without the necessity of skilled personnel. The approximate cost of setup is estimated around 1 USD, weight 55 g. Therefore, the presented method offers the simple, rapid, portable and cost-effective means for onsite sensing of arsenic in soil. Combined with the geometric information inside the smartphones, the system will allow the monitoring of the contamination status of soils in a nation-wide manner.

  7. Miniaturized Sample Preparation and Rapid Detection of Arsenite in Contaminated Soil Using a Smartphone.

    Science.gov (United States)

    Siddiqui, Mohd Farhan; Kim, Soocheol; Jeon, Hyoil; Kim, Taeho; Joo, Chulmin; Park, Seungkyung

    2018-03-04

    Conventional methods for analyzing heavy metal contamination in soil and water generally require laboratory equipped instruments, complex procedures, skilled personnel and a significant amount of time. With the advancement in computing and multitasking performances, smartphone-based sensors potentially allow the transition of the laboratory-based analytical processes to field applicable, simple methods. In the present work, we demonstrate the novel miniaturized setup for simultaneous sample preparation and smartphone-based optical sensing of arsenic As(III) in the contaminated soil. Colorimetric detection protocol utilizing aptamers, gold nanoparticles and NaCl have been optimized and tested on the PDMS-chip to obtain the high sensitivity with the limit of detection of 0.71 ppm (in the sample) and a correlation coefficient of 0.98. The performance of the device is further demonstrated through the comparative analysis of arsenic-spiked soil samples with standard laboratory method, and a good agreement with a correlation coefficient of 0.9917 and the average difference of 0.37 ppm, are experimentally achieved. With the android application on the device to run the experiment, the whole process from sample preparation to detection is completed within 3 hours without the necessity of skilled personnel. The approximate cost of setup is estimated around 1 USD, weight 55 g. Therefore, the presented method offers the simple, rapid, portable and cost-effective means for onsite sensing of arsenic in soil. Combined with the geometric information inside the smartphones, the system will allow the monitoring of the contamination status of soils in a nation-wide manner.

  8. Collection and preparation of samples for gamma spectrometry

    International Nuclear Information System (INIS)

    Pan Jingquan

    1994-01-01

    The paper presents the basic principles of sample collection and preparation: setting up unified sampling program, methods and procedures, sample packing, transportation and storage, determination of sample quantity, sample pretreatment and preparation of samples to be analysed, etc. for gamma spectrometry. And the paper also describes briefly the main methods and special issues of sampling and preparation for the same environmental and biological samples, such as, air, water, grass, soil and foods

  9. Effort versus Reward: Preparing Samples for Fungal Community Characterization in High-Throughput Sequencing Surveys of Soils.

    Directory of Open Access Journals (Sweden)

    Zewei Song

    Full Text Available Next generation fungal amplicon sequencing is being used with increasing frequency to study fungal diversity in various ecosystems; however, the influence of sample preparation on the characterization of fungal community is poorly understood. We investigated the effects of four procedural modifications to library preparation for high-throughput sequencing (HTS. The following treatments were considered: 1 the amount of soil used in DNA extraction, 2 the inclusion of additional steps (freeze/thaw cycles, sonication, or hot water bath incubation in the extraction procedure, 3 the amount of DNA template used in PCR, and 4 the effect of sample pooling, either physically or computationally. Soils from two different ecosystems in Minnesota, USA, one prairie and one forest site, were used to assess the generality of our results. The first three treatments did not significantly influence observed fungal OTU richness or community structure at either site. Physical pooling captured more OTU richness compared to individual samples, but total OTU richness at each site was highest when individual samples were computationally combined. We conclude that standard extraction kit protocols are well optimized for fungal HTS surveys, but because sample pooling can significantly influence OTU richness estimates, it is important to carefully consider the study aims when planning sampling procedures.

  10. Protocol for Cohesionless Sample Preparation for Physical Experimentation

    Science.gov (United States)

    2016-05-01

    Standard test method for consolidated drained triaxial compression test for soils . In Annual book of ASTM standards. West Conshohocken, PA: ASTM...derived wherein uncertainties and laboratory scatter associated with soil fabric-behavior variance during sample preparation are mitigated. Samples of...wherein comparable analysis between different laboratory tests’ results can be made by ensuring a comparable soil fabric prior to laboratory testing

  11. Supporting Sampling and Sample Preparation Tools for Isotope and Nuclear Analysis

    International Nuclear Information System (INIS)

    2016-03-01

    Nuclear and related techniques can help develop climate-smart agricultural practices by optimizing water and nutrient use efficiency, assessing organic carbon sequestration in soil, and assisting in the evaluation of soil erosion control measures. Knowledge on the behaviour of radioactive materials in soil, water and foodstuffs is also essential in enhancing nuclear emergency preparedness and response. Appropriate sampling and sample preparation are the first steps to ensure the quality and effective use of the measurements and this publication provides comprehensive detail on the necessary steps

  12. Innovative methods for inorganic sample preparation

    Energy Technology Data Exchange (ETDEWEB)

    Essling, A.M.; Huff, E.A.; Graczyk, D.G.

    1992-04-01

    Procedures and guidelines are given for the dissolution of a variety of selected materials using fusion, microwave, and Parr bomb techniques. These materials include germanium glass, corium-concrete mixtures, and zeolites. Emphasis is placed on sample-preparation approaches that produce a single master solution suitable for complete multielement characterization of the sample. In addition, data are presented on the soil microwave digestion method approved by the Environmental Protection Agency (EPA). Advantages and disadvantages of each sample-preparation technique are summarized.

  13. Innovative methods for inorganic sample preparation

    International Nuclear Information System (INIS)

    Essling, A.M.; Huff, E.A.; Graczyk, D.G.

    1992-04-01

    Procedures and guidelines are given for the dissolution of a variety of selected materials using fusion, microwave, and Parr bomb techniques. These materials include germanium glass, corium-concrete mixtures, and zeolites. Emphasis is placed on sample-preparation approaches that produce a single master solution suitable for complete multielement characterization of the sample. In addition, data are presented on the soil microwave digestion method approved by the Environmental Protection Agency (EPA). Advantages and disadvantages of each sample-preparation technique are summarized

  14. Standard methods for sampling and sample preparation for gamma spectroscopy

    International Nuclear Information System (INIS)

    Taskaeva, M.; Taskaev, E.; Nikolov, P.

    1993-01-01

    The strategy for sampling and sample preparation is outlined: necessary number of samples; analysis and treatment of the results received; quantity of the analysed material according to the radionuclide concentrations and analytical methods; the minimal quantity and kind of the data needed for making final conclusions and decisions on the base of the results received. This strategy was tested in gamma spectroscopic analysis of radionuclide contamination of the region of Eleshnitsa Uranium Mines. The water samples was taken and stored according to the ASTM D 3370-82. The general sampling procedures were in conformity with the recommendations of ISO 5667. The radionuclides was concentrated by coprecipitation with iron hydroxide and ion exchange. The sampling of soil samples complied with the rules of ASTM C 998, and their sample preparation - with ASTM C 999. After preparation the samples were sealed hermetically and measured. (author)

  15. Prompt Gamma Ray Analysis of Soil Samples

    Energy Technology Data Exchange (ETDEWEB)

    Naqvi, A.A.; Khiari, F.Z.; Haseeb, S.M.A.; Hussein, Tanvir; Khateeb-ur-Rehman [Department of Physics, King Fahd University of Petroleum and Minerals, Dhahran (Saudi Arabia); Isab, A.H. [Department of Chemistry, King Fahd University of Petroleum and Minerals, Dhahran (Saudi Arabia)

    2015-07-01

    Neutron moderation effects were measured in bulk soil samples through prompt gamma ray measurements from water and benzene contaminated soil samples using 14 MeV neutron inelastic scattering. The prompt gamma rays were measured using a cylindrical 76 mm x 76 mm (diameter x height) LaBr{sub 3}:Ce detector. Since neutron moderation effects strongly depend upon hydrogen concentration of the sample, for comparison purposes, moderation effects were studied from samples containing different hydrogen concentrations. The soil samples with different hydrogen concentration were prepared by mixing soil with water as well as benzene in different weight proportions. Then, the effects of increasing water and benzene concentrations on the yields of hydrogen, carbon and silicon prompt gamma rays were measured. Moderation effects are more pronounced in soil samples mixed with water as compared to those from soil samples mixed with benzene. This is due to the fact that benzene contaminated soil samples have about 30% less hydrogen concentration by weight than the water contaminated soil samples. Results of the study will be presented. (authors)

  16. Performance evaluation soil samples utilizing encapsulation technology

    Science.gov (United States)

    Dahlgran, James R.

    1999-01-01

    Performance evaluation soil samples and method of their preparation using encapsulation technology to encapsulate analytes which are introduced into a soil matrix for analysis and evaluation by analytical laboratories. Target analytes are mixed in an appropriate solvent at predetermined concentrations. The mixture is emulsified in a solution of polymeric film forming material. The emulsified solution is polymerized to form microcapsules. The microcapsules are recovered, quantitated and introduced into a soil matrix in a predetermined ratio to form soil samples with the desired analyte concentration.

  17. 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...

  18. Procedures for sampling radium-contaminated soils

    International Nuclear Information System (INIS)

    Fleischhauer, H.L.

    1985-10-01

    Two procedures for sampling the surface layer (0 to 15 centimeters) of radium-contaminated soil are recommended for use in remedial action projects. Both procedures adhere to the philosophy that soil samples should have constant geometry and constant volume in order to ensure uniformity. In the first procedure, a ''cookie cutter'' fashioned from pipe or steel plate, is driven to the desired depth by means of a slide hammer, and the sample extracted as a core or plug. The second procedure requires use of a template to outline the sampling area, from which the sample is obtained using a trowel or spoon. Sampling to the desired depth must then be performed incrementally. Selection of one procedure over the other is governed primarily by soil conditions, the cookie cutter being effective in nongravelly soils, and the template procedure appropriate for use in both gravelly and nongravelly soils. In any event, a minimum sample volume of 1000 cubic centimeters is recommended. The step-by-step procedures are accompanied by a description of the minimum requirements for sample documentation. Transport of the soil samples from the field is then addressed in a discussion of the federal regulations for shipping radioactive materials. Interpretation of those regulations, particularly in light of their application to remedial action soil-sampling programs, is provided in the form of guidance and suggested procedures. Due to the complex nature of the regulations, however, there is no guarantee that our interpretations of them are complete or entirely accurate. Preparation of soil samples for radium-226 analysis by means of gamma-ray spectroscopy is described

  19. NH4NO3 extractable trace element contents of soil samples prepared for proficiency testing--a stability study.

    Science.gov (United States)

    Traub, H; Scharf, H

    2001-06-01

    In view of its intended use as a sample for proficiency testing or as a reference material the stability of the extractable trace element contents of a soil from an irrigation field was tested using the extraction with 1 mol/L ammonium nitrate solution according to DIN 19730. Therefore, changes of the extractability of sterilized and non sterilized soil samples stored at different temperatures were evaluated over a period of 18 months. Sets of bottles were kept at -20 degrees C, +4 degrees C, about +20 degrees C and +40 degrees C, respectively. The NH4NO3 extractable contents of Cd, Cr, Cu, Ni, Pb and Zn were determined immediately after bottling and then after 3, 6, 12 and 18 months with ICP-AES or ETAAS. Appropriate storage conditions are of utmost importance to prevent deterioration of soil samples prepared for the determination of NH4NO3 extractable trace element contents. Temperatures above +20 degrees C must be avoided. The observed changes in the extractability of the metals (especially for Cr and Cu) most likely could be related to thermal degradation of the organic matter of the soil. There is no need to sterilize dry soil samples, because microbiological activity in soils with a low moisture content appears to be negligible with regard to trace element mobilization.

  20. Finding even more anthropogenic indicators in mildly prepared sediment samples

    DEFF Research Database (Denmark)

    Enevold, Renée; Odgaard, Bent Vad

    2016-01-01

    be worth the effort to prepare the NPP samples with as mild a preparation method as possible. We have mildly prepared NPP samples from a small forest hollow, Tårup Lund, Denmark. From the recovered NPP assemblages we attempt identifying anthropogenic indicators by comparing to the environmental information......NPPs in anthropogenic soils and archaeological samples are often numerous in types as well as in abundance. Preparing these soil samples with methods based on acid digestion holds the potential of severe bias leaving the NPP assemblages devoid of acid vulnerable NPPs. In many cases it might...... derived from sediment, pollen and macrofossil analyses. The sediment from the forest hollow encompasses environmental information from the last 6000 years, including a period of locally intense pastoral and/or agricultural activity during the Iron Age. Keywords: NPP diversity, forest hollow, anthropogenic...

  1. Sample preparation techniques in trace element analysis by X-ray emission spectroscopy

    International Nuclear Information System (INIS)

    Valkovic, V.

    1983-11-01

    The report, written under a research contract with the IAEA, contains a detailed presentation of the most difficult problem encountered in the trace element analysis by methods of the X-ray emission spectroscopy, namely the sample preparation techniques. The following items are covered. Sampling - with specific consideration of aerosols, water, soil, biological materials, petroleum and its products, storage of samples and their handling. Pretreatment of samples - preconcentration, ashing, solvent extraction, ion exchange and electrodeposition. Sample preparations for PIXE - analysis - backings, target uniformity and homogeneity, effects of irradiation, internal standards and specific examples of preparation (aqueous, biological, blood serum and solid samples). Sample preparations for radioactive sources or tube excitation - with specific examples (water, liquid and solid samples, soil, geological, plants and tissue samples). Finally, the problem of standards and reference materials, as well as that of interlaboratory comparisons, is discussed

  2. Dielectrophoretic sample preparation for environmental monitoring of microorganisms: Soil particle removal.

    Science.gov (United States)

    Fatoyinbo, Henry O; McDonnell, Martin C; Hughes, Michael P

    2014-07-01

    Detection of pathogens from environmental samples is often hampered by sensors interacting with environmental particles such as soot, pollen, or environmental dust such as soil or clay. These particles may be of similar size to the target bacterium, preventing removal by filtration, but may non-specifically bind to sensor surfaces, fouling them and causing artefactual results. In this paper, we report the selective manipulation of soil particles using an AC electrokinetic microfluidic system. Four heterogeneous soil samples (smectic clay, kaolinitic clay, peaty loam, and sandy loam) were characterised using dielectrophoresis to identify the electrical difference to a target organism. A flow-cell device was then constructed to evaluate dielectrophoretic separation of bacteria and clay in a continous flow through mode. The average separation efficiency of the system across all soil types was found to be 68.7% with a maximal separation efficiency for kaolinitic clay at 87.6%. This represents the first attempt to separate soil particles from bacteria using dielectrophoresis and indicate that the technique shows significant promise; with appropriate system optimisation, we believe that this preliminary study represents an opportunity to develop a simple yet highly effective sample processing system.

  3. Determination of Pu in soil samples

    International Nuclear Information System (INIS)

    Torres C, C. O.; Hernandez M, H.; Romero G, E. T.; Vega C, H. R.

    2016-10-01

    The irreversible consequences of accidents occurring in nuclear plants and in nuclear fuel reprocessing sites are mainly the distribution of different radionuclides in different matrices such as the soil. The distribution in the superficial soil is related to the internal and external exposure to the radiation of the affected population. The internal contamination with radionuclides such as Pu is of great relevance to the nuclear forensic science, where is important to know the chemical and isotopic compositions of nuclear materials. The objective of this work is to optimize the radiochemical separation of plutonium (Pu) from soil samples and to determine their concentration. The soil samples were prepared using acid digestion assisted by microwave; purification of Pu was carried out with AG1X8 resin using ion exchange chromatography. Pu isotopes were measured using ICP-SFMS. In order to reduce the interference due to the presence of "2"3"8UH "+ in the samples, a solvent removal system (Apex) was used. In addition, the limit of detection and quantification of Pu was determined. It was found that the recovery efficiency of Pu in soil samples ranges from 70 to 93%. (Author)

  4. Bioremediation of PAH contaminated soil samples

    International Nuclear Information System (INIS)

    Joshi, M.M.; Lee, S.

    1994-01-01

    Soils contaminated with polynuclear aromatic hydrocarbons (PAHs) pose a hazard to life. The remediation of such sites can be done using physical, chemical, and biological treatment methods or a combination of them. It is of interest to study the decontamination of soil using bioremediation. The experiments were conducted using Acinetobacter (ATCC 31012) at room temperature without pH or temperature control. In the first series of experiments, contaminated soil samples obtained from Alberta Research Council were analyzed to determine the toxic contaminant and their composition in the soil. These samples were then treated using aerobic fermentation and removal efficiency for each contaminant was determined. In the second series of experiments, a single contaminant was used to prepare a synthetic soil sample. This sample of known composition was then treated using aerobic fermentation in continuously stirred flasks. In one set of flasks, contaminant was the only carbon source and in the other set, starch was an additional carbon source. In the third series of experiments, the synthetic contaminated soil sample was treated in continuously stirred flasks in the first set and in fixed bed in the second set and the removal efficiencies were compared. The removal efficiencies obtained indicated the extent of biodegradation for various contaminants, the effect of additional carbon source, and performance in fixed bed without external aeration

  5. Sample preparation method for ICP-MS measurement of 99Tc in a large amount of environmental samples

    International Nuclear Information System (INIS)

    Kondo, M.; Seki, R.

    2002-01-01

    Sample preparation for measurement of 99 Tc in a large amount of soil and water samples by ICP-MS has been developed using 95m Tc as a yield tracer. This method is based on the conventional method for a small amount of soil samples using incineration, acid digestion, extraction chromatography (TEVA resin) and ICP-MS measurement. Preliminary concentration of Tc has been introduced by co-precipitation with ferric oxide. The matrix materials in a large amount of samples were more sufficiently removed with keeping the high recovery of Tc than previous method. The recovery of Tc was 70-80% for 100 g soil samples and 60-70% for 500 g of soil and 500 L of water samples. The detection limit of this method was evaluated as 0.054 mBq/kg in 500 g soil and 0.032 μBq/L in 500 L water. The determined value of 99 Tc in the IAEA-375 (soil sample collected near the Chernobyl Nuclear Reactor) was 0.25 ± 0.02 Bq/kg. (author)

  6. 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

  7. 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.

  8. 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.

  9. Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction

    Energy Technology Data Exchange (ETDEWEB)

    Pena, M.T.; Pensado, Luis; Casais, M.C.; Mejuto, M.C.; Cela, Rafael [Universidad de Santiago de Compostela, Dpto. Quimica Analitica, Nutricion y Bromatologia. Instituto de Investigacion y Analisis Alimentario, Santiago de Compostela (Spain)

    2007-04-15

    A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 {mu}g kg{sup -1} dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials. (orig.)

  10. Sample preparation of sewage sludge and soil samples for the determination of polycyclic aromatic hydrocarbons based on one-pot microwave-assisted saponification and extraction.

    Science.gov (United States)

    Pena, M Teresa; Pensado, Luis; Casais, M Carmen; Mejuto, M Carmen; Cela, Rafael

    2007-04-01

    A microwave-assisted sample preparation (MASP) procedure was developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) in sewage sludge and soil samples. The procedure involved the simultaneous microwave-assisted extraction of PAHs with n-hexane and the hydrolysis of samples with methanolic potassium hydroxide. Because of the complex nature of the samples, the extracts were submitted to further cleaning with silica and Florisil solid-phase extraction cartridges connected in series. Naphthalene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benz[a]anthracene, chrysene, benzo[e]pyrene, benzo[b]fluoranthene, benzo[k]fluoranthene, benzo[a]pyrene, dibenz[a,h]anthracene, benzo[g,h,i]perylene, and indeno[1,2,3-cd]pyrene, were considered in the study. Quantification limits obtained for all of these compounds (between 0.4 and 14.8 microg kg(-1) dry mass) were well below of the limits recommended in the USA and EU. Overall recovery values ranged from 60 to 100%, with most losses being due to evaporation in the solvent exchange stages of the procedure, although excellent extraction recoveries were obtained. Validation of the accuracy was carried out with BCR-088 (sewage sludge) and BCR-524 (contaminated industrial soil) reference materials.

  11. Sample preparation

    International Nuclear Information System (INIS)

    Anon.

    1992-01-01

    Sample preparation prior to HPLC analysis is certainly one of the most important steps to consider in trace or ultratrace analysis. For many years scientists have tried to simplify the sample preparation process. It is rarely possible to inject a neat liquid sample or a sample where preparation may not be any more complex than dissolution of the sample in a given solvent. The last process alone can remove insoluble materials, which is especially helpful with the samples in complex matrices if other interactions do not affect extraction. Here, it is very likely a large number of components will not dissolve and are, therefore, eliminated by a simple filtration process. In most cases, the process of sample preparation is not as simple as dissolution of the component interest. At times, enrichment is necessary, that is, the component of interest is present in very large volume or mass of material. It needs to be concentrated in some manner so a small volume of the concentrated or enriched sample can be injected into HPLC. 88 refs

  12. High-throughput automated microfluidic sample preparation for accurate microbial genomics.

    Science.gov (United States)

    Kim, Soohong; De Jonghe, Joachim; Kulesa, Anthony B; Feldman, David; Vatanen, Tommi; Bhattacharyya, Roby P; Berdy, Brittany; Gomez, James; Nolan, Jill; Epstein, Slava; Blainey, Paul C

    2017-01-27

    Low-cost shotgun DNA sequencing is transforming the microbial sciences. Sequencing instruments are so effective that sample preparation is now the key limiting factor. Here, we introduce a microfluidic sample preparation platform that integrates the key steps in cells to sequence library sample preparation for up to 96 samples and reduces DNA input requirements 100-fold while maintaining or improving data quality. The general-purpose microarchitecture we demonstrate supports workflows with arbitrary numbers of reaction and clean-up or capture steps. By reducing the sample quantity requirements, we enabled low-input (∼10,000 cells) whole-genome shotgun (WGS) sequencing of Mycobacterium tuberculosis and soil micro-colonies with superior results. We also leveraged the enhanced throughput to sequence ∼400 clinical Pseudomonas aeruginosa libraries and demonstrate excellent single-nucleotide polymorphism detection performance that explained phenotypically observed antibiotic resistance. Fully-integrated lab-on-chip sample preparation overcomes technical barriers to enable broader deployment of genomics across many basic research and translational applications.

  13. Improved sample preparation and counting techniques for enhanced tritium measurement sensitivity

    Science.gov (United States)

    Moran, J.; Aalseth, C.; Bailey, V. L.; Mace, E. K.; Overman, C.; Seifert, A.; Wilcox Freeburg, E. D.

    2015-12-01

    Tritium (T) measurements offer insight to a wealth of environmental applications including hydrologic tracking, discerning ocean circulation patterns, and aging ice formations. However, the relatively short half-life of T (12.3 years) limits its effective age dating range. Compounding this limitation is the decrease in atmospheric T content by over two orders of magnitude (from 1000-2000 TU in 1962 to testing in the 1960's. We are developing sample preparation methods coupled to direct counting of T via ultra-low background proportional counters which, when combined, offer improved T measurement sensitivity (~4.5 mmoles of H2 equivalent) and will help expand the application of T age dating to smaller sample sizes linked to persistent environmental questions despite the limitations above. For instance, this approach can be used to T date ~ 2.2 mmoles of CH4 collected from sample-limited systems including microbial communities, soils, or subsurface aquifers and can be combined with radiocarbon dating to distinguish the methane's formation age from C age in a system. This approach can also expand investigations into soil organic C where the improved sensitivity will permit resolution of soil C into more descriptive fractions and provide direct assessments of the stability of specific classes of organic matter in soils environments. We are employing a multiple step sample preparation system whereby organic samples are first combusted with resulting CO2 and H2O being used as a feedstock to synthesize CH4. This CH4 is mixed with Ar and loaded directly into an ultra-low background proportional counter for measurement of T β decay in a shallow underground laboratory. Analysis of water samples requires only the addition of geologic CO2 feedstock with the sample for methane synthesis. The chemical nature of the preparation techniques enable high sample throughput with only the final measurement requiring T decay with total sample analysis time ranging from 2 -5 weeks

  14. Methods for preparing comparative standards and field samples for neutron activation analysis of soil

    International Nuclear Information System (INIS)

    Glasgow, D.C.; Dyer, F.F.; Robinson, L.

    1995-01-01

    One of the more difficult problems associated with comparative neutron activation analysis (CNAA) is the preparation of standards which are tailor-made to the desired irradiation and counting conditions. Frequently, there simply is not a suitable standard available commercially, or the resulting gamma spectrum is convoluted with interferences. In a recent soil analysis project, the need arose for standards which contained about 35 elements. In response, a computer spreadsheet was developed to calculate the appropriate amount of each element so that the resulting gamma spectrum is relatively free of interferences. Incorporated in the program are options for calculating all of the irradiation and counting parameters including activity produced, necessary flux/bombardment time, counting time, and appropriate source-to-detector distance. The result is multi-element standards for CNAA which have optimal concentrations. The program retains ease of use without sacrificing capability. In addition to optimized standard production, a novel soil homogenization technique was developed which is a low cost, highly efficient alternative to commercially available homogenization systems. Comparative neutron activation analysis for large scale projects has been made easier through these advancements. This paper contains details of the design and function of the NAA spreadsheet and innovative sample handling techniques. (author) 7 refs.; 5 tabs

  15. Methods for preparing comparative standards and field samples for neutron activation analysis of soil

    International Nuclear Information System (INIS)

    Glasgow, D.C.; Dyer, F.F.; Robinson, L.

    1994-01-01

    One of the more difficult problems associated with comparative neutron activation analysis (CNAA) is the preparation of standards which are tailor-made to the desired irradiation and counting conditions. Frequently, there simply is not a suitable standard available commercially, or the resulting gamma spectrum is convoluted with interferences. In a recent soil analysis project, the need arose for standards which contained about 35 elements. In response, a computer spreadsheet was developed to calculate the appropriate amount of each element so that the resulting gamma spectrum is relatively free of interferences. Incorporated in the program are options for calculating all of the irradiation and counting parameters including activity produced, necessary flux/bombardment time, counting time, and appropriate source-to-detector distance. The result is multi-element standards for CNAA which have optimal concentrations. The program retains ease of use without sacrificing capability. In addition to optimized standard production, a novel soil homogenization technique was developed which is a low cost, highly efficient alternative to commercially available homogenization systems. Comparative neutron activation analysis for large scale projects has been made easier through these advancements. This paper contains details of the design and function of the NAA spreadsheet and innovative sample handling techniques

  16. Extraction of Plutonium From Spiked INEEL Soil Samples Using the Ligand-Assisted Supercritical Fluid Extraction (LA-SFE) Technique

    International Nuclear Information System (INIS)

    Fox, R.V.; Mincher, B.J.; Holmes, R.G.G.

    1999-01-01

    In order to investigate the effectiveness of ligand-assisted supercritical fluid extraction for the removal of transuranic contaminations from soils an Idaho National Engineering and Environmental Laboratory (INEEL) silty-clay soil sample was obtained from near the Radioactive Waste Management Complex area and subjected to three different chemical preparations before being spiked with plutonium. The spiked INEEL soil samples were subjected to a sequential aqueous extraction procedure to determine radionuclide portioning in each sample. Results from those extractions demonstrate that plutonium consistently partitioned into the residual fraction across all three INEEL soil preparations whereas americium partitioned 73% into the iron/manganese fraction for soil preparation A, with the balance partitioning into the residual fraction. Plutonium and americium were extracted from the INEEL soil samples using a ligand-assisted supercritical fluid extraction technique. Initial supercritical fluid extraction runs produced plutonium extraction technique. Initial supercritical fluid extraction runs produced plutonium extraction efficiencies ranging from 14% to 19%. After a second round wherein the initial extraction parameters were changed, the plutonium extraction efficiencies increased to 60% and as high as 80% with the americium level in the post-extracted soil samples dropping near to the detection limits. The third round of experiments are currently underway. These results demonstrate that the ligand-assisted supercritical fluid extraction technique can effectively extract plutonium from the spiked INEEL soil preparations

  17. Sampling and analysis of alien materials in soil

    Energy Technology Data Exchange (ETDEWEB)

    Liphard, K G

    1987-02-01

    For the determination of alien materials in soil, sampling is the decisive step. After minute planning, samples can be obtained by probing, boring or abrasion. Some types of substances can be verified by advance sampling, partly already in the field. Inorganic substances present as anions or cations are eluted and determined with water, heavy metals are determined after preparing a number of solutions by spectroscopic methods. Organic alien substances are extracted with solvents and, as a rule, analysed by chromatography.

  18. Determination of uranium and thorium isotopes in soil samples by coprecipitation

    International Nuclear Information System (INIS)

    Ngo Quang Huy; Trinh Thi Bich; Nguyen Van Suc

    2012-01-01

    The paper presents a procedure to prepare soil samples for U and Th isotope measurement by alpha-spectrometry after coprecipitation with LaF 3 . In this procedure the reduction of U(VI) to U(IV) was performed by Zn metal in 4M HCl solution. The recoveries of chemical separation equal to ε U-chemistry = 78±4% for uranium and ε Th-chemistry = 82±4% for thorium. Canberra alpha-spectrometer was used with PIPS detectors of A-1200-37-AM Model of 1200 mm 2 active area. The counting efficiency of the measuring system equals to ε counting = 18% and the total efficiencies were ε U = ε counting - ε U-chemistry = 14.0 ± 0.7% for uranium and ε Th = ε counting - ε Th-chemistry = 14.7 ± 0.7% for thorium. The recoveries of chemical separation were rather high (about 80%), that leads to the use of a small weight of soil sample (about 0.5 g). The efficiencies were also stable, that allows analyzing the soil sample without using radiotracers. They are advantages of the sample preparation procedure of this work. (author)

  19. Analysis of soil and sewage sludge by ICP-OES and the German standard DIN 38414 sample preparation technique (P3)

    International Nuclear Information System (INIS)

    Edlund, M.; Heitland, P.; Visser, H.

    2002-01-01

    Full text: The elemental analyses of soil and sewage sludge has developed to become one of the main applications for ICP optical emission spectrometry (ICP-OES) and is described in many official procedures. These methods include different acid mixtures and digestion techniques. Even though the German standard DIN 38414 part 7 and the Dutch NEN 6465 do not guarantee complete recoveries for all elements, they are widely accepted in Europe. This paper describes sample preparation, line selection and investigates precision, accuracy and Limits of detection. The SPECTRO CIROSCCD EOP with axial plasma observation and the SPECTRO CIROSCCD SOP with radial observation were compared and evaluated for the analyses of soil and sewage sludge. Accuracy was investigated using the certified reference materials CRM-141 R, CRM-143 R and GSD 11. Both instruments show excellent performance in terms of speed, precision, accuracy and detection limits for the determination of trace metals in soil and sewage sludge. (author)

  20. Degradation of hydrocarbons in soil samples analyzed within accepted analytical holding times

    International Nuclear Information System (INIS)

    Jackson, J.; Thomey, N.; Dietlein, L.F.

    1992-01-01

    Samples which are collected in conjunction with subsurface investigations at leaking petroleum storage tank sites and petroleum refineries are routinely analyzed for benzene, toluene, ethylbenzene, xylenes (BTEX), and total petroleum hydrocarbons (TPH). Water samples are preserved by the addition of hydrochloric acid and maintained at four degrees centigrade prior to analysis. This is done to prevent bacterial degradation of hydrocarbons. Chemical preservation is not presently performed on soil samples. Instead, the samples are cooled and maintained at four degrees centigrade. This study was done to measure the degree of degradation of hydrocarbons in soil samples which are analyzed within accepted holding times. Soil samples were collected and representative subsamples were prepared from the initial sample. Subsamples were analyzed in triplicate for BTEX and TPH throughout the length of the approved holding times to measure the extent of sample constituent degradation prior to analysis. Findings imply that for sandy soils, BTEX and TPH concentrations can be highly dependent upon the length of time which elapses between sample collection and analysis

  1. Soil sampling in emergency situations

    International Nuclear Information System (INIS)

    Carvalho, Zenildo Lara de; Ramos Junior, Anthenor Costa

    1997-01-01

    The soil sampling methods used in Goiania's accident (1987) by the environmental team of Brazilian Nuclear Energy Commission (CNEN) are described. The development of this method of soil sampling to a emergency sampling method used in a Nuclear Emergency Exercise in Angra dos Reis Reactor Site (1991) is presented. A new method for soil sampling based on a Chernobyl environmental monitoring experience (1995) is suggested. (author)

  2. Measurement of radioactivity in the environment - Soil - Part 2: Guidance for the selection of the sampling strategy, sampling and pre-treatment of samples

    International Nuclear Information System (INIS)

    2007-01-01

    This part of ISO 18589 specifies the general requirements, based on ISO 11074 and ISO/IEC 17025, for all steps in the planning (desk study and area reconnaissance) of the sampling and the preparation of samples for testing. It includes the selection of the sampling strategy, the outline of the sampling plan, the presentation of general sampling methods and equipment, as well as the methodology of the pre-treatment of samples adapted to the measurements of the activity of radionuclides in soil. This part of ISO 18589 is addressed to the people responsible for determining the radioactivity present in soil for the purpose of radiation protection. It is applicable to soil from gardens, farmland, urban or industrial sites, as well as soil not affected by human activities. This part of ISO 18589 is applicable to all laboratories regardless of the number of personnel or the range of the testing performed. When a laboratory does not undertake one or more of the activities covered by this part of ISO 18589, such as planning, sampling or testing, the corresponding requirements do not apply. Information is provided on scope, normative references, terms and definitions and symbols, principle, sampling strategy, sampling plan, sampling process, pre-treatment of samples and recorded information. Five annexes inform about selection of the sampling strategy according to the objectives and the radiological characterization of the site and sampling areas, diagram of the evolution of the sample characteristics from the sampling site to the laboratory, example of sampling plan for a site divided in three sampling areas, example of a sampling record for a single/composite sample and example for a sample record for a soil profile with soil description. A bibliography is provided

  3. 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

  4. X-ray spectrometry and X-ray microtomography techniques for soil and geological samples analysis

    International Nuclear Information System (INIS)

    Kubala-Kukuś, A.; Banaś, D.; Braziewicz, J.; Dziadowicz, M.; Kopeć, E.; Majewska, U.; Mazurek, M.; Pajek, M.; Sobisz, M.; Stabrawa, I.; Wudarczyk-Moćko, J.; Góźdź, S.

    2015-01-01

    A particular subject of X-ray fluorescence analysis is its application in studies of the multielemental sample of composition in a wide range of concentrations, samples with different matrices, also inhomogeneous ones and those characterized with different grain size. Typical examples of these kinds of samples are soil or geological samples for which XRF elemental analysis may be difficult due to XRF disturbing effects. In this paper the WDXRF technique was applied in elemental analysis concerning different soil and geological samples (therapeutic mud, floral soil, brown soil, sandy soil, calcium aluminum cement). The sample morphology was analyzed using X-ray microtomography technique. The paper discusses the differences between the composition of samples, the influence of procedures with respect to the preparation of samples as regards their morphology and, finally, a quantitative analysis. The results of the studies were statistically tested (one-way ANOVA and correlation coefficients). For lead concentration determination in samples of sandy soil and cement-like matrix, the WDXRF spectrometer calibration was performed. The elemental analysis of the samples was complemented with knowledge of chemical composition obtained by X-ray powder diffraction.

  5. X-ray spectrometry and X-ray microtomography techniques for soil and geological samples analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kubala-Kukuś, A.; Banaś, D.; Braziewicz, J. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Dziadowicz, M.; Kopeć, E. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Majewska, U. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Mazurek, M.; Pajek, M.; Sobisz, M.; Stabrawa, I. [Institute of Physics, Jan Kochanowski University, ul. Świetokrzyska 15, 25-406 Kielce (Poland); Wudarczyk-Moćko, J. [Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Góźdź, S. [Holycross Cancer Center, ul. Artwińskiego 3, 25-734 Kielce (Poland); Institute of Public Health, Jan Kochanowski University, IX Wieków Kielc 19, 25-317 Kielce (Poland)

    2015-12-01

    A particular subject of X-ray fluorescence analysis is its application in studies of the multielemental sample of composition in a wide range of concentrations, samples with different matrices, also inhomogeneous ones and those characterized with different grain size. Typical examples of these kinds of samples are soil or geological samples for which XRF elemental analysis may be difficult due to XRF disturbing effects. In this paper the WDXRF technique was applied in elemental analysis concerning different soil and geological samples (therapeutic mud, floral soil, brown soil, sandy soil, calcium aluminum cement). The sample morphology was analyzed using X-ray microtomography technique. The paper discusses the differences between the composition of samples, the influence of procedures with respect to the preparation of samples as regards their morphology and, finally, a quantitative analysis. The results of the studies were statistically tested (one-way ANOVA and correlation coefficients). For lead concentration determination in samples of sandy soil and cement-like matrix, the WDXRF spectrometer calibration was performed. The elemental analysis of the samples was complemented with knowledge of chemical composition obtained by X-ray powder diffraction.

  6. Quantification of trace arsenic in soils by field-portable X-ray fluorescence spectrometry: considerations for sample preparation and measurement conditions.

    Science.gov (United States)

    Parsons, Chris; Margui Grabulosa, Eva; Pili, Eric; Floor, Geerke H; Roman-Ross, Gabriela; Charlet, Laurent

    2013-11-15

    Recent technological improvements have led to the widespread adoption of field portable energy dispersive X-ray fluorescence (FP-XRF) by governmental agencies, environmental consultancies and research institutions. FP-XRF units often include analysis modes specifically designed for the quantification of trace elements in soils. Using these modes, X-ray tube based FP-XRF units can offer almost "point and shoot" ease of use and results comparable to those of laboratory based instruments. Nevertheless, FP-XRF analysis is sensitive to spectral interferences as well as physical and chemical matrix effects which can result in decreased precision and accuracy. In this study, an X-ray tube-based FP-XRF analyser was used to determine trace (low ppm) concentrations of As in a floodplain soil. The effect of different sample preparation and analysis conditions on precision and accuracy were systematically evaluated. We propose strategies to minimise sources of error and maximise data precision and accuracy, achieving in situ limits of detection and precision of 6.8 ppm and 14.4%RSD, respectively for arsenic. We demonstrate that soil moisture, even in relatively dry soils, dramatically affects analytical performance with a signal loss of 37% recorded for arsenic at 20 wt% soil moisture relative to dry soil. We also highlight the importance of the use of certified reference materials and independent measurement methods to ensure accurate correction of field values. Copyright © 2012 Elsevier B.V. All rights reserved.

  7. Efficiency calibration and measurement of self-absorption correction of environmental gamma spectroscopy of soils samples using Marinelli beaker

    International Nuclear Information System (INIS)

    Abdi, M. R.; Mostajaboddavati, M.; Hassanzadeh, S.; Faghihian, H.; Rezaee, Kh.; Kamali, M.

    2006-01-01

    A nonlinear function in combination with the method of mixing activity calibrated is applied for fitting the experimental peak efficiency of HPGe spectrometers in 59-2614 keV energy range. The preparation of Marinelli beaker standards of mixed gamma and RG-set at secular equilibrium with its daughter radionuclides was studied. Standards were prepared by mixing of known amounts of 13B a, 241 Am, 152 Eu, 207 Bi, 24 Na, Al 2 O 3 powder and soil. The validity of these standards was checked by comparison with certified standard reference material RG-set and IAEA-Soil-6 Self-absorption was measured for the activity calculation of the gamma-ray lines about series of 238 U daughter, 232 Th series, 137 Cs and 40 K in soil samples. Self-absorption in the sample will depend on a number of factor including sample composition, density, sample size and gamma-ray energy. Seven Marinelli beaker standards were prepared in different degrees of compaction with bulk density ( ρ) of 1.000 to 1.600 g cm -3 . The detection efficiency versus density was obtained and the equation of self-absorption correction factors calculated for soil samples

  8. A Comparison of Soil-Water Sampling Techniques

    Science.gov (United States)

    Tindall, J. A.; Figueroa-Johnson, M.; Friedel, M. J.

    2007-12-01

    The representativeness of soil pore water extracted by suction lysimeters in ground-water monitoring studies is a problem that often confounds interpretation of measured data. Current soil water sampling techniques cannot identify the soil volume from which a pore water sample is extracted, neither macroscopic, microscopic, or preferential flowpath. This research was undertaken to compare values of extracted suction lysimeters samples from intact soil cores with samples obtained by the direct extraction methods to determine what portion of soil pore water is sampled by each method. Intact soil cores (30 centimeter (cm) diameter by 40 cm height) were extracted from two different sites - a sandy soil near Altamonte Springs, Florida and a clayey soil near Centralia in Boone County, Missouri. Isotopically labeled water (O18? - analyzed by mass spectrometry) and bromide concentrations (KBr- - measured using ion chromatography) from water samples taken by suction lysimeters was compared with samples obtained by direct extraction methods of centrifugation and azeotropic distillation. Water samples collected by direct extraction were about 0.25 ? more negative (depleted) than that collected by suction lysimeter values from a sandy soil and about 2-7 ? more negative from a well structured clayey soil. Results indicate that the majority of soil water in well-structured soil is strongly bound to soil grain surfaces and is not easily sampled by suction lysimeters. In cases where a sufficient volume of water has passed through the soil profile and displaced previous pore water, suction lysimeters will collect a representative sample of soil pore water from the sampled depth interval. It is suggested that for stable isotope studies monitoring precipitation and soil water, suction lysimeter should be installed at shallow depths (10 cm). Samples should also be coordinated with precipitation events. The data also indicate that each extraction method be use to sample a different

  9. Effects of different soil preparation techniques on the Anatolian Black Pine (Pinus nigra Arnold subsp. pallasiana (Lamb. Holmboe regeneration

    Directory of Open Access Journals (Sweden)

    Adil Çalışkan

    2014-07-01

    Full Text Available In this study, the effects of different soil preparation treatments on regeneration of black pine success were examined and some suggestions were given according to the results. Twelve sample plots were randomly set in the research area. The size of each sample plot was 4 m². Sample plots were seeded equally with a total number of 2304 (48 seeds per m2 seeds in April 2012. The number of surviving seedlings was recorded every month from May to November in 2012. Surviving seedlings were recorded again in November 2013 and growths of thirty seedlings which are selected randomly from the all sample plots were examined. It was found that soil treatment with machine was more successful in regeneration at semi-arid regions like Cerkes-Turkey. Plowing equipment as mechanical soil cultivation has more economically advantageous in first years. However, the success and quality of seedlings were better in soil preparation with ripper equipment compared to plowing.

  10. Soil sampling

    International Nuclear Information System (INIS)

    Fortunati, G.U.; Banfi, C.; Pasturenzi, M.

    1994-01-01

    This study attempts to survey the problems associated with techniques and strategies of soil sampling. Keeping in mind the well defined objectives of a sampling campaign, the aim was to highlight the most important aspect of representativeness of samples as a function of the available resources. Particular emphasis was given to the techniques and particularly to a description of the many types of samplers which are in use. The procedures and techniques employed during the investigations following the Seveso accident are described. (orig.)

  11. Determination of Pu in soil samples; Determinacion de Pu en muestras de suelo

    Energy Technology Data Exchange (ETDEWEB)

    Torres C, C. O.; Hernandez M, H.; Romero G, E. T. [ININ, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico); Vega C, H. R., E-mail: carioli_32907@hotmail.com [Universidad Autonoma de Zacatecas, Unidad Academica de Estudios Nucleares, Cipres No. 10, Fracc. La Penuela, 98068 Zacatecas, Zac. (Mexico)

    2016-10-15

    The irreversible consequences of accidents occurring in nuclear plants and in nuclear fuel reprocessing sites are mainly the distribution of different radionuclides in different matrices such as the soil. The distribution in the superficial soil is related to the internal and external exposure to the radiation of the affected population. The internal contamination with radionuclides such as Pu is of great relevance to the nuclear forensic science, where is important to know the chemical and isotopic compositions of nuclear materials. The objective of this work is to optimize the radiochemical separation of plutonium (Pu) from soil samples and to determine their concentration. The soil samples were prepared using acid digestion assisted by microwave; purification of Pu was carried out with AG1X8 resin using ion exchange chromatography. Pu isotopes were measured using ICP-SFMS. In order to reduce the interference due to the presence of {sup 238}UH {sup +} in the samples, a solvent removal system (Apex) was used. In addition, the limit of detection and quantification of Pu was determined. It was found that the recovery efficiency of Pu in soil samples ranges from 70 to 93%. (Author)

  12. 40 CFR 761.323 - Sample preparation.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Sample preparation. 761.323 Section... Remediation Waste Samples § 761.323 Sample preparation. (a) The comparison study requires analysis of a... concentrations by dilution. Any excess material resulting from the preparation of these samples, which is not...

  13. Sample preparation in foodomic analyses.

    Science.gov (United States)

    Martinović, Tamara; Šrajer Gajdošik, Martina; Josić, Djuro

    2018-04-16

    Representative sampling and adequate sample preparation are key factors for successful performance of further steps in foodomic analyses, as well as for correct data interpretation. Incorrect sampling and improper sample preparation can be sources of severe bias in foodomic analyses. It is well known that both wrong sampling and sample treatment cannot be corrected anymore. These, in the past frequently neglected facts, are now taken into consideration, and the progress in sampling and sample preparation in foodomics is reviewed here. We report the use of highly sophisticated instruments for both high-performance and high-throughput analyses, as well as miniaturization and the use of laboratory robotics in metabolomics, proteomics, peptidomics and genomics. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  14. Preparation of Acrylamide-based Anionic Polyelectrolytes for Soil Establishment

    Directory of Open Access Journals (Sweden)

    Ahmad Rabiee

    2012-12-01

    Full Text Available Synthetic water soluble acrylamide-based polymers have wide range of ap-plications  in  the  feld  of  soil  establishment  and  non-desertifcation.  In  this research, the acrylamide-based anionic polyelectrolytes were prepared by  solution polymerization. The polymerization was carried out using AIBN as a radical initiator and at different degrees of anionic charges ranging between 10% and 30% using sodium hydroxide as hydrolyzing agents. The chemical structure of the  synthetic polymers was studied and confrmed by FTIR technique. The charge density on polymer backbone was determined by titration method. The rheological behavior of polymer solutions was evaluated by Brookfeld viscometer. The results show that the viscosity decreases with increasing the shear rate of solutions. Molecular weights of samples were measured by laser light scattering analyzer. The morphology of the polymer was studied by SEM and the EDX was used for elemental analysis determination. The anionic polymers with 10-30% negative charges were mixed with clay in order to evaluate the soil establishment. The results show that an anionic polyelectro-lyte can make soil particles more cohesive and improve soil physical properties.

  15. Soil Gas Sampling

    Science.gov (United States)

    Field Branches Quality System and Technical Procedures: This document describes general and specific procedures, methods and considerations to be used and observed when collecting soil gas samples for field screening or laboratory analysis.

  16. Quality control for measurement of soil samples containing 237Np and 241Am as radiotracer

    International Nuclear Information System (INIS)

    Sha Lianmao; Zhang Caihong; Song Hailong; Ren Xiaona; Han Yuhu; Zhang Aiming; Chu Taiwei

    2003-01-01

    This paper reports quality control (QC) for the measurement of soil samples containing 237 Np and 241 Am as radiotracers in migration test of transuranic nuclides. All of the QC were done independently by the QA members of analytical work. It mainly included checking 5%-10% of the total analyzed samples; preparing blank samples, blind replicate sample and spiked samples used as quality control samples to check the quality of analytical work

  17. Improved detection of endoparasite DNA in soil sample PCR by the use of anti-inhibitory substances.

    Science.gov (United States)

    Krämer, F; Vollrath, T; Schnieder, T; Epe, C

    2002-09-26

    Although there have been numerous microbial examinations of soil for the presence of human pathogenic developmental parasite stages of Ancylostoma caninum and Toxocara canis, molecular techniques (e.g. DNA extraction, purification and subsequent PCR) have scarcely been applied. Here, DNA preparations of soil samples artificially contaminated with genomic DNA or parasite eggs were examined by PCR. A. caninum and T. canis-specific primers based on the ITS-2 sequence were used for amplification. After the sheer DNA preparation a high content of PCR-interfering substances was still detectable. Subsequently, two different inhibitors of PCR-interfering agents (GeneReleaser, Bioventures Inc. and Maximator, Connex GmbH) were compared in PCR. Both substances increased PCR sensitivity greatly. However, comparison of the increase in sensitivity achieved with the two compounds demonstrated the superiority of Maximator, which enhanced sensitivity to the point of permitting positive detection of a single A. caninum egg and three T. canis eggs in a soil sample. This degree of sensitivity could not be achieved with GeneReleaser for either parasite Furthermore, Maximator not only increased sensitivity; it also cost less, required less time and had a lower risk of contamination. Future applications of molecular methods in epidemiological examinations of soil samples are discussed/elaborated.

  18. Response of soil aggregate stability to storage time of soil samples

    International Nuclear Information System (INIS)

    Gerzabek, M.H.; Roessner, H.

    1993-04-01

    The aim of the present study was to investigate the well known phenomenon of changing aggregate stability values as result of soil sample storage. In order to evaluate the impact of soil microbial activity, the soil sample was split into three subsamples. Two samples were sterilized by means of chloroform fumigation and gamma irradiation, respectively. However, the aggregate stability measurements at three different dates were not correlated with the microbial activity (dehydrogenase activity). The moisture content of the aggregate samples seems to be of higher significance. Samples with lower moisture content (range: 0.4 to 1.9%) exhibited higher aggregate stabilities. Thus, airdried aggregate samples without further treatment don't seem to be suitable for standardized stability measurements. (authors)

  19. The Phobos-Grunt microgravity soil preparation system

    Science.gov (United States)

    Yung, Kai-leung; Lam, Chi Wo; Ko, Sui Man; Foster, James Abbott

    2017-12-01

    To understand the composition of regolith on distant bodies it is important to make quantitative measurement of its composition. However, many instruments on board space missions can only make qualitative measurements. The SOil Preparation SYStem (SOPSYS) designed for the Phobos-grunt mission in 2011 was a unique spacecraft subsystem that can grind, sieve, transport and measure samples of regolith in the absence of gravity. Its mission was to produce a compact plug of regolith sample composed of particles no larger than 1 mm for a gas analytic package. It delivers a sample with specified volume enabling a quantitative analysis of the volatiles produced at different temperatures through heating. To minimize cross contamination, SOPSYS self-cleans after each sample is delivered. The apparatus was a cooperative development between China and Russia for the Phobos-Grunt mission to the Martian moon Phobos and will be reused on the upcoming reattempt of that mission and other similar missions. The paper presents an overview of the subsystem and the results of qualification model testing. The flight unit of SOPSYS has a low mass of 622 g including control electronics and compact dimensions of 247 mm by 102 mm by 45 mm.

  20. [Efficiency of the preparation "Ekolan-M" for purification of oil polluted soil].

    Science.gov (United States)

    Nogina, T M; Dumanskaia, T U; Khomenko, L A; Podgorskiĭ, V S

    2012-01-01

    The efficiency of purification of oil contaminated loamy chernozem by the preparation "Ekolan-M" was investigated. During 12 months a complex soil bioremediation using the preparation and alfalfa, as the land-improving plant, at the final stage of purification resulted in the reduction of hydrocarbon content by 97.0%, and without the preparation - by 65.5 %. In the version of experiment with the preparation a 100% decrease of soil phytotoxicity was achieved and a significant stimulation of plant growth and development was observed. The process of soil purification was accompanied by intensive development of hydrocarbon-oxidizing microorganisms, the amount of which during the process of oil concentration gradually decreased, approaching the level in the control uncontaminated soil.

  1. Soil Gas Sample Handling: Evaluation of Water Removal and Sample Ganging

    Energy Technology Data Exchange (ETDEWEB)

    Fritz, Brad G. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Abrecht, David G. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hayes, James C. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Mendoza, Donaldo P. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2016-10-31

    Soil gas sampling is currently conducted in support of Nuclear Test Ban treaty verification. Soil gas samples are collected and analyzed for isotopes of interest. Some issues that can impact sampling and analysis of these samples are excess moisture and sample processing time. Here we discuss three potential improvements to the current sampling protocol; a desiccant for water removal, use of molecular sieve to remove CO2 from the sample during collection, and a ganging manifold to allow composite analysis of multiple samples.

  2. Synchrotron/crystal sample preparation

    Science.gov (United States)

    Johnson, R. Barry

    1993-01-01

    The Center for Applied Optics (CAO) of the University of Alabama in Huntsville (UAH) prepared this final report entitled 'Synchrotron/Crystal Sample Preparation' in completion of contract NAS8-38609, Delivery Order No. 53. Hughes Danbury Optical Systems (HDOS) is manufacturing the Advanced X-ray Astrophysics Facility (AXAF) mirrors. These thin-walled, grazing incidence, Wolter Type-1 mirrors, varying in diameter from 1.2 to 0.68 meters, must be ground and polished using state-of-the-art techniques in order to prevent undue stress due to damage or the presence of crystals and inclusions. The effect of crystals on the polishing and grinding process must also be understood. This involves coating special samples of Zerodur and measuring the reflectivity of the coatings in a synchrotron system. In order to gain the understanding needed on the effect of the Zerodur crystals by the grinding and polishing process, UAH prepared glass samples by cutting, grinding, etching, and polishing as required to meet specifications for witness bars for synchrotron measurements and for investigations of crystals embedded in Zerodur. UAH then characterized these samples for subsurface damage and surface roughness and figure.

  3. Preparing Soil for Turfgrass Establishment - Southern Utah

    OpenAIRE

    Caron, Michael; Schaible, Candace; Heflebower, Rick; Cardon, Grant; Beddes, Taun; Kopp, Kelly

    2017-01-01

    This fact sheet provides information for successfully establishing a lawn including planning, soil preparation, appropriate seed or sod choice, and an understanding of turfgrass requirements in southern Utah.

  4. Sampling depth confounds soil acidification outcomes

    Science.gov (United States)

    In the northern Great Plains (NGP) of North America, surface sampling depths of 0-15 or 0-20 cm are suggested for testing soil characteristics such as pH. However, acidification is often most pronounced near the soil surface. Thus, sampling deeper can potentially dilute (increase) pH measurements an...

  5. Latin Hypercube Sampling (LHS) at variable resolutions for enhanced watershed scale Soil Sampling and Digital Soil Mapping.

    Science.gov (United States)

    Hamalainen, Sampsa; Geng, Xiaoyuan; He, Juanxia

    2017-04-01

    Latin Hypercube Sampling (LHS) at variable resolutions for enhanced watershed scale Soil Sampling and Digital Soil Mapping. Sampsa Hamalainen, Xiaoyuan Geng, and Juanxia, He. AAFC - Agriculture and Agr-Food Canada, Ottawa, Canada. The Latin Hypercube Sampling (LHS) approach to assist with Digital Soil Mapping has been developed for some time now, however the purpose of this work was to complement LHS with use of multiple spatial resolutions of covariate datasets and variability in the range of sampling points produced. This allowed for specific sets of LHS points to be produced to fulfil the needs of various partners from multiple projects working in the Ontario and Prince Edward Island provinces of Canada. Secondary soil and environmental attributes are critical inputs that are required in the development of sampling points by LHS. These include a required Digital Elevation Model (DEM) and subsequent covariate datasets produced as a result of a Digital Terrain Analysis performed on the DEM. These additional covariates often include but are not limited to Topographic Wetness Index (TWI), Length-Slope (LS) Factor, and Slope which are continuous data. The range of specific points created in LHS included 50 - 200 depending on the size of the watershed and more importantly the number of soil types found within. The spatial resolution of covariates included within the work ranged from 5 - 30 m. The iterations within the LHS sampling were run at an optimal level so the LHS model provided a good spatial representation of the environmental attributes within the watershed. Also, additional covariates were included in the Latin Hypercube Sampling approach which is categorical in nature such as external Surficial Geology data. Some initial results of the work include using a 1000 iteration variable within the LHS model. 1000 iterations was consistently a reasonable value used to produce sampling points that provided a good spatial representation of the environmental

  6. [Sample preparation and bioanalysis in mass spectrometry].

    Science.gov (United States)

    Bourgogne, Emmanuel; Wagner, Michel

    2015-01-01

    The quantitative analysis of compounds of clinical interest of low molecular weight (sample preparation. Sample preparation is a crucial part of chemical/biological analysis and in a sense is considered the bottleneck of the whole analytical process. The main objectives of sample preparation are the removal of potential interferences, analyte preconcentration, and converting (if needed) the analyte into a more suitable form for detection or separation. Without chromatographic separation, endogenous compounds, co-eluted products may affect a quantitative method in mass spectrometry performance. This work focuses on three distinct parts. First, quantitative bioanalysis will be defined, different matrices and sample preparation techniques currently used in bioanalysis by mass spectrometry of/for small molecules of clinical interest in biological fluids. In a second step the goals of sample preparation will be described. Finally, in a third step, sample preparation strategies will be made either directly ("dilute and shoot") or after precipitation.

  7. METALLOGRAPHIC SAMPLE PREPARATION STATION-CONSTRUCTIVE CONCEPT

    Directory of Open Access Journals (Sweden)

    AVRAM Florin Timotei

    2016-11-01

    Full Text Available In this paper we propose to present the issues involved in the case of the constructive conception of a station for metallographic sample preparation. This station is destined for laboratory work. The metallographic station is composed of a robot ABB IRB1600, a metallographic microscope, a gripping device, a manipulator, a laboratory grinding and polishing machine. The robot will be used for manipulation of the sample preparation and the manipulator take the sample preparation for processing.

  8. Including Below Detection Limit Samples in Post Decommissioning Soil Sample Analyses

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jung Hwan; Yim, Man Sung [KAIST, Daejeon (Korea, Republic of)

    2016-05-15

    To meet the required standards the site owner has to show that the soil at the facility has been sufficiently cleaned up. To do this one must know the contamination of the soil at the site prior to clean up. This involves sampling that soil to identify the degree of contamination. However there is a technical difficulty in determining how much decontamination should be done. The problem arises when measured samples are below the detection limit. Regulatory guidelines for site reuse after decommissioning are commonly challenged because the majority of the activity in the soil at or below the limit of detection. Using additional statistical analyses of contaminated soil after decommissioning is expected to have the following advantages: a better and more reliable probabilistic exposure assessment, better economics (lower project costs) and improved communication with the public. This research will develop an approach that defines an acceptable method for demonstrating compliance of decommissioned NPP sites and validates that compliance. Soil samples from NPP often contain censored data. Conventional methods for dealing with censored data sets are statistically biased and limited in their usefulness.

  9. Validated sampling strategy for assessing contaminants in soil stockpiles

    International Nuclear Information System (INIS)

    Lame, Frank; Honders, Ton; Derksen, Giljam; Gadella, Michiel

    2005-01-01

    Dutch legislation on the reuse of soil requires a sampling strategy to determine the degree of contamination. This sampling strategy was developed in three stages. Its main aim is to obtain a single analytical result, representative of the true mean concentration of the soil stockpile. The development process started with an investigation into how sample pre-treatment could be used to obtain representative results from composite samples of heterogeneous soil stockpiles. Combining a large number of random increments allows stockpile heterogeneity to be fully represented in the sample. The resulting pre-treatment method was then combined with a theoretical approach to determine the necessary number of increments per composite sample. At the second stage, the sampling strategy was evaluated using computerised models of contaminant heterogeneity in soil stockpiles. The now theoretically based sampling strategy was implemented by the Netherlands Centre for Soil Treatment in 1995. It was applied to all types of soil stockpiles, ranging from clean to heavily contaminated, over a period of four years. This resulted in a database containing the analytical results of 2570 soil stockpiles. At the final stage these results were used for a thorough validation of the sampling strategy. It was concluded that the model approach has indeed resulted in a sampling strategy that achieves analytical results representative of the mean concentration of soil stockpiles. - A sampling strategy that ensures analytical results representative of the mean concentration in soil stockpiles is presented and validated

  10. Preparation of Environmental and Food Samples to Support the Heavy Metals Detection by Stripping Electrochemical

    International Nuclear Information System (INIS)

    Iswani S

    2002-01-01

    Preparation of environmental and food samples to support the heavy metals detection by stripping electrochemistry was done. The water samples taken directly from the ground water were acidified with 1 mL of HNO 3 acic suprapure was not digested, while the soils samples which have already dried in the oven at 105 o C, ware grinded and sieved through 150 μm, werte digested with HNO 3 acic suprapure in the digestion bomb at 150 o C for 3-4 hours. The mussels samples which have already freezed in the freezer were peeled, dried with N 2 liquid, grinded and dried again in the freeze drier at the pressure of ≅ 10 -2 mBar, and then were grinded again, weighted, digested with HNO 3 acic and HClO 4 suprapure in the digestion bomb at 150 o C for 3 hours. Food samples were homogenized by electric mixer, dried with freeze dried, homogenized again by using ZrO 2 ball mill, weighted, digested by HPA (high Pressure Asher). The heavy metals in the food samples solution of digestion product were detected by using Polarographic Analyzer EGandG of SWV and DPASV methods, while in the water, soils and the mussels solution were detected by using PDV 2000 and Polarograf E-505, DPASV method. The method validity were tested with SRM materials such as soil-5, soil-7, water W-4, and coppepoda. The heavy metals detection results in the water, soils, mussels, and food by electrochemical method were reported in this paper. (author)

  11. Sample preparation guidelines for two-dimensional electrophoresis.

    Science.gov (United States)

    Posch, Anton

    2014-12-01

    Sample preparation is one of the key technologies for successful two-dimensional electrophoresis (2DE). Due to the great diversity of protein sample types and sources, no single sample preparation method works with all proteins; for any sample the optimum procedure must be determined empirically. This review is meant to provide a broad overview of the most important principles in sample preparation in order to avoid a multitude of possible pitfalls. Sample preparation protocols from the expert in the field were screened and evaluated. On the basis of these protocols and my own comprehensive practical experience important guidelines are given in this review. The presented guidelines will facilitate straightforward protocol development for researchers new to gel-based proteomics. In addition the available choices are rationalized in order to successfully prepare a protein sample for 2DE separations. The strategies described here are not limited to 2DE and can also be applied to other protein separation techniques.

  12. 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

  13. Soil Sampling Operating Procedure

    Science.gov (United States)

    EPA Region 4 Science and Ecosystem Support Division (SESD) document that describes general and specific procedures, methods, and considerations when collecting soil samples for field screening or laboratory analysis.

  14. A simple and automated sample preparation system for subsequent halogens determination: Combustion followed by pyrohydrolysis.

    Science.gov (United States)

    Pereira, L S F; Pedrotti, M F; Vecchia, P Dalla; Pereira, J S F; Flores, E M M

    2018-06-20

    A simple and automated system based on combustion followed by a pyrohydrolysis reaction was proposed for further halogens determination. This system was applied for digestion of soils containing high (90%) and also low (10%) organic matter content for further halogens determination. The following parameters were evaluated: sample mass, use of microcrystalline cellulose and heating time. For analytes absorption, a diluted alkaline solution (6 mL of 25 mmol L -1  NH 4 OH) was used in all experiments. Up to 400 mg of soil with high organic matter content and 100 mg of soil with low organic matter content (mixed with 400 mg of cellulose) could be completely digested using the proposed system. Quantitative results for all halogens were obtained using less than 12 min of sample preparation step (about 1.8 min for sample combustion and 10 min for pyrohydrolysis). The accuracy was evaluated using a certified reference material of coal and spiked samples. No statistical difference was observed between the certified values and results obtained by the proposed method. Additionally, the recoveries obtained using spiked samples were in the range of 98-103% with relative standard deviation values lower than 5%. The limits of quantification obtained for F, Cl, Br and I for soil with high (400 mg of soil) and low (100 mg of soil) organic matter were in the range of 0.01-2 μg g -1 and 0.07-59 μg g -1 , respectively. The proposed system was considered as a simple and suitable alternative for soils digestion for further halogens determination by ion chromatography and inductively coupled plasma mass spectrometry techniques. Copyright © 2018 Elsevier B.V. All rights reserved.

  15. Sampling soils for transuranic nuclides: a review

    International Nuclear Information System (INIS)

    Fowler, E.B.; Essington, E.H.

    1976-01-01

    A review of the literature pertinent to the sampling of soils for radionuclides is presented; emphasis is placed on transuranic nuclides. Sampling of soils is discussed relative to systems of heterogeneous distributions and varied particle sizes encountered in certain environments. Sampling methods that have been used for two different sources of contamination, global fallout, and accidental or operational releases, are included

  16. Laser ablation inductively coupled plasma mass spectrometry analysis of agricultural soils using the sol-gel technique of pellet preparation

    International Nuclear Information System (INIS)

    Hubova, I.; Hola, M.; Vaculovic, T.; Pinkas, J.; Prokes, L.; Stefan, I.; Kanicky, V.

    2009-01-01

    Full text: Monitoring of metals in agricultural soils is gaining importance as they are accumulated by plants. A LAICPQMS method with Nd:YAG 213 nm laser has been developed for determination of Cr, Ni, Cu, Zn and Pb in soil pellets prepared by the sol-gel technique. LA-ICPMS analysis of archive samples was verified by XRF of wax-soil pellets and ICPMS with nebulization of solutions obtained by total soil decomposition and by analysis of reference materials. Sequention extraction was used for fractionation analysis. (author)

  17. Determination of strontium-90 in soil samples

    Energy Technology Data Exchange (ETDEWEB)

    Chang, C C

    1976-06-01

    The determination of /sup 90/Sr in soil by tri-n-butyl phosphate (TBP) is often interfered with iron which is always present in soil sample. Based on the method given by the U.S. Environmental Protection Agency, HClO/sub 4/ is added to remove iron ions while the soil sample is analyzed with TBP. The effect of different concentrations of HClO/sub 4/ on extraction yield of iron and chemical yield of yttrium is investigated. The experimental results show that 2N HClO/sub 4/ is the optimum concentration. The chemical yield of yttrium can reach about 60 percent, and all iron ions can be removed. This method has successfully been applied to analyze the soil samples taken from the site of the nuclear power plant in North Taiwan.

  18. Soil separator and sampler and method of sampling

    Science.gov (United States)

    O'Brien, Barry H [Idaho Falls, ID; Ritter, Paul D [Idaho Falls, ID

    2010-02-16

    A soil sampler includes a fluidized bed for receiving a soil sample. The fluidized bed may be in communication with a vacuum for drawing air through the fluidized bed and suspending particulate matter of the soil sample in the air. In a method of sampling, the air may be drawn across a filter, separating the particulate matter. Optionally, a baffle or a cyclone may be included within the fluidized bed for disentrainment, or dedusting, so only the finest particulate matter, including asbestos, will be trapped on the filter. The filter may be removable, and may be tested to determine the content of asbestos and other hazardous particulate matter in the soil sample.

  19. Sampling for validation of digital soil maps

    NARCIS (Netherlands)

    Brus, D.J.; Kempen, B.; Heuvelink, G.B.M.

    2011-01-01

    The increase in digital soil mapping around the world means that appropriate and efficient sampling strategies are needed for validation. Data used for calibrating a digital soil mapping model typically are non-random samples. In such a case we recommend collection of additional independent data and

  20. Application of radiochemical methods for development of new biological preparation designed for soil bioremediation

    International Nuclear Information System (INIS)

    Kim, A.A.; Djuraeva, G.T.; Djumaniyazova, G.I.; Yadgarov, Kh.T.

    2006-01-01

    Full text: Internationally the bioremediation of agricultural lands contaminated by persistent chloroorganic compounds by means of the microbial methods are used as the most low-cost and the most effective. One of the factors reducing efficacy of microbial degradation, is often the low quantity of microorganisms - destructors in the soil. Therefore, we have designed bioremediation technology of soils, contaminated by organochlorine compounds, with use of the alive microorganisms as active agent. We developed the biological preparation containing 5 aboriginal active strains of bacteria - destructors of persistent chloroorganic compounds and investigated the ability of biological preparation to increase the bioremediation potential of contaminated soils. To carry out the investigation we developed the complex of radiochemical methods with use of tritium labeled PCBs, including the following methods: 1.The method to define the accumulation and degradation of PCBs in soil bacteria in culture allows determination of quantitative characteristics of bacterial strains. 2. The method to define the PCBs degradation by soil bacteria strains in model conditions in the soil allows to estimate the PCB-destructive activity of strains after introducing in soil. 3. A method to define the PCB-destructive activity of own microbiota of contaminated soil. 4. A method to define the effect of stimulation of the PCB-destructive activity of biological preparation and own microbiota of soil with the help of biofertilizers. By using the developed radiochemical methods we have carried out investigation on creation of new biological preparation on the basis of strains of soil bacteria - destructors of PCBs. We also determined the quality and quantity characteristics of HCCH and PCBs-destructive activity of new biological preparation. It is shown that the new biological preparation is capable of accumulation and destruction of the PCBs in culture and in soil at model conditions. Thus, the

  1. Microfluidic Sample Preparation for Diagnostic Cytopathology

    Science.gov (United States)

    Mach, Albert J.; Adeyiga, Oladunni B.; Di Carlo, Dino

    2014-01-01

    The cellular components of body fluids are routinely analyzed to identify disease and treatment approaches. While significant focus has been placed on developing cell analysis technologies, tools to automate the preparation of cellular specimens have been more limited, especially for body fluids beyond blood. Preparation steps include separating, concentrating, and exposing cells to reagents. Sample preparation continues to be routinely performed off-chip by technicians, preventing cell-based point-of-care diagnostics, increasing the cost of tests, and reducing the consistency of the final analysis following multiple manually-performed steps. Here, we review the assortment of biofluids for which suspended cells are analyzed, along with their characteristics and diagnostic value. We present an overview of the conventional sample preparation processes for cytological diagnosis. We finally discuss the challenges and opportunities in developing microfluidic devices for the purpose of automating or miniaturizing these processes, with particular emphases on preparing large or small volume samples, working with samples of high cellularity, automating multi-step processes, and obtaining high purity subpopulations of cells. We hope to convey the importance of and help identify new research directions addressing the vast biological and clinical applications in preparing and analyzing the array of available biological fluids. Successfully addressing the challenges described in this review can lead to inexpensive systems to improve diagnostic accuracy while simultaneously reducing overall systemic healthcare costs. PMID:23380972

  2. Determination of mercury in ash and soil samples by oxygen flask combustion method-Cold vapor atomic fluorescence spectrometry (CVAFS)

    International Nuclear Information System (INIS)

    Geng Wenhua; Nakajima, Tsunenori; Takanashi, Hirokazu; Ohki, Akira

    2008-01-01

    A simple method was developed for the determination of mercury (Hg) in coal fly ash (CFA), waste incineration ash (WIA), and soil by use of oxygen flask combustion (OFC) followed by cold vapor atomic fluorescence spectrometry (CVAFS). A KMnO 4 solution was used as an absorbent in the OFC method, and the sample containing a combustion agent and an ash or soil sample was combusted by the OFC method. By use of Hg-free graphite as the combustion agent, the determination of Hg in ash and soil was successfully carried out; the Hg-free graphite was prepared by use of a mild pyrolysis procedure at 500 deg. C. For six certified reference materials (three CFA samples and three soil samples), the values of Hg obtained by this method were in good agreement with the certified or reference values. In addition, real samples including nine CFAs collected from some coal-fired power plants, five WIAs collected from waste incineration plants, and two soils were analyzed by the present method, and the data were compared to those from microwave-acid digestion (MW-AD) method

  3. 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.

  4. 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.

  5. Soil sampling strategies: Evaluation of different approaches

    Energy Technology Data Exchange (ETDEWEB)

    De Zorzi, Paolo [Agenzia per la Protezione dell' Ambiente e per i Servizi Tecnici (APAT), Servizio Metrologia Ambientale, Via di Castel Romano, 100-00128 Roma (Italy)], E-mail: paolo.dezorzi@apat.it; Barbizzi, Sabrina; Belli, Maria [Agenzia per la Protezione dell' Ambiente e per i Servizi Tecnici (APAT), Servizio Metrologia Ambientale, Via di Castel Romano, 100-00128 Roma (Italy); Mufato, Renzo; Sartori, Giuseppe; Stocchero, Giulia [Agenzia Regionale per la Prevenzione e Protezione dell' Ambiente del Veneto, ARPA Veneto, U.O. Centro Qualita Dati, Via Spalato, 14-36045 Vicenza (Italy)

    2008-11-15

    The National Environmental Protection Agency of Italy (APAT) performed a soil sampling intercomparison, inviting 14 regional agencies to test their own soil sampling strategies. The intercomparison was carried out at a reference site, previously characterised for metal mass fraction distribution. A wide range of sampling strategies, in terms of sampling patterns, type and number of samples collected, were used to assess the mean mass fraction values of some selected elements. The different strategies led in general to acceptable bias values (D) less than 2{sigma}, calculated according to ISO 13258. Sampling on arable land was relatively easy, with comparable results between different sampling strategies.

  6. Soil sampling strategies: Evaluation of different approaches

    International Nuclear Information System (INIS)

    De Zorzi, Paolo; Barbizzi, Sabrina; Belli, Maria; Mufato, Renzo; Sartori, Giuseppe; Stocchero, Giulia

    2008-01-01

    The National Environmental Protection Agency of Italy (APAT) performed a soil sampling intercomparison, inviting 14 regional agencies to test their own soil sampling strategies. The intercomparison was carried out at a reference site, previously characterised for metal mass fraction distribution. A wide range of sampling strategies, in terms of sampling patterns, type and number of samples collected, were used to assess the mean mass fraction values of some selected elements. The different strategies led in general to acceptable bias values (D) less than 2σ, calculated according to ISO 13258. Sampling on arable land was relatively easy, with comparable results between different sampling strategies

  7. Soil sampling strategies: evaluation of different approaches.

    Science.gov (United States)

    de Zorzi, Paolo; Barbizzi, Sabrina; Belli, Maria; Mufato, Renzo; Sartori, Giuseppe; Stocchero, Giulia

    2008-11-01

    The National Environmental Protection Agency of Italy (APAT) performed a soil sampling intercomparison, inviting 14 regional agencies to test their own soil sampling strategies. The intercomparison was carried out at a reference site, previously characterised for metal mass fraction distribution. A wide range of sampling strategies, in terms of sampling patterns, type and number of samples collected, were used to assess the mean mass fraction values of some selected elements. The different strategies led in general to acceptable bias values (D) less than 2sigma, calculated according to ISO 13258. Sampling on arable land was relatively easy, with comparable results between different sampling strategies.

  8. Sampling soils for 137Cs using various field-sampling volumes

    International Nuclear Information System (INIS)

    Nyhan, J.W.; Schofield, T.G.; White, G.C.; Trujillo, G.

    1981-10-01

    The sediments from a liquid effluent receiving area at the Los Alamos National Laboratory and soils from intensive study area in the fallout pathway of Trinity were sampled for 137 Cs using 25-, 500-, 2500-, and 12 500-cm 3 field sampling volumes. A highly replicated sampling program was used to determine mean concentrations and inventories of 137 Cs at each site, as well as estimates of spatial, aliquoting, and counting variance components of the radionuclide data. The sampling methods were also analyzed as a function of soil size fractions collected in each field sampling volume and of the total cost of the program for a given variation in the radionuclide survey results. Coefficients of variation (CV) of 137 Cs inventory estimates ranged from 0.063 to 0.14 for Mortandad Canyon sediments, where CV values for Trinity soils were observed from 0.38 to 0.57. Spatial variance components of 137 Cs concentration data were usually found to be larger than either the aliquoting or counting variance estimates and were inversely related to field sampling volume at the Trinity intensive site. Subsequent optimization studies of the sampling schemes demonstrated that each aliquot should be counted once, and that only 2 to 4 aliquots out of an many as 30 collected need be assayed for 137 Cs. The optimization studies showed that as sample costs increased to 45 man-hours of labor per sample, the variance of the mean 137 Cs concentration decreased dramatically, but decreased very little with additional labor

  9. Novel Sample-handling Approach for XRD Analysis with Minimal Sample Preparation

    Science.gov (United States)

    Sarrazin, P.; Chipera, S.; Bish, D.; Blake, D.; Feldman, S.; Vaniman, D.; Bryson, C.

    2004-01-01

    Sample preparation and sample handling are among the most critical operations associated with X-ray diffraction (XRD) analysis. These operations require attention in a laboratory environment, but they become a major constraint in the deployment of XRD instruments for robotic planetary exploration. We are developing a novel sample handling system that dramatically relaxes the constraints on sample preparation by allowing characterization of coarse-grained material that would normally be impossible to analyze with conventional powder-XRD techniques.

  10. Preparation, Characterization, and UV Irradiation of Mars Soil Analogues Under Simulated Martian Conditions to Support Detection of Molecular Biomarkers

    Science.gov (United States)

    Fornaro, T.; Brucato, J. R.; ten Kate, I. L.; Siljeström, S.; Steele, A.; Cody, G. D.; Hazen, R. M.

    2018-04-01

    We present laboratory activities of preparation, characterization, and UV irradiation processing of Mars soil analogues, which are key to support both in situ exploration and sample return missions devoted to detection of molecular biomarkers on Mars.

  11. Diffusion probe for gas sampling in undisturbed soil

    DEFF Research Database (Denmark)

    Petersen, Søren O

    2014-01-01

    Soil-atmosphere fluxes of trace gases such as methane (CH4) and nitrous oxide (N2O) are determined by complex interactions between biological activity and soil conditions. Soil gas concentration profiles may, in combination with other information about soil conditions, help to understand emission...... controls. This note describes a simple and robust diffusion probe for soil gas sampling as part of flux monitoring programs. It can be deployed with minimum disturbance of in-situ conditions, also at sites with a high or fluctuating water table. Separate probes are used for each sampling depth...... on peat soils used for grazing showed soil gas concentrations of CH4 and N2O as influenced by topography, site conditions, and season. The applicability of the diffusion probe for trace gas monitoring is discussed....

  12. Ultrasonic assisted extraction - an alternative for sample preparation (M4)

    International Nuclear Information System (INIS)

    Santos Junior, P.; Barbosa Junior, F.; Krug, F.J.; Trevizan, L.C.; Nobrega, J.A.

    2002-01-01

    Full text: In the last years the ultrasound assisted metal extraction has been frequency proposed as a simple and inexpensive alternative for sample preparation of biological and inorganic samples. The extraction effect is considered as being caused by acoustic cavitation, that is, bubble formation and subsequent disruptive action. The collapse of bubbles created by sonication of solutions results in the generation of extremely high local temperature and pressure gradients, which may be regarded as localized 'hot spots'. On a timescale of about 10 -10 s, effective local pressures and temperature of about 10 5 atm and about 5000 K, respectively, are generated under sonochemical conditions. Usually, this method uses a diluted acid medium decreasing blank values and reducing both reagents and time consumption compared to traditional wet digestion systems using conductive or microwave-assisted heating. Furthermore, sonication can also allow the preparation of samples directly within the sample container, thereby preventing sample losses and minimizing sample contamination. Although some controversial results concerning metals extraction behavior have been reported, they could be explained by analyte-matrix interaction and the ability of the ultrasonic processor to generate ultrasound (i.e. the use of an ultrasonic bath or an ultrasonic probe at different power, frequency, and amplitude). This contribution presents a review of ultrasound assisted metal extraction and recent performance data obtained in our laboratory for determination of elements in biological materials, soils and sediments by ICP-OES and ETAAS. The effect of extraction parameters, such as type and concentration of the leaching solution, sonication time and performance of ultrasonic processor (bath or probe) will be presented. (author)

  13. 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.

  14. Sampling and analysis plan for assessment of beryllium in soils surrounding TA-40 building 15

    Energy Technology Data Exchange (ETDEWEB)

    Ruedig, Elizabeth [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2016-12-19

    Technical Area (TA) 40 Building 15 (40-15) is an active firing site at Los Alamos National Laboratory. The weapons facility operations (WFO) group plans to build an enclosure over the site in 2017, so that test shots may be conducted year-round. The enclosure project is described in PRID 16P-0209. 40-15 is listed on LANL OSH-ISH’s beryllium inventory, which reflects the potential for beryllium in/on soils and building surfaces at 40-15. Some areas in and around 40-15 have previously been sampled for beryllium, but past sampling efforts did not achieve complete spatial coverage of the area. This Sampling and Analysis Plan (SAP) investigates the area surrounding 40-15 via 9 deep (≥1-ft.) soil samples and 11 shallow (6-in.) soil samples. These samples will fill the spatial data gaps for beryllium at 40-15, and will be used to support OSH-ISH’s final determination of 40-15’s beryllium registry status. This SAP has been prepared by the Environmental Health Physics program in consultation with the Industrial Hygiene program. Industrial Hygiene is the owner of LANL’s beryllium program, and will make a final determination with regard to the regulatory status of beryllium at 40-15.

  15. Analysis of soil samples from OMRE decommissioning project

    International Nuclear Information System (INIS)

    Simpson, O.D.; Chapin, J.A.; Hine, R.E.; Mandler, J.W.; Orme, M.P.; Soli, G.A.

    1979-01-01

    In order to establish that the present Organic Moderated Reactor Experiment (OMRE) site does not exceed the criteria for radioactive contamination, samples obtained from the remainder of the facility that was not removed such as soil, concrete pads, various structural materials, and the leach pond area were analyzed to determine their radioactive content. The results of the analyses performed on soil samples are presented. Results of this study indicate that the activity at the OMRE decommissioned area is confined to localized areas (i.e., the leach pond area and reactor area). Comparisons of radionuclide concentrations measured in soil taken from the lip of the leach pond with concentrations in soil obtained outside the Idaho National Engineering Laboratory (INEL) site boundaries indicate that the concentration in the soil at the edge of the leach pond is at background levels. The vertical augering technique was determined to be the best approach for obtaining shallow soil samples at the INEL. Selection of this technique was based on ease of operation and analytical results. Less area is disturbed per sample than with the horizontal trenching and coring techniques. The radionuclide analysis of the samples shows the existence of a few regions in the reactor and leach pond areas that were still above INEL release criteria. These regions have been or are being further decontaminated

  16. A soil sampling reference site: The challenge in defining reference material for sampling

    International Nuclear Information System (INIS)

    De Zorzi, Paolo; Barbizzi, Sabrina; Belli, Maria; Fajgelj, Ales; Jacimovic, Radojko; Jeran, Zvonka; Sansone, Umberto; Perk, Marcel van der

    2008-01-01

    In the frame of the international SOILSAMP project, funded and coordinated by the Italian Environmental Protection Agency, an agricultural area was established as a reference site suitable for performing soil sampling inter-comparison exercises. The reference site was characterized for trace element content in soil, in terms of the spatial and temporal variability of their mass fraction. Considering that the behaviour of long-lived radionuclides in soil can be expected to be similar to that of some stable trace elements and that the distribution of these trace elements in soil can simulate the distribution of radionuclides, the reference site characterised in term of trace elements, can be also used to compare the soil sampling strategies developed for radionuclide investigations

  17. A soil sampling reference site: The challenge in defining reference material for sampling

    Energy Technology Data Exchange (ETDEWEB)

    De Zorzi, Paolo [Agenzia per la Protezione dell' Ambiente e per i Servizi Tecnici (APAT), Servizio Metrologia Ambientale, Via di Castel Romano, Rome 100-00128 (Italy)], E-mail: paolo.dezorzi@apat.it; Barbizzi, Sabrina; Belli, Maria [Agenzia per la Protezione dell' Ambiente e per i Servizi Tecnici (APAT), Servizio Metrologia Ambientale, Via di Castel Romano, Rome 100-00128 (Italy); Fajgelj, Ales [International Atomic Energy Agency (IAEA), Agency' s Laboratories Seibersdorf, Vienna A-1400 (Austria); Jacimovic, Radojko; Jeran, Zvonka; Sansone, Umberto [Jozef Stefan Institute, Jamova 39, Ljubljana 1000 (Slovenia); Perk, Marcel van der [Department of Physical Geography, Utrecht University, P.O. Box 80115, TC Utrecht 3508 (Netherlands)

    2008-11-15

    In the frame of the international SOILSAMP project, funded and coordinated by the Italian Environmental Protection Agency, an agricultural area was established as a reference site suitable for performing soil sampling inter-comparison exercises. The reference site was characterized for trace element content in soil, in terms of the spatial and temporal variability of their mass fraction. Considering that the behaviour of long-lived radionuclides in soil can be expected to be similar to that of some stable trace elements and that the distribution of these trace elements in soil can simulate the distribution of radionuclides, the reference site characterised in term of trace elements, can be also used to compare the soil sampling strategies developed for radionuclide investigations.

  18. A soil sampling reference site: the challenge in defining reference material for sampling.

    Science.gov (United States)

    de Zorzi, Paolo; Barbizzi, Sabrina; Belli, Maria; Fajgelj, Ales; Jacimovic, Radojko; Jeran, Zvonka; Sansone, Umberto; van der Perk, Marcel

    2008-11-01

    In the frame of the international SOILSAMP project, funded and coordinated by the Italian Environmental Protection Agency, an agricultural area was established as a reference site suitable for performing soil sampling inter-comparison exercises. The reference site was characterized for trace element content in soil, in terms of the spatial and temporal variability of their mass fraction. Considering that the behaviour of long-lived radionuclides in soil can be expected to be similar to that of some stable trace elements and that the distribution of these trace elements in soil can simulate the distribution of radionuclides, the reference site characterised in term of trace elements, can be also used to compare the soil sampling strategies developed for radionuclide investigations.

  19. Sample sizes to control error estimates in determining soil bulk density in California forest soils

    Science.gov (United States)

    Youzhi Han; Jianwei Zhang; Kim G. Mattson; Weidong Zhang; Thomas A. Weber

    2016-01-01

    Characterizing forest soil properties with high variability is challenging, sometimes requiring large numbers of soil samples. Soil bulk density is a standard variable needed along with element concentrations to calculate nutrient pools. This study aimed to determine the optimal sample size, the number of observation (n), for predicting the soil bulk density with a...

  20. Method for spiking soil samples with organic compounds

    DEFF Research Database (Denmark)

    Brinch, Ulla C; Ekelund, Flemming; Jacobsen, Carsten S

    2002-01-01

    We examined the harmful side effects on indigenous soil microorganisms of two organic solvents, acetone and dichloromethane, that are normally used for spiking of soil with polycyclic aromatic hydrocarbons for experimental purposes. The solvents were applied in two contamination protocols to either...... higher than in control soil, probably due mainly to release of predation from indigenous protozoa. In order to minimize solvent effects on indigenous soil microorganisms when spiking native soil samples with compounds having a low water solubility, we propose a common protocol in which the contaminant...... tagged with luxAB::Tn5. For both solvents, application to the whole sample resulted in severe side effects on both indigenous protozoa and bacteria. Application of dichloromethane to the whole soil volume immediately reduced the number of protozoa to below the detection limit. In one of the soils...

  1. Analysis of core samples from jet grouted soil

    International Nuclear Information System (INIS)

    Allan, M.L.; Kukacka, L.E.

    1995-10-01

    Superplasticized cementitious grouts were tested for constructing subsurface containment barriers using jet grouting in July, 1994. The grouts were developed in the Department of Applied Science at Brookhaven National Laboratory. The test site was located close to the Chemical Waste Landfill at Sandia National Laboratories, Albuquerque, NM. Sandia was responsible for the placement contract. The jet grouted soil was exposed to the service environment for one year and core samples were extracted to evaluate selected properties. The cores were tested for strength, density, permeability (hydraulic conductivity) and cementitious content. The tests provided an opportunity to determine the performance of the grouts and grout-treated soil. Several recommendations arise from the results of the core tests. These are: (1) grout of the same mix proportions as the final grout should be used as a drilling fluid in order to preserve the original mix design and utilize the benefits of superplasticizers; (2) a high shear mixer should be used for preparation of the grout; (3) the permeability under unsaturated conditions requires consideration when subsurface barriers are used in the vadose zone; and (4) suitable methods for characterizing the permeability of barriers in-situ should be applied

  2. Sampling of soils for transuranic nuclides: a review

    International Nuclear Information System (INIS)

    Fowler, E.B.; Essington, E.H.

    1977-01-01

    A review of the literature pertinent to the sampling of soils for radionuclides is presented; emphasis is placed on transuranic nuclides. Sampling of soils is discussed relative to systems of heterogeneous distributions and varied particle sizes encountered in certain environments. Sampling methods that have been used for two different sources of contamination, global fallout, and accidental or operational releases, are included

  3. Analysis of Mars Analogue Soil Samples Using Solid-Phase Microextraction, Organic Solvent Extraction and Gas Chromatography/Mass Spectrometry

    Science.gov (United States)

    Orzechowska, G. E.; Kidd, R. D.; Foing, B. H.; Kanik, I.; Stoker, C.; Ehrenfreund, P.

    2011-01-01

    Polycyclic aromatic hydrocarbons (PAHs) are robust and abundant molecules in extraterrestrial environments. They are found ubiquitously in the interstellar medium and have been identified in extracts of meteorites collected on Earth. PAHs are important target molecules for planetary exploration missions that investigate the organic inventory of planets, moons and small bodies. This study is part of an interdisciplinary preparation phase to search for organic molecules and life on Mars. We have investigated PAH compounds in desert soils to determine their composition, distribution and stability. Soil samples (Mars analogue soils) were collected at desert areas of Utah in the vicinity of the Mars Desert Research Station (MDRS), in the Arequipa region in Peru and from the Jutland region of Denmark. The aim of this study was to optimize the solid-phase microextraction (SPME) method for fast screening and determination of PAHs in soil samples. This method minimizes sample handling and preserves the chemical integrity of the sample. Complementary liquid extraction was used to obtain information on five- and six-ring PAH compounds. The measured concentrations of PAHs are, in general, very low, ranging from 1 to 60 ng g(sup -1). The texture of soils is mostly sandy loam with few samples being 100% silt. Collected soils are moderately basic with pH values of 8-9 except for the Salten Skov soil, which is slightly acidic. Although the diverse and variable microbial populations of the samples at the sample sites might have affected the levels and variety of PAHs detected, SPME appears to be a rapid, viable field sampling technique with implications for use on planetary missions.

  4. Soil Gas Sampling Operating Procedure

    Science.gov (United States)

    EPA Region 4 Science and Ecosystem Support Division (SESD) document that describes general and specific procedures, methods, and considerations when collecting soil gas samples for field screening or laboratory analysis.

  5. Green approaches in sample preparation of bioanalytical samples prior to chromatographic analysis.

    Science.gov (United States)

    Filippou, Olga; Bitas, Dimitrios; Samanidou, Victoria

    2017-02-01

    Sample preparation is considered to be the most challenging step of the analytical procedure, since it has an effect on the whole analytical methodology, therefore it contributes significantly to the greenness or lack of it of the entire process. The elimination of the sample treatment steps, pursuing at the same time the reduction of the amount of the sample, strong reductions in consumption of hazardous reagents and energy also maximizing safety for operators and environment, the avoidance of the use of big amount of organic solvents, form the basis for greening sample preparation and analytical methods. In the last decade, the development and utilization of greener and sustainable microextraction techniques is an alternative to classical sample preparation procedures. In this review, the main green microextraction techniques (solid phase microextraction, stir bar sorptive extraction, hollow-fiber liquid phase microextraction, dispersive liquid - liquid microextraction, etc.) will be presented, with special attention to bioanalytical applications of these environment-friendly sample preparation techniques which comply with the green analytical chemistry principles. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Quantitative sample preparation of some heavy elements

    International Nuclear Information System (INIS)

    Jaffey, A.H.

    1977-01-01

    A discussion is given of some techniques that have been useful in quantitatively preparing and analyzing samples used in the half-life determinations of some plutonium and uranium isotopes. Application of these methods to the preparation of uranium and plutonium samples used in neutron experiments is discussed

  7. Determining photon energy absorption parameters for different soil samples

    International Nuclear Information System (INIS)

    Kucuk, Nil; Cakir, Merve; Tumsavas, Zeynal

    2013-01-01

    The mass attenuation coefficients (μ s ) for five different soil samples were measured at 661.6, 1173.2 and 1332.5 keV photon energies. The soil samples were separately irradiated with 137 Cs and 60 Co (370 kBq) radioactive point gamma sources. The measurements were made by performing transmission experiments with a 2″ x 2″ NaI(Tl) scintillation detector, which had an energy resolution of 7% at 0.662 MeV for the gamma-rays from the decay of 137 Cs. The effective atomic numbers (Z eff ) and the effective electron densities (N eff ) were determined experimentally and theoretically using the obtained μ s values for the soil samples. Furthermore, the Z eff and N eff values of the soil samples were computed for the total photon interaction cross-sections using theoretical data over a wide energy region ranging from 1 keV to 15 MeV. The experimental values of the soils were found to be in good agreement with the theoretical values. Sandy loam and sandy clay loam soils demonstrated poor photon energy absorption characteristics. However, clay loam and clay soils had good photon energy absorption characteristics. (author)

  8. 7 CFR 27.21 - Preparation of samples of cotton.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 2 2010-01-01 2010-01-01 false Preparation of samples of cotton. 27.21 Section 27.21... REGULATIONS COTTON CLASSIFICATION UNDER COTTON FUTURES LEGISLATION Regulations Inspection and Samples § 27.21 Preparation of samples of cotton. The samples from each bale shall be prepared as specified in this section...

  9. Shrinkage Module of Soil Samples with Different Cement Content

    Directory of Open Access Journals (Sweden)

    Mohannad Sabry

    2017-12-01

    Full Text Available The differences in soil's body mass during shrinkage over time have changes in soil physical properties which provide an important reason to check the design of underground foundations in expansive soils. In this paper, a state-of-art of the soil heat stress-strain relationship prediction methods is checked using soil engineering laboratory experiments and Matlab R2013b numerical modelling. The shrinkage of soils with different cement content of (0%, 2%, 4%, 6% and 8% with the same water content of 20 percent in room temperature for 24 hours, are critically reviewed in terms of their predictive shrinkage along with their strengths and flexural behaviour. The review highlights the prediction methods present to determine the effect of heat stress on the shrinkage of soil samples with different cement content after classifying the soils into clay, silt and sand depending on their particle size using sieve and hydrometer experiments. The results of the soil engineering laboratory experiments showed that as the cement content increases, the shrinkage of soil decreases as a result of increased elasticity in soil. The numerical analysis using finite element method in Matlab R2013b shows that as the cement content increases the displacement in the soil sample decreases and that the soil sample with 8% cement content has more resistance to shrinkage and less displacement than the soil with 6% cement, which has less resistance to heat stresses and more displacement.

  10. Sample preparation in alkaline media

    International Nuclear Information System (INIS)

    Nobrega, Joaquim A.; Santos, Mirian C.; Sousa, Rafael A. de; Cadore, Solange; Barnes, Ramon M.; Tatro, Mark

    2006-01-01

    The use of tetramethylammonium hydroxide, tertiary amines and strongly alkaline reagents for sample treatment involving extraction and digestion procedures is discussed in this review. The preparation of slurries is also discussed. Based on literature data, alkaline media offer a good alternative for sample preparation involving an appreciable group of analytes in different types of samples. These reagents are also successfully employed in tailored speciation procedures wherein there is a critical dependence on maintenance of chemical forms. The effects of these reagents on measurements performed using spectroanalytical techniques are discussed. Several undesirable effects on transport and atomization processes necessitate use of the method of standard additions to obtain accurate results. It is also evident that alkaline media can improve the performance of techniques such as inductively coupled plasma mass spectrometry and accessories, such as autosamplers coupled to graphite furnace atomic absorption spectrometers

  11. Urine sample preparation for proteomic analysis.

    Science.gov (United States)

    Olszowy, Pawel; Buszewski, Boguslaw

    2014-10-01

    Sample preparation for both environmental and more importantly biological matrices is a bottleneck of all kinds of analytical processes. In the case of proteomic analysis this element is even more important due to the amount of cross-reactions that should be taken into consideration. The incorporation of new post-translational modifications, protein hydrolysis, or even its degradation is possible as side effects of proteins sample processing. If protocols are evaluated appropriately, then identification of such proteins does not bring difficulties. However, if structural changes are provided without sufficient attention then protein sequence coverage will be reduced or even identification of such proteins could be impossible. This review summarizes obstacles and achievements in protein sample preparation of urine for proteome analysis using different tools for mass spectrometry analysis. The main aim is to present comprehensively the idea of urine application as a valuable matrix. This article is dedicated to sample preparation and application of urine mainly in novel cancer biomarkers discovery. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Elemental contents in soil samples in Wad Hamid, River Nile State

    International Nuclear Information System (INIS)

    Mohammed, Khansaa Elawad Elhag

    2016-03-01

    In the present study a total of 30 samples were collected from Wad Hamid River Nile State. Sampling area of (two feddan) of agricultural soil. The sampling area was divided in two locations (fertile and non fertile soil). The samples were analyzed for their content of 13 elements (K, Ca, Ti, Mn, Fe, Cu, Zn, Pb, Rb, Sr, Y, Zr, and Np). 10 samples from location 1 (non-fertile soil) and 20 samples from location 2 (fertile soil). X-ray fluorescence (X RF) Spectrometer (system used based on 1"0"9"Cd excitation 1"0"9"Cd source which has an average energy of 22.6 kev and able to excite the elements from Z = 13 to 92 using K and L lines) used to identify the elemental concentration in soil samples. The reliability of X RF technique as multi elements detecting method for measuring elements concentration in soil sample , (IAEA-SOIL-7) standard reference material was used. Measured values found in agreement with the certified values. The average elemental concentration of K,Ca, Ti, Fe, Cu, Zn, Pb, Sr, Y, Zr, and Np in location 1 were 878, 29690, 13400, 983, 70380, 10.07, 19.07, 40.92,261.4, 23.59,294.8, 47.82, while the average elemental concentration in location 2 were 9848, 27780, 13076,13076,989, 68135, 9.6, 96.3 19.86, 43.7, 225.5, 22.49, 284.75, 46.15, respectively. comparison between the average elemental concentration in fertile soil and non-fertile was done correlations between element were performed Cluster analyses of element in soil samples were obtained comparison between this study and data from literature were done. The elemental concentration in location 1 (non- fertile soil) are higher than location 2 ( fertile soil) because the plant absorbed fertilizer of soil and transfer most elements in soil to plant. (Author)

  13. Soil preparation and forage sowing time for crop-livestock integration in corn culture

    Directory of Open Access Journals (Sweden)

    Luiz Fernando de Andrade Fritsch

    2012-01-01

    Full Text Available This work was carried out during the 2008/2009 crop season, in an Oxisol. It was used a split-plot arrangement design, with each plot corresponding to a different soil preparation system and each split-plot corresponding to a different sowing time of the forage Brachiaria brizantha Stapf. The soil preparation systems were: heavy harrowing (HH, disk plough (DP, chisel plough (CP and no-till (NT, and the forage sowing times were: 0, 8, 16 and 25 days after sowing (DAS of corn, arranged in 16 treatments with 3 replicates. The productive and vegetative characteristics of the corn were evaluated. Soil preparations have influenced plant height and the first ear height, with the highest value found for the heavy harrow treatment. Forage sowing time had no influence on vegetative characteristics of the corn and productive characteristics were not influenced by the soil preparations. The forage sowing time had influence on corn productivity, causing decrease in competition with corn forage from 5 DAS. The productivity was highly correlated with the number of grains per ear.

  14. Distribution of pesticide residues in soil and uncertainty of sampling.

    Science.gov (United States)

    Suszter, Gabriela K; Ambrus, Árpád

    2017-08-03

    Pesticide residues were determined in about 120 soil cores taken randomly from the top 15 cm layer of two sunflower fields about 30 days after preemergence herbicide treatments. Samples were extracted with acetone-ethyl acetate mixture and the residues were determined with GC-TSD. Residues of dimethenamid, pendimethalin, and prometryn ranged from 0.005 to 2.97 mg/kg. Their relative standard deviations (CV) were between 0.66 and 1.13. The relative frequency distributions of residues in soil cores were very similar to those observed in root and tuber vegetables grown in pesticide treated soils. Based on all available information, a typical CV of 1.00 was estimated for pesticide residues in primary soil samples (soil cores). The corresponding expectable relative uncertainty of sampling is 20% when composite samples of size 25 are taken. To obtain a reliable estimate of the average residues in the top 15 cm layer of soil of a field up to 8 independent replicate random samples should be taken. To obtain better estimate of the actual residue level of the sampled filed would be marginal if larger number of samples were taken.

  15. Recent advances in applications of nanomaterials for sample preparation.

    Science.gov (United States)

    Xu, Linnan; Qi, Xiaoyue; Li, Xianjiang; Bai, Yu; Liu, Huwei

    2016-01-01

    Sample preparation is a key step for qualitative and quantitative analysis of trace analytes in complicated matrix. Along with the rapid development of nanotechnology in material science, numerous nanomaterials have been developed with particularly useful applications in analytical chemistry. Benefitting from their high specific areas, increased surface activities, and unprecedented physical/chemical properties, the potentials of nanomaterials for rapid and efficient sample preparation have been exploited extensively. In this review, recent progress of novel nanomaterials applied in sample preparation has been summarized and discussed. Both nanoparticles and nanoporous materials are evaluated for their unusual performance in sample preparation. Various compositions and functionalizations extended the applications of nanomaterials in sample preparations, and distinct size and shape selectivity was generated from the diversified pore structures of nanoporous materials. Such great variety make nanomaterials a kind of versatile tools in sample preparation for almost all categories of analytes. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. 105-DR Large sodium fire facility soil sampling data evaluation report

    International Nuclear Information System (INIS)

    Adler, J.G.

    1996-01-01

    This report evaluates the soil sampling activities, soil sample analysis, and soil sample data associated with the closure activities at the 105-DR Large Sodium Fire Facility. The evaluation compares these activities to the regulatory requirements for meeting clean closure. The report concludes that there is no soil contamination from the waste treatment activities

  17. Alpha liquid-scintillation spectrometry used for the measurement of uranium/thorium-disequilibria in soil samples

    International Nuclear Information System (INIS)

    Fueeg, B.; Tschachtli, T.; Kraehenbuehl, U.

    1997-01-01

    For the measurements of low-level radioactivity of natural samples. It is of interest to have a system with high counting efficiency. Alpha liquid-scintillation spectrometry is attractive, because it offers a 4 π geometry. Some chemical separation can be obtained using extractive scintillators. Due to quenching problems for natural samples, additional separation power is needed. A new sample preparation method was developed employing extraction chromatographic resin for measuring 238 U, 234 U, 232 Th, 230 Th, 228 Th and 226 Ra in soil samples, without using any uranium- or thorium-tracer for determining the chemical yields. This method was tested by analyzing the two different reference materials, IAEA-375, soil from Tschernobyl, as well as IAEA SDA-1, a deep-sea sediment with a high calcium content. For all analyzed radionuclides the recoveries were better than 90% with errors (confidence level of 95%) smaller than 5%. The minimal detectable concentration ranges between 0.2 and 0.8 Bq/kg, based on a one gram aliquot of sample and 80'000 seconds counting time. (orig.)

  18. Liquid scintillation: Sample preparation and counting atypical emissions

    International Nuclear Information System (INIS)

    Anon.

    1991-01-01

    Liquid scintillation sample preparation has the most published information but the least amount of definitive technical direction because the chemical and physical nature of the samples from biological investigations varies widely. This chapter discusses the following related topics: Aqueous Samples; Tissue Solubilizers; Absorption of 14 CO 2 ; Sample Combustion Methods; Heterogeneous Systems; Sample Preparation Problems (colored samples, chemiluminescence, photoluminescence, static electricity); Counting Various Types of Emitters; Counting Atypical Emissions. 2 refs., 2 figs

  19. Sampling design for use by the soil decontamination project

    International Nuclear Information System (INIS)

    Rutherford, D.W.; Stevens, J.R.

    1981-01-01

    This report proposes a general approach to the problem and discusses sampling of soil to map the contaminated area and to provide samples for characterizaton of soil components and contamination. Basic concepts in sample design are reviewed with reference to environmental transuranic studies. Common designs are reviewed and evaluated for use with specific objectives that might be required by the soil decontamination project. Examples of a hierarchial design pilot study and a combined hierarchial and grid study are proposed for the Rocky Flats 903 pad area

  20. Sampling for Soil Carbon Stock Assessment in Rocky Agricultural Soils

    Science.gov (United States)

    Beem-Miller, Jeffrey P.; Kong, Angela Y. Y.; Ogle, Stephen; Wolfe, David

    2016-01-01

    Coring methods commonly employed in soil organic C (SOC) stock assessment may not accurately capture soil rock fragment (RF) content or soil bulk density (rho (sub b)) in rocky agricultural soils, potentially biasing SOC stock estimates. Quantitative pits are considered less biased than coring methods but are invasive and often cost-prohibitive. We compared fixed-depth and mass-based estimates of SOC stocks (0.3-meters depth) for hammer, hydraulic push, and rotary coring methods relative to quantitative pits at four agricultural sites ranging in RF content from less than 0.01 to 0.24 cubic meters per cubic meter. Sampling costs were also compared. Coring methods significantly underestimated RF content at all rocky sites, but significant differences (p is less than 0.05) in SOC stocks between pits and corers were only found with the hammer method using the fixed-depth approach at the less than 0.01 cubic meters per cubic meter RF site (pit, 5.80 kilograms C per square meter; hammer, 4.74 kilograms C per square meter) and at the 0.14 cubic meters per cubic meter RF site (pit, 8.81 kilograms C per square meter; hammer, 6.71 kilograms C per square meter). The hammer corer also underestimated rho (sub b) at all sites as did the hydraulic push corer at the 0.21 cubic meters per cubic meter RF site. No significant differences in mass-based SOC stock estimates were observed between pits and corers. Our results indicate that (i) calculating SOC stocks on a mass basis can overcome biases in RF and rho (sub b) estimates introduced by sampling equipment and (ii) a quantitative pit is the optimal sampling method for establishing reference soil masses, followed by rotary and then hydraulic push corers.

  1. Genotyping of Toxoplasma Gondii Isolates from Soil Samples in Tehran, Iran

    Directory of Open Access Journals (Sweden)

    M Tavalla

    2013-06-01

    Full Text Available Background: The protozoan parasite Toxoplasma gondii can infect any warm blooded nucleated cells. One of the ways for human infection is ingestion of oocysts directly from soil or via infected fruits or vegetables. To survey the potential role of T. gondii oocyst in soil samples, the present study was conducted in Tehran City, Iran.Methods: A total of 150 soil samples were collected around rubbish dumps, children's play ground, parks and public places. Oocysts recovery was performed by sodium nitrate flotation method on soil samples. For molecular detection, PCR reaction targeting B1 gene was performed and then, the posi­tive results were confirmed using repetitive 529 bp DNA fragment in other PCR reaction. Finally, the positive samples were genotyped at the SAG2 locus.Results: Toxoplasma DNA was found in 13 soil samples. After genotyping and RFLP analysis in SAG2 locus, nine positive samples were revealed type III, one positive sample was type I whereas three samples revealed mixed infection (type, I & III.Conclusion: The predominant genotype in Tehran soil samples is type III.

  2. Analysis of large soil samples for actinides

    Science.gov (United States)

    Maxwell, III; Sherrod, L [Aiken, SC

    2009-03-24

    A method of analyzing relatively large soil samples for actinides by employing a separation process that includes cerium fluoride precipitation for removing the soil matrix and precipitates plutonium, americium, and curium with cerium and hydrofluoric acid followed by separating these actinides using chromatography cartridges.

  3. Recent advances in column switching sample preparation in bioanalysis.

    Science.gov (United States)

    Kataoka, Hiroyuki; Saito, Keita

    2012-04-01

    Column switching techniques, using two or more stationary phase columns, are useful for trace enrichment and online automated sample preparation. Target fractions from the first column are transferred online to a second column with different properties for further separation. Column switching techniques can be used to determine the analytes in a complex matrix by direct sample injection or by simple sample treatment. Online column switching sample preparation is usually performed in combination with HPLC or capillary electrophoresis. SPE or turbulent flow chromatography using a cartridge column and in-tube solid-phase microextraction using a capillary column have been developed for convenient column switching sample preparation. Furthermore, various micro-/nano-sample preparation devices using new polymer-coating materials have been developed to improve extraction efficiency. This review describes current developments and future trends in novel column switching sample preparation in bioanalysis, focusing on innovative column switching techniques using new extraction devices and materials.

  4. Laser-induced breakdown spectroscopy for space exploration applications: Influence of the ambient pressure on the calibration curves prepared from soil and clay samples

    International Nuclear Information System (INIS)

    Salle, Beatrice; Cremers, David A.; Maurice, Sylvestre; Wiens, Roger C.

    2005-01-01

    Recently, there has been an increasing interest in the laser-induced breakdown spectroscopy (LIBS) technique for stand-off detection of geological samples for use on landers and rovers to Mars, and for other space applications. For space missions, LIBS analysis capabilities must be investigated and instrumental development is required to take into account constraints such as size, weight, power and the effect of environmental atmosphere (pressure and ambient gas) on flight instrument performance. In this paper, we study the in-situ LIBS method at reduced pressure (7 Torr CO 2 to simulate the Martian atmosphere) and near vacuum (50 mTorr in air to begin to simulate the Moon or asteroids' pressure) as well as at atmospheric pressure in air (for Earth conditions and comparison). Here in-situ corresponds to distances on the order of 150 mm in contrast to stand-off analysis at distance of many meters. We show the influence of the ambient pressure on the calibration curves prepared from certified soil and clay pellets. In order to detect simultaneously all the elements commonly observed in terrestrial soils, we used an Echelle spectrograph. The results are discussed in terms of calibration curves, measurement precision, plasma light collection system efficiency and matrix effects

  5. Modular microfluidic system for biological sample preparation

    Science.gov (United States)

    Rose, Klint A.; Mariella, Jr., Raymond P.; Bailey, Christopher G.; Ness, Kevin Dean

    2015-09-29

    A reconfigurable modular microfluidic system for preparation of a biological sample including a series of reconfigurable modules for automated sample preparation adapted to selectively include a) a microfluidic acoustic focusing filter module, b) a dielectrophoresis bacteria filter module, c) a dielectrophoresis virus filter module, d) an isotachophoresis nucleic acid filter module, e) a lyses module, and f) an isotachophoresis-based nucleic acid filter.

  6. The Impact of Including Below Detection Limit Samples in Post Decommissioning Soil Sample Analyses

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jung Hwan; Yim, Man-Sung [KAIST, Daejeon (Korea, Republic of)

    2016-10-15

    To meet the required standards the site owner has to show that the soil at the facility has been sufficiently cleaned up. To do this one must know the contamination of the soil at the site prior to clean up. This involves sampling that soil to identify the degree of contamination. However there is a technical difficulty in determining how much decontamination should be done. The problem arises when measured samples are below the detection limit. Regulatory guidelines for site reuse after decommissioning are commonly challenged because the majority of the activity in the soil at or below the limit of detection. Using additional statistical analyses of contaminated soil after decommissioning is expected to have the following advantages: a better and more reliable probabilistic exposure assessment, better economics (lower project costs) and improved communication with the public. This research will develop an approach that defines an acceptable method for demonstrating compliance of decommissioned NPP sites and validates that compliance. Soil samples from NPP often contain censored data. Conventional methods for dealing with censored data sets are statistically biased and limited in their usefulness. In this research, additional methods are performed using real data from a monazite manufacturing factory.

  7. Indigenous development of automated metallographic sample preparation system

    International Nuclear Information System (INIS)

    Kulkarni, A.P.; Pandit, K.M.; Deshmukh, A.G.; Sahoo, K.C.

    2005-01-01

    Surface preparation of specimens for Metallographic studies on irradiated material involves a lot of remote handling of radioactive material by skilled manpower. These are laborious and man-rem intensive activities and put limitations on number of samples that can be prepared for the metallographic studies. To overcome these limitations, automated systems have been developed for surface preparation of specimens in PIE division. The system includes (i) Grinding and polishing stations (ii) Water jet cleaning station (iii) Ultrasonic cleaning stations (iv) Drying station (v) Sample loading and unloading station (vi) Dispenser for slurries and diluents and (vii) Automated head for movement of the sample holder disc from one station to other. System facilities the operator for programming/changing sequence of the sample preparations including remote changing of grinding/polishing discs from the stations. Two such systems have been installed and commissioned in Hot Cell for PIE Division. These are being used for preparation of irradiated samples from nuclear fuels and structural components. This development has increased the throughput of metallography work and savings in terms of (man-severts) radiation exposure to operators. This presentation will provide details of the challenges in undertaking this developmental work. (author)

  8. SEAMIST trademark soil sampling for tritiated water: First year's results

    International Nuclear Information System (INIS)

    Mallon, B.; Martins, S.A.; Houpis, J.L.; Lowry, W.; Cremer, C.D.

    1992-01-01

    SEAMIST trademark is a recently developed sampling system that enables one to measure various soil parameters by means of an inverted, removable, impermeable membrane tube inserted in a borehole. This membrane tube can have various measuring devices installed on it, such as gas ports, adsorbent pads, and electrical sensors. These membrane tubes are made of a laminated polymer. The Lawrence Livermore National Laboratory in Livermore, California, has installed two of these systems to monitor tritium in soil resulting from a leak in an underground storage tank. One tube is equipped with gas ports to sample soil vapor and the other with adsorbent pads to sample soil moisture. Borehole stability was maintained using either sand-filled or air-inflated tubes. Both system implementations yielded concentrations or activities that compared well with the measured concentrations of tritium in the soil taken during borehole construction. In addition, an analysis of the data suggest that both systems prevented the vertical migration of tritium in the boreholes. Also, a neutron probe was successfully used in a blank membrane inserted in one of the boreholes to monitor the moisture in the soil without exposing the probe to the tritium. The neutron log showed excellent agreement with the soil moisture content measured in soil samples taken during borehole construction. This paper describes the two SEAMIST trademark systems used and presents sampling results and comparisons

  9. New materials for sample preparation techniques in bioanalysis.

    Science.gov (United States)

    Nazario, Carlos Eduardo Domingues; Fumes, Bruno Henrique; da Silva, Meire Ribeiro; Lanças, Fernando Mauro

    2017-02-01

    The analysis of biological samples is a complex and difficult task owing to two basic and complementary issues: the high complexity of most biological matrices and the need to determine minute quantities of active substances and contaminants in such complex sample. To succeed in this endeavor samples are usually subject to three steps of a comprehensive analytical methodological approach: sample preparation, analytes isolation (usually utilizing a chromatographic technique) and qualitative/quantitative analysis (usually with the aid of mass spectrometric tools). Owing to the complex nature of bio-samples, and the very low concentration of the target analytes to be determined, selective sample preparation techniques is mandatory in order to overcome the difficulties imposed by these two constraints. During the last decade new chemical synthesis approaches has been developed and optimized, such as sol-gel and molecularly imprinting technologies, allowing the preparation of novel materials for sample preparation including graphene and derivatives, magnetic materials, ionic liquids, molecularly imprinted polymers, and much more. In this contribution we will review these novel techniques and materials, as well as their application to the bioanalysis niche. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Natural radioactivity in soil samples of Kocaeli basin, Turkey

    International Nuclear Information System (INIS)

    Karakelle, B.; Oeztuerk, N.; Erkol, A.Y.; Koese, A.; Varinlioglu, A.; Yilmaz, F.

    2002-01-01

    The city of Kocaeli is in the western part of Anatolia in Turkey and has a population of approximately 1.000.000. There is no information about radioactivity in the Kocaeli soils samples so far. For this reason, the concentrations of the natural radionuclides in soil samples from 27 different sampling stations in Kocaeli Basin and its surroundings have been determined. The results have been compared with other radioactivity measurements in different country's soils. The typical concentrations of 137 Cs, 238 U, 40 K, 226 Ra, 232 Th found in surface soil samples ranged from 2 ± 0.6 to 25 ± 6 Bq/kg, from 11 ± 4 to 49 ± 10 Bq/kg, from 161 ± 30 to 964 ± 127 Bq/kg, from 10 ± 4 to 58 ± 11 Bq/kg, and from 11 ± 3 to 65 ± 13 Bq/kg, respectively. (author)

  11. Stability of mercury concentration measurements in archived soil and peat samples

    Science.gov (United States)

    Navrátil, Tomáš; Burns, Douglas; Nováková, Tereza; Kaňa, Jiří; Rohovec, Jan; Roll, Michal; Ettler, Vojtěch

    2018-01-01

    Archived soil samples can provide important information on the history of environmental contamination and by comparison with recently collected samples, temporal trends can be inferred. Little previous work has addressed whether mercury (Hg) concentrations in soil samples are stable with long-term storage under standard laboratory conditions. In this study, we have re-analyzed using cold vapor atomic adsorption spectroscopy a set of archived soil samples that ranged from relatively pristine mountainous sites to a polluted site near a non-ferrous metal smelter with a wide range of Hg concentrations (6 - 6485 µg kg-1). Samples included organic and mineral soils and peats with a carbon content that ranged from 0.2 to 47.7%. Soil samples were stored in polyethylene bags or bottles and held in laboratory rooms where temperature was not kept to a constant value. Mercury concentrations in four subsets of samples were originally measured in 2000, 2005, 2006 and 2007, and re-analyzed in 2017, i.e. after 17, 12, 11 and 10 years of storage. Statistical analyses of either separated or lumped data yielded no significant differences between the original and current Hg concentrations. Based on these analyses, we show that archived soil and peat samples can be used to evaluate historical soil mercury contamination.

  12. Sample Preparation for Electron Probe Microanalysis-Pushing the Limits.

    Science.gov (United States)

    Geller, Joseph D; Engle, Paul D

    2002-01-01

    There are two fundamental considerations in preparing samples for electron probe microanalysis (EPMA). The first one may seem obvious, but we often find it is overlooked. That is, the sample analyzed should be representative of the population from which it comes. The second is a direct result of the assumptions in the calculations used to convert x-ray intensity ratios, between the sample and standard, to concentrations. Samples originate from a wide range of sources. During their journey to being excited under the electron beam for the production of x rays there are many possibilities for sample alteration. Handling can contaminate samples by adding extraneous matter. In preparation, the various abrasives used in sizing the sample by sawing, grinding and polishing can embed themselves. The most accurate composition of a contaminated sample is, at best, not representative of the original sample; it is misleading. Our laboratory performs EPMA analysis on customer submitted samples and prepares over 250 different calibration standards including pure elements, compounds, alloys, glasses and minerals. This large variety of samples does not lend itself to mass production techniques, including automatic polishing. Our manual preparation techniques are designed individually for each sample. The use of automated preparation equipment does not lend itself to this environment, and is not included in this manuscript. The final step in quantitative electron probe microanalysis is the conversion of x-ray intensities ratios, known as the "k-ratios," to composition (in mass fraction or atomic percent) and/or film thickness. Of the many assumptions made in the ZAF (where these letters stand for atomic number, absorption and fluorescence) corrections the localized geometry between the sample and electron beam, or takeoff angle, must be accurately known. Small angular errors can lead to significant errors in the final results. The sample preparation technique then becomes very

  13. Instrumental neutron activation analysis of soil sample

    International Nuclear Information System (INIS)

    Abdul Khalik Haji Wood.

    1983-01-01

    This paper describes the analysis of soil samples collected from 5 different location around Sungai Lui, Kajang, Selangor, Malaysia. These sample were taken at 22-24 cm from the top of the ground and were analysed using the techniques of Instrumental Neutron Activation Analysis (INAA). The analysis on soil sample taken above 22-24 cm level were done in order to determine if there is any variation in elemental contents at different sampling levels. The results indicate a wide variation in the contents of the samples. About 30 elements have been analysed. The major ones are Na, I, Cl, Mg, Al, K, Ti, Ca and Fe. Trace elements analysed were Ba, Sc, V, Cr, Mn, Ga, As, Zn, Br, Rb, Co, Hf, Zr, Th, U, Sb, Cs, Ce, Sm, Eu, Tb, Dy, Yb, Lu and La. (author)

  14. Optimizing Soil Moisture Sampling Locations for Validation Networks for SMAP

    Science.gov (United States)

    Roshani, E.; Berg, A. A.; Lindsay, J.

    2013-12-01

    Soil Moisture Active Passive satellite (SMAP) is scheduled for launch on Oct 2014. Global efforts are underway for establishment of soil moisture monitoring networks for both the pre- and post-launch validation and calibration of the SMAP products. In 2012 the SMAP Validation Experiment, SMAPVEX12, took place near Carman Manitoba, Canada where nearly 60 fields were sampled continuously over a 6 week period for soil moisture and several other parameters simultaneous to remotely sensed images of the sampling region. The locations of these sampling sites were mainly selected on the basis of accessibility, soil texture, and vegetation cover. Although these criteria are necessary to consider during sampling site selection, they do not guarantee optimal site placement to provide the most efficient representation of the studied area. In this analysis a method for optimization of sampling locations is presented which combines the state-of-art multi-objective optimization engine (non-dominated sorting genetic algorithm, NSGA-II), with the kriging interpolation technique to minimize the number of sampling sites while simultaneously minimizing the differences between the soil moisture map resulted from the kriging interpolation and soil moisture map from radar imaging. The algorithm is implemented in Whitebox Geospatial Analysis Tools, which is a multi-platform open-source GIS. The optimization framework is subject to the following three constraints:. A) sampling sites should be accessible to the crew on the ground, B) the number of sites located in a specific soil texture should be greater than or equal to a minimum value, and finally C) the number of sampling sites with a specific vegetation cover should be greater than or equal to a minimum constraint. The first constraint is implemented into the proposed model to keep the practicality of the approach. The second and third constraints are considered to guarantee that the collected samples from each soil texture categories

  15. Preparation of honey sample for tritium monitoring

    International Nuclear Information System (INIS)

    Chen Bingru; Wang Chenlian; Wang Weihua

    1989-01-01

    The method of preparation of honey sample for tritium monitoring was described. The equipments consist of an air and honey supply system, a quartz combustor with CM-type monolithic combustion catalyst and a condensation system. In the equipments, honey sample was converted into cooling water by the distilling, cracking and carbonizing procedures for tritium counting. The recovery ratio is 99.0 ± 4.5 percent for tritiated water and 96.0 ± 2.0 for tritiated organic compounds. It is a feasible preparing method for the total tritium monitoring in honey sample

  16. Preparation of Sandy Soil Stabilizer for Roads Based on Radiation Modified Polymer Composite

    International Nuclear Information System (INIS)

    Elnahas, H.H.

    2016-01-01

    Radiation modified polymer composite (RMPC) was studied to build an extremely durable sandy road, construct a trail or bath, or control dust and erosion. A dilute solution of composite binds sandy soil fines through a coagulation bonding process. The result is a dense soil structure that has superior resistance to cracks and water penetration and can also solve erosion control problems. In erosion control applications, diluted composite is merely sprayed into sandy soil without compaction, effectively sealing the surface to prevent air-born dust or deterioration from erosion. The prepared composite has an elastic and melt-able film formation that imparts thermal compacting to the stabilized sandy soil after full dryness for sandy road leveling, repairing and restoration processes. The prepared composite is environmentally economical when compared with traditional sandy soil stabilizing (SSS) or sealing methods.

  17. Soil Sampling Plan for the transuranic storage area soil overburden and final report: Soil overburden sampling at the RWMC transuranic storage area

    International Nuclear Information System (INIS)

    Stanisich, S.N.

    1994-12-01

    This Soil Sampling Plan (SSP) has been developed to provide detailed procedural guidance for field sampling and chemical and radionuclide analysis of selected areas of soil covering waste stored at the Transuranic Storage Area (TSA) at the Idaho National Engineering Laboratory's (INEL) Radioactive Waste Management Complex (RWMC). The format and content of this SSP represents a complimentary hybrid of INEL Waste Management--Environmental Restoration Program, and Comprehensive Environmental Response, Compensation and Liability Act (CERCLA) Remedial Investigation/Feasibility Study (RI/FS) sampling guidance documentation. This sampling plan also functions as a Quality Assurance Project Plan (QAPP). The QAPP as a controlling mechanism during sampling to ensure that all data collected are valid, reliabile, and defensible. This document outlines organization, objectives and quality assurance/quality control (QA/QC) activities to achieve the desired data quality goals. The QA/QC requirements for this project are outlined in the Data Collection Quality Assurance Plan (DCQAP) for the Buried Waste Program. The DCQAP is a program plan and does not outline the site specific requirements for the scope of work covered by this SSP

  18. How to Perform Precise Soil and Sediment Sampling? One solution: The Fine Increment Soil Collector (FISC)

    Energy Technology Data Exchange (ETDEWEB)

    Mabit, L.; Toloza, A. [Soil and Water Management and Crop Nutrition Laboratory, IAEA, Seibersdorf (Austria); Meusburger, K.; Alewell, C. [Environmental Geosciences, Department of Environmental Sciences, University of Basel, Basel (Switzerland); Iurian, A-R. [Babes-Bolyai University, Faculty of Environmental Science and Engineering, Cluj-Napoca (Romania); Owens, P. N. [Environmental Science Program and Quesnel River Research Centre, University of Northern British Columbia, Prince George, British Columbia (Canada)

    2014-07-15

    Soil and sediment related research for terrestrial agrienvironmental assessments requires accurate depth incremental sampling to perform detailed analysis of physical, geochemical and biological properties of soil and exposed sediment profiles. Existing equipment does not allow collecting soil/sediment increments at millimetre resolution. The Fine Increment Soil Collector (FISC), developed by the SWMCN Laboratory, allows much greater precision in incremental soil/sediment sampling. It facilitates the easy recovery of collected material by using a simple screw-thread extraction system (see Figure 1). The FISC has been designed specifically to enable standardized scientific investigation of shallow soil/sediment samples. In particular, applications have been developed in two IAEA Coordinated Research Projects (CRPs): CRP D1.20.11 on “Integrated Isotopic Approaches for an Area-wide Precision Conservation to Control the Impacts of Agricultural Practices on Land Degradation and Soil Erosion” and CRP D1.50.15 on “Response to Nuclear Emergencies Affecting Food and Agriculture.”.

  19. How to Perform Precise Soil and Sediment Sampling? One solution: The Fine Increment Soil Collector (FISC)

    International Nuclear Information System (INIS)

    Mabit, L.; Toloza, A.; Meusburger, K.; Alewell, C.; Iurian, A-R.; Owens, P.N.

    2014-01-01

    Soil and sediment related research for terrestrial agrienvironmental assessments requires accurate depth incremental sampling to perform detailed analysis of physical, geochemical and biological properties of soil and exposed sediment profiles. Existing equipment does not allow collecting soil/sediment increments at millimetre resolution. The Fine Increment Soil Collector (FISC), developed by the SWMCN Laboratory, allows much greater precision in incremental soil/sediment sampling. It facilitates the easy recovery of collected material by using a simple screw-thread extraction system (see Figure 1). The FISC has been designed specifically to enable standardized scientific investigation of shallow soil/sediment samples. In particular, applications have been developed in two IAEA Coordinated Research Projects (CRPs): CRP D1.20.11 on “Integrated Isotopic Approaches for an Area-wide Precision Conservation to Control the Impacts of Agricultural Practices on Land Degradation and Soil Erosion” and CRP D1.50.15 on “Response to Nuclear Emergencies Affecting Food and Agriculture.”

  20. Platelet-rich fibrin prepared from stored whole-blood samples.

    Science.gov (United States)

    Isobe, Kazushige; Suzuki, Masashi; Watanabe, Taisuke; Kitamura, Yutaka; Suzuki, Taiji; Kawabata, Hideo; Nakamura, Masayuki; Okudera, Toshimitsu; Okudera, Hajime; Uematsu, Kohya; Nakata, Koh; Tanaka, Takaaki; Kawase, Tomoyuki

    2017-12-01

    In regenerative therapy, self-clotted platelet concentrates, such as platelet-rich fibrin (PRF), are generally prepared on-site and are immediately used for treatment. If blood samples or prepared clots can be preserved for several days, their clinical applicability will expand. Here, we prepared PRF from stored whole-blood samples and examined their characteristics. Blood samples were collected from non-smoking, healthy male donors (aged 27-67 years, N = 6), and PRF clots were prepared immediately or after storage for 1-2 days. Fibrin fiber was examined by scanning electron microscopy. Bioactivity was evaluated by means of a bioassay system involving human periosteal cells, whereas PDGF-BB concentrations were determined by an enzyme-linked immunosorbent assay. Addition of optimal amounts of a 10% CaCl 2 solution restored the coagulative ability of whole-blood samples that contained an anticoagulant (acid citrate dextrose) and were stored for up to 2 days at ambient temperature. In PRF clots prepared from the stored whole-blood samples, the thickness and cross-links of fibrin fibers were almost identical to those of freshly prepared PRF clots. PDGF-BB concentrations in the PRF extract were significantly lower in stored whole-blood samples than in fresh samples; however, both extracts had similar stimulatory effects on periosteal-cell proliferation. Quality of PRF clots prepared from stored whole-blood samples is not reduced significantly and can be ensured for use in regenerative therapy. Therefore, the proposed method enables a more flexible treatment schedule and choice of a more suitable platelet concentrate immediately before treatment, not after blood collection.

  1. The effect of sample preparation on uranium hydriding

    International Nuclear Information System (INIS)

    Banos, A.; Stitt, C.A.; Scott, T.B.

    2016-01-01

    Highlights: • Distinct differences in uranium hydride growth rates and characteristics between different surface preparation methods. • The primary difference between the categories of sample preparations is the level of strain present in the surface. • Greater surface-strain, leads to higher nucleation number density, implying a preferred attack of strained vs unstrained metal. • As strain is reduced, surface features such as carbides and grain boundaries become more important in controlling the UH3 location. - Abstract: The influence of sample cleaning preparation on the early stages of uranium hydriding has been examined, by using four identical samples but concurrently prepared using four different methods. The samples were reacted together in the same corrosion cell to ensure identical exposure conditions. From the analysis, it was found that the hydride nucleation rate was proportional to the level of strain exhibiting higher number density for the more strained surfaces. Additionally, microstructure of the metal plays a secondary role regarding initial hydrogen attack on the highly strained surfaces yet starts to dominate the system while moving to more pristine samples.

  2. Saturation and porosity measurements of different soil samples by gamma ray transmission

    International Nuclear Information System (INIS)

    Akbal, S.; Filiz Baytas, A.

    2000-01-01

    Gamma-ray transmission methods have been used accurately for the study of the properties of soil samples. In this study, the soil samples were collected from various regions of Turkey and a Nal (TI) detector measured the attenuation of strongly collimated monoenergetic gamma beam (from Cs-137) through soil samples. The water saturation and porosity were therefore calculated from the transmission measurements for each soil sample. (authors)

  3. Efficient sample preparation from complex biological samples using a sliding lid for immobilized droplet extractions.

    Science.gov (United States)

    Casavant, Benjamin P; Guckenberger, David J; Beebe, David J; Berry, Scott M

    2014-07-01

    Sample preparation is a major bottleneck in many biological processes. Paramagnetic particles (PMPs) are a ubiquitous method for isolating analytes of interest from biological samples and are used for their ability to thoroughly sample a solution and be easily collected with a magnet. There are three main methods by which PMPs are used for sample preparation: (1) removal of fluid from the analyte-bound PMPs, (2) removal of analyte-bound PMPs from the solution, and (3) removal of the substrate (with immobilized analyte-bound PMPs). In this paper, we explore the third and least studied method for PMP-based sample preparation using a platform termed Sliding Lid for Immobilized Droplet Extractions (SLIDE). SLIDE leverages principles of surface tension and patterned hydrophobicity to create a simple-to-operate platform for sample isolation (cells, DNA, RNA, protein) and preparation (cell staining) without the need for time-intensive wash steps, use of immiscible fluids, or precise pinning geometries. Compared to other standard isolation protocols using PMPs, SLIDE is able to perform rapid sample preparation with low (0.6%) carryover of contaminants from the original sample. The natural recirculation occurring within the pinned droplets of SLIDE make possible the performance of multistep cell staining protocols within the SLIDE by simply resting the lid over the various sample droplets. SLIDE demonstrates a simple easy to use platform for sample preparation on a range of complex biological samples.

  4. Sample size choices for XRCT scanning of highly unsaturated soil mixtures

    Directory of Open Access Journals (Sweden)

    Smith Jonathan C.

    2016-01-01

    Full Text Available Highly unsaturated soil mixtures (clay, sand and gravel are used as building materials in many parts of the world, and there is increasing interest in understanding their mechanical and hydraulic behaviour. In the laboratory, x-ray computed tomography (XRCT is becoming more widely used to investigate the microstructures of soils, however a crucial issue for such investigations is the choice of sample size, especially concerning the scanning of soil mixtures where there will be a range of particle and void sizes. In this paper we present a discussion (centred around a new set of XRCT scans on sample sizing for scanning of samples comprising soil mixtures, where a balance has to be made between realistic representation of the soil components and the desire for high resolution scanning, We also comment on the appropriateness of differing sample sizes in comparison to sample sizes used for other geotechnical testing. Void size distributions for the samples are presented and from these some hypotheses are made as to the roles of inter- and intra-aggregate voids in the mechanical behaviour of highly unsaturated soils.

  5. PCR detection of Burkholderia multivorans in water and soil samples.

    Science.gov (United States)

    Peeters, Charlotte; Daenekindt, Stijn; Vandamme, Peter

    2016-08-12

    Although semi-selective growth media have been developed for the isolation of Burkholderia cepacia complex bacteria from the environment, thus far Burkholderia multivorans has rarely been isolated from such samples. Because environmental B. multivorans isolates mainly originate from water samples, we hypothesized that water rather than soil is its most likely environmental niche. The aim of the present study was to assess the occurrence of B. multivorans in water samples from Flanders (Belgium) using a fast, culture-independent PCR assay. A nested PCR approach was used to achieve high sensitivity, and specificity was confirmed by sequencing the resulting amplicons. B. multivorans was detected in 11 % of the water samples (n = 112) and 92 % of the soil samples (n = 25) tested. The percentage of false positives was higher for water samples compared to soil samples, showing that the presently available B. multivorans recA primers lack specificity when applied to the analysis of water samples. The results of the present study demonstrate that B. multivorans DNA is commonly present in soil samples and to a lesser extent in water samples in Flanders (Belgium).

  6. On the development of automatic sample preparation devices

    International Nuclear Information System (INIS)

    Oesselmann, J.

    1987-01-01

    Modern mass spectrometers for stable isotope analysis offer accurate isotope ratio results from gaseous samples (CO 2 , N 2 , H 2 , SO 2 ) in a completely automated fashion. However, most samples of interest either are associated with contaminant gases or the gas has to be liberated by a chemical procedure prior to measurement. In most laboratories this sample preparation step is performed manually. As a consequence, sample throughput is rather low and - despite skilful operation - the preparation procedure varies slightly from one sample to the next affecting mainly the reproducibility of the data. (author)

  7. Sample Preparation for Electron Probe Microanalysis—Pushing the Limits

    Science.gov (United States)

    Geller, Joseph D.; Engle, Paul D.

    2002-01-01

    There are two fundamental considerations in preparing samples for electron probe microanalysis (EPMA). The first one may seem obvious, but we often find it is overlooked. That is, the sample analyzed should be representative of the population from which it comes. The second is a direct result of the assumptions in the calculations used to convert x-ray intensity ratios, between the sample and standard, to concentrations. Samples originate from a wide range of sources. During their journey to being excited under the electron beam for the production of x rays there are many possibilities for sample alteration. Handling can contaminate samples by adding extraneous matter. In preparation, the various abrasives used in sizing the sample by sawing, grinding and polishing can embed themselves. The most accurate composition of a contaminated sample is, at best, not representative of the original sample; it is misleading. Our laboratory performs EPMA analysis on customer submitted samples and prepares over 250 different calibration standards including pure elements, compounds, alloys, glasses and minerals. This large variety of samples does not lend itself to mass production techniques, including automatic polishing. Our manual preparation techniques are designed individually for each sample. The use of automated preparation equipment does not lend itself to this environment, and is not included in this manuscript. The final step in quantitative electron probe microanalysis is the conversion of x-ray intensities ratios, known as the “k-ratios,” to composition (in mass fraction or atomic percent) and/or film thickness. Of the many assumptions made in the ZAF (where these letters stand for atomic number, absorption and fluorescence) corrections the localized geometry between the sample and electron beam, or takeoff angle, must be accurately known. Small angular errors can lead to significant errors in the final results. The sample preparation technique then becomes very

  8. Soil sampling and analysis plan for the 3718-F Alkali Metal Treatment and Storage Facility closure activities

    Energy Technology Data Exchange (ETDEWEB)

    Sonnichsen, J.C.

    1997-05-01

    Amendment V.13.B.b to the approved closure plan (DOE-RL 1995a) requires that a soil sampling and analysis plan be prepared and submitted to the Washington State Department of Ecology (Ecology) for review and approval. Amendment V.13.B.c requires that a diagram of the 3718-F Alkali Metal Treatment and Storage Facility unit (the treatment, storage, and disposal [TSD] unit) boundary that is to be closed, including the maximum extent of operation, be prepared and submitted as part is of the soil sampling and analysis plan. This document describes the sampling and analysis that is to be performed in response to these requirements and amends the closure plan. Specifically, this document supersedes Section 6.2, lines 43--46, and Section 7.3.6 of the closure plan. Results from the analysis will be compared to cleanup levels identified in the closure plan. These cleanup levels will be established using residential exposure assumptions in accordance with the Model Toxics Control Act (MTCA) Cleanup Regulation (Washington Administrative Code [WAC] 173-340) as required in Amendment V.13.B.I. Results of all sampling, including the raw analytical data, a summary of analytical results, a data validation package, and a narrative summary with conclusions will be provided to Ecology as specified in Amendment V.13.B.e. The results and process used to collect and analyze the soil samples will be certified by a licensed professional engineer. These results and a certificate of closure for the balance of the TSD unit, as outlined in Chapter 7.0 of the approved closure plan (storage shed, concrete pad, burn building, scrubber, and reaction tanks), will provide the basis for a closure determination.

  9. Soil sampling and analysis plan for the 3718-F Alkali Metal Treatment and Storage Facility closure activities

    International Nuclear Information System (INIS)

    Sonnichsen, J.C.

    1997-01-01

    Amendment V.13.B.b to the approved closure plan (DOE-RL 1995a) requires that a soil sampling and analysis plan be prepared and submitted to the Washington State Department of Ecology (Ecology) for review and approval. Amendment V.13.B.c requires that a diagram of the 3718-F Alkali Metal Treatment and Storage Facility unit (the treatment, storage, and disposal [TSD] unit) boundary that is to be closed, including the maximum extent of operation, be prepared and submitted as part is of the soil sampling and analysis plan. This document describes the sampling and analysis that is to be performed in response to these requirements and amends the closure plan. Specifically, this document supersedes Section 6.2, lines 43--46, and Section 7.3.6 of the closure plan. Results from the analysis will be compared to cleanup levels identified in the closure plan. These cleanup levels will be established using residential exposure assumptions in accordance with the Model Toxics Control Act (MTCA) Cleanup Regulation (Washington Administrative Code [WAC] 173-340) as required in Amendment V.13.B.I. Results of all sampling, including the raw analytical data, a summary of analytical results, a data validation package, and a narrative summary with conclusions will be provided to Ecology as specified in Amendment V.13.B.e. The results and process used to collect and analyze the soil samples will be certified by a licensed professional engineer. These results and a certificate of closure for the balance of the TSD unit, as outlined in Chapter 7.0 of the approved closure plan (storage shed, concrete pad, burn building, scrubber, and reaction tanks), will provide the basis for a closure determination

  10. 40 CFR 205.160-2 - Test sample selection and preparation.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 24 2010-07-01 2010-07-01 false Test sample selection and preparation... sample selection and preparation. (a) Vehicles comprising the sample which are required to be tested... maintained in any manner unless such preparation, tests, modifications, adjustments or maintenance are part...

  11. FISHprep: A Novel Integrated Device for Metaphase FISH Sample Preparation

    DEFF Research Database (Denmark)

    Shah, Pranjul Jaykumar; Vedarethinam, Indumathi; Kwasny, Dorota

    2011-01-01

    We present a novel integrated device for preparing metaphase chromosomes spread slides (FISHprep). The quality of cytogenetic analysis from patient samples greatly relies on the efficiency of sample pre-treatment and/or slide preparation. In cytogenetic slide preparation, cell cultures...... are routinely used to process samples (for culture, arrest and fixation of cells) and/or to expand limited amount of samples (in case of prenatal diagnostics). Arguably, this expansion and other sample pretreatments form the longest part of the entire diagnostic protocols spanning over 3–4 days. We present here...... with minimal handling for metaphase FISH slide preparation....

  12. Independent assessment of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) sample preparation quality: Effect of sample preparation on MALDI-MS of synthetic polymers.

    Science.gov (United States)

    Kooijman, Pieter C; Kok, Sander; Honing, Maarten

    2017-02-28

    Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) provides detailed and in-depth information about the molecular characteristics of synthetic polymers. To obtain the most accurate results the sample preparation parameters should be chosen to suit the sample and the aim of the experiment. Because the underlying principles of MALDI are still not fully known, a priori determination of optimal sample preparation protocols is often not possible. Employing an automated sample preparation quality assessment method recently presented by us we quantified the sample preparation quality obtained using various sample preparation protocols. Six conventional matrices with and without added potassium as a cationization agent and six ionic liquid matrices (ILMs) were assessed using poly(ethylene glycol) (PEG), polytetrahydrofuran (PTHF) and poly(methyl methacrylate) (PMMA) as samples. All sample preparation protocols were scored and ranked based on predefined quality parameters and spot-to-spot repeatability. Clearly distinctive preferences were observed in matrix identity and cationization agent for PEG, PTHF and PMMA, as the addition of an excess of potassium cationization agent results in an increased score for PMMA and a contrasting matrix-dependent effect for PTHF and PEG. The addition of excess cationization agent to sample mixtures dissipates any overrepresentation of high molecular weight polymer species. Our results show reduced ionization efficiency and similar sample deposit homogeneity for all tested ILMs, compared with well-performing conventional MALDI matrices. The results published here represent a start in the unsupervised quantification of sample preparation quality for MALDI samples. This method can select the best sample preparation parameters for any synthetic polymer sample and the results can be used to formulate hypotheses on MALDI principles. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

  13. Sampling Design of Soil Physical Properties in a Conilon Coffee Field

    Directory of Open Access Journals (Sweden)

    Eduardo Oliveira de Jesus Santos

    Full Text Available ABSTRACT Establishing the number of samples required to determine values of soil physical properties ultimately results in optimization of labor and allows better representation of such attributes. The objective of this study was to analyze the spatial variability of soil physical properties in a Conilon coffee field and propose a soil sampling method better attuned to conditions of the management system. The experiment was performed in a Conilon coffee field in Espírito Santo state, Brazil, under a 3.0 × 2.0 × 1.0 m (4,000 plants ha-1 double spacing design. An irregular grid, with dimensions of 107 × 95.7 m and 65 sampling points, was set up. Soil samples were collected from the 0.00-0.20 m depth from each sampling point. Data were analyzed under descriptive statistical and geostatistical methods. Using statistical parameters, the adequate number of samples for analyzing the attributes under study was established, which ranged from 1 to 11 sampling points. With the exception of particle density, all soil physical properties showed a spatial dependence structure best fitted to the spherical model. Establishment of the number of samples and spatial variability for the physical properties of soils may be useful in developing sampling strategies that minimize costs for farmers within a tolerable and predictable level of error.

  14. Degradation of aldrin im samples of 'cerrado' Brazilian soils

    International Nuclear Information System (INIS)

    Musumeci, M.R.; Ruegg, E.F.

    1981-01-01

    14 C-aldrin degradation was studied in the laboratory, in samples of 'cerrado' Brazilian soils, during a period of 240 days. Recovery of radiocarbon decreased with time, although radiocarbon was not incorporated to the soil organic matter as show by soil combustion. In both soils 14 C-aldrin degraded to dieldrin and another compound that showed caracteristics of a hydrosoluble derivative of aldrin 14 C-aldrin was more persistent in sandy soil but amendment of this soil with nutrients or fertilizers did not enhanced aldrin degradation in this soil. (Author) [pt

  15. Contribution of soil fauna to soil functioning in degraded environments: a multidisciplinary approach

    Science.gov (United States)

    Gargiulo, Laura; Mele, Giacomo; Moradi, Jabbar; Kukla, Jaroslav; Jandová, Kateřina; Frouz, Jan

    2016-04-01

    The restoration of the soil functions is essential for the recovery of highly degraded sites and, consequently, the study of the soil fauna role in the soil development in such environments has great potential from a practical point of view. The soils of the post-mining sites represent unique models for the study of the natural ecological succession because mining creates similar environments characterized by the same substrate, but by different ages according to the year of closure of mines. The aim of this work was to assess the contribution of different species of macrofauna on the evolution of soil structure and on the composition and activity of the microbial community in soil samples subjected to ecological restoration or characterized by spontaneous ecological succession. For this purpose, an experimental test was carried out in two sites characterized by different post-mining conditions: 1) natural succession, 2) reclamation with planting trees. These sites are located in the post-mining area of Sokolov (Czech Republic). For the experimental test repacked soil cores were prepared in laboratory with sieved soil sampled from the two sites. The soil cores were prepared maintaining the sequence of soil horizons present in the field. These samples were inoculated separately with two genera of earthworms (Lumbricus and Aporrectodea) and two of centipedes (Julida and Polydesmus). In particular, based on their body size, were inoculated for each cylinder 2 individuals of millipedes, 1 individual of Lumbricus and 4 individuals of Aporrectodea. For each treatment and for control samples 5 replicates were prepared and all samples were incubated in field for 1 month in the two original sampling sites. After the incubation the samples were removed from the field and transported in laboratory in order to perform the analysis of microbial respiration, of PLFA (phospholipid-derived fatty acids) and ergosterol contents and finally for the characterization of soil structure

  16. Using Environmental Variables for Studying of the Quality of Sampling in Soil Mapping

    OpenAIRE

    A. Jafari; Norair Toomanian; R. Taghizadeh Mehrjerdi

    2016-01-01

    Introduction: Methods of soil survey are generally empirical and based on the mental development of the surveyor, correlating soil with underlying geology, landforms, vegetation and air-photo interpretation. Since there are no statistical criteria for traditional soil sampling; this may lead to bias in the areas being sampled. In digital soil mapping, soil samples may be used to elaborate quantitative relationships or models between soil attributes and soil covariates. Because the relationshi...

  17. Congener Production in Blood Samples During Preparation and Storage

    DEFF Research Database (Denmark)

    Felby, Søren; Nielsen, Erik

    1995-01-01

    Retsmedicin, congener production, preparation, head space GC, acetone, isobutanol, storage, blood samples, n-propanol, methanol, methylethylketone......Retsmedicin, congener production, preparation, head space GC, acetone, isobutanol, storage, blood samples, n-propanol, methanol, methylethylketone...

  18. Measurement of technetium-99 in soil samples collected in Marshall Islands

    Energy Technology Data Exchange (ETDEWEB)

    Tagami, K.; Uchida, S. [National Inst. of Radiological Sciences, Environmental and Toxicological Sciences Research Group, Chiba (Japan)

    2000-07-01

    Extraction techniques for recovery of technetium-99 ({sup 99}Tc) for ICP-MS measurements were evaluated using soil samples collected from the Marshall Islands. The results of three different extraction techniques were compared: (M1) acid leaching of Tc from ashed soil; (M2) acid leaching of Tc from raw dry soil; and (M3) Tc volatilization from ashed soil using a combustion apparatus. Total Tc recoveries varied considerably between the extraction techniques but each method yielded similar analytical results for {sup 99}Tc. Applications of these extraction techniques to a series of environmental samples and ICP-MS measurements have yielded first data on the {sup 99}Tc content of Marshall Islands soil samples contaminated with close-in radioactive fallout from nuclear weapons testing. The {sup 99}Tc activity concentration in the soil samples ranged between 0.1 and 1.1 mBq/g-dw. The limit of detection for {sup 99}Tc by ICP-MS was 0.17 mBq per sample or 0.014 mBq/g-dw under standard operating conditions. (author)

  19. Measurement of technetium-99 in soil samples collected in Marshall Islands

    International Nuclear Information System (INIS)

    Tagami, K.; Uchida, S.

    2000-01-01

    Extraction techniques for recovery of technetium-99 ( 99 Tc) for ICP-MS measurements were evaluated using soil samples collected from the Marshall Islands. The results of three different extraction techniques were compared: (M1) acid leaching of Tc from ashed soil; (M2) acid leaching of Tc from raw dry soil; and (M3) Tc volatilization from ashed soil using a combustion apparatus. Total Tc recoveries varied considerably between the extraction techniques but each method yielded similar analytical results for 99 Tc. Applications of these extraction techniques to a series of environmental samples and ICP-MS measurements have yielded first data on the 99 Tc content of Marshall Islands soil samples contaminated with close-in radioactive fallout from nuclear weapons testing. The 99 Tc activity concentration in the soil samples ranged between 0.1 and 1.1 mBq/g-dw. The limit of detection for 99 Tc by ICP-MS was 0.17 mBq per sample or 0.014 mBq/g-dw under standard operating conditions. (author)

  20. Uranium determination in soil samples using Eichrom resins

    International Nuclear Information System (INIS)

    Marabini, S.; Serdeiro, Nelidad H.

    2003-01-01

    Traditionally, the radiochemical methods for uranium activity determination in soil samples by alpha spectrometry, use some techniques like solvent extraction, precipitation and ion exchange in the separation and purification stages. In the last years, some new materials have been developed for using in extraction chromatography, specific for actinides determinations. In the present method the long and tedious stages were eliminated, and the reagents consumption and concentration were minimised. This new procedure was applied to soils since it is one of the most complex matrices. In order to reduce time and chemical reagents, the soil samples up to 0,5 g were leached with nitric, hydrofluoric and perchloric acids in hermetic sealed recipients of Teflon at 150 C degrees during 5 hours. UTEVA Eichrom resin was used for uranium separation and purification. The uranium activity concentration was determined by alpha spectrometry. Several standard samples were analysed and the results are presented. (author)

  1. Trends in sample preparation 2002. Development and application. Book of abstracts

    International Nuclear Information System (INIS)

    Wenzl, T.; Eberl, M.; Zischka, M.; Knapp, G.

    2002-01-01

    This conference comprised topics dealing with sample preparation such as: sample decomposition, solvent extraction, derivatization techniques and uncertainty in sample preparation. In particular microwave assisted sample preparation techniques and equipment were discussed. The papers were organized under the general topics: trace element analysis, trace analysis of organic compounds, high performance instrumentation in sample preparation, speciation analysis and posters session. Those papers of INIS interest are cited individually. (nevyjel)

  2. Trends in sample preparation 2002. Development and application. Book of abstracts

    Energy Technology Data Exchange (ETDEWEB)

    Wenzl, T; Eberl, M; Zischka, M; Knapp, G [eds.

    2002-07-01

    This conference comprised topics dealing with sample preparation such as: sample decomposition, solvent extraction, derivatization techniques and uncertainty in sample preparation. In particular microwave assisted sample preparation techniques and equipment were discussed. The papers were organized under the general topics: trace element analysis, trace analysis of organic compounds, high performance instrumentation in sample preparation, speciation analysis and posters session. Those papers of INIS interest are cited individually. (nevyjel)

  3. High-throughput diagnosis of potato cyst nematodes in soil samples.

    Science.gov (United States)

    Reid, Alex; Evans, Fiona; Mulholland, Vincent; Cole, Yvonne; Pickup, Jon

    2015-01-01

    Potato cyst nematode (PCN) is a damaging soilborne pest of potatoes which can cause major crop losses. In 2010, a new European Union directive (2007/33/EC) on the control of PCN came into force. Under the new directive, seed potatoes can only be planted on land which has been found to be free from PCN infestation following an official soil test. A major consequence of the new directive was the introduction of a new harmonized soil sampling rate resulting in a threefold increase in the number of samples requiring testing. To manage this increase with the same staffing resources, we have replaced the traditional diagnostic methods. A system has been developed for the processing of soil samples, extraction of DNA from float material, and detection of PCN by high-throughput real-time PCR. Approximately 17,000 samples are analyzed each year using this method. This chapter describes the high-throughput processes for the production of float material from soil samples, DNA extraction from the entire float, and subsequent detection and identification of PCN within these samples.

  4. Preparation of in-house calibration source for the use in radioactivity analysis of the environmental samples. Consideration of homogeneity

    International Nuclear Information System (INIS)

    Aba, A.; Ismaeel, A.

    2013-01-01

    An in-house reference material has been prepared in Kuwait Institute for Scientific Research radioecology laboratory, for quality control purposes of gamma spectrometer systems. The material contains a known amount of uranium ore reference material (prepared by the International Atomic Energy Agency and coded as IAEA-RGU-1) which is mixed with marine sediment collected from Kuwait bay. The IAEA-RGU-1 has been certified that it is in equilibrium state with the decay daughters, and stable to be used for quality control purposes. Nevertheless, the homogeneous distribution of the doped material with the prepared source should be verified. This has been examined using gamma spectrometry measurements in conjunction with analysis of variance statistical tools, Dixon, box plots and Grubbs tests. The calculated total uncertainty has been utilized to establish the recommended specific activity ranges of 226 Ra, 224 Th, 214 Pb, 214 Bi and 210 Pb radioisotopes in the prepared source. The obtained results showed that the estimated uncertainty arising from the sample inhomogeneity has a significant contribution in the total uncertainty. The stability control charts of the ultra-low background gamma spectrometry system demonstrated the suitability of the prepared material for the purpose of quality control. However, the emitted gamma-rays from the prepared source covers the required energy range for determination of natural and artificial radionuclides in different species of environmental samples such as marine sediment, soil samples, and samples contaminated by naturally occurring radioactive material produced by oil industry. In addition, the material might be used for system calibration in case its traceability is proven. The experimental data revealed the significance of the homogeneity in preparing environmental samples for radioactivity measurements; in particular when small sample quantities of environmental samples are required to be analyzed. (author)

  5. Studies and further needed investigations on radioactive contaminants in soil samples

    International Nuclear Information System (INIS)

    Belivermis, M.; Kilic, O.; Topcuoglu, S.; Cotuk, Y.; Kalayci, G.; Pestreli, D.

    2009-01-01

    Following the Chernobyl nuclear reactor accident, the radionuclides were deposited on the marine and terrestrial environments of Turkey and other countries as wet and / or dry fallout. It is well known that, the soil is the main reservoir at the terrestrial environment. The geographic distribution of the Chernobyl radionuclides per unit area is significantly different. Many countries have drawn radiation maps using the radionuclide data of the soil samples. The radioecological monitoring study in the soil samples are also investigated in the our country. However, the exist data is limited for whole region of Turkey. In general, the type study, that make, in uncultivated soil sample use of different soil layers (0-5, 5-10, 10-20, 20-30 cm). In our previous studies, the activity concentration of gamma emitting radionuclides were determined in soil samples (0-5 cm) from the Thrace (73 sites) and East and South Marmara (100 sites) regions. Moreover, the mean values of the annual effective dose equivalent were also calculated. In literature, numerous studies have been published concerning vertical migration of 1 37Cs in uncultivated soil samples use of different soil types. However, we have not enough data on this subject. On the other hand, we want to present a previously published data on the vertical distribution of 1 37Cs radionuclide in an uncultivated site in the eastern Black Sea region. It is well known that the determination of soil to plant transfer factors of radiocesium that take account all economically crops on the soil varieties is a need to support dose assessment or countermeasure studies. Previously published IAEA reports, we determined transfer factors for some crops of 1 37Cs radionuclides in cultivated soil samples (0-20 cm depth) in the eastern Black Sea region. At the same time, we have given a new project to IAEA for the determination of transfer factor of radiocesium from soil to some crops for Akkuyu Nuclear Power Plant site.

  6. Curiosity analyzes Martian soil samples

    Science.gov (United States)

    Showstack, Randy; Balcerak, Ernie

    2012-12-01

    NASA's Mars Curiosity rover has conducted its first analysis of Martian soil samples using multiple instruments, the agency announced at a 3 December news briefing at the AGU Fall Meeting in San Francisco. "These results are an unprecedented look at the chemical diversity in the area," said NASA's Michael Meyer, program scientist for Curiosity.

  7. An evaluation of soil sampling for 137Cs using various field-sampling volumes.

    Science.gov (United States)

    Nyhan, J W; White, G C; Schofield, T G; Trujillo, G

    1983-05-01

    The sediments from a liquid effluent receiving area at the Los Alamos National Laboratory and soils from an intensive study area in the fallout pathway of Trinity were sampled for 137Cs using 25-, 500-, 2500- and 12,500-cm3 field sampling volumes. A highly replicated sampling program was used to determine mean concentrations and inventories of 137Cs at each site, as well as estimates of spatial, aliquoting, and counting variance components of the radionuclide data. The sampling methods were also analyzed as a function of soil size fractions collected in each field sampling volume and of the total cost of the program for a given variation in the radionuclide survey results. Coefficients of variation (CV) of 137Cs inventory estimates ranged from 0.063 to 0.14 for Mortandad Canyon sediments, whereas CV values for Trinity soils were observed from 0.38 to 0.57. Spatial variance components of 137Cs concentration data were usually found to be larger than either the aliquoting or counting variance estimates and were inversely related to field sampling volume at the Trinity intensive site. Subsequent optimization studies of the sampling schemes demonstrated that each aliquot should be counted once, and that only 2-4 aliquots out of as many as 30 collected need be assayed for 137Cs. The optimization studies showed that as sample costs increased to 45 man-hours of labor per sample, the variance of the mean 137Cs concentration decreased dramatically, but decreased very little with additional labor.

  8. On-line Automated Sample Preparation-Capillary Gas Chromatography for the Analysis of Plasma Samples.

    NARCIS (Netherlands)

    Louter, A.J.H.; van der Wagt, R.A.C.A.; Brinkman, U.A.T.

    1995-01-01

    An automated sample preparation module, (the automated sample preparation with extraction columns, ASPEC), was interfaced with a capillary gas chromatograph (GC) by means of an on-column interface. The system was optimised for the determination of the antidepressant trazodone in plasma. The clean-up

  9. Aluminium, extractable from soil samples by the acid ammonium acetate soil-testing method

    Directory of Open Access Journals (Sweden)

    Osmo Mäkitie

    1968-05-01

    Full Text Available The extractant, 0.5 M acetic acid –0.5 M ammonium acetate at pH 4.65, which is used in soil-testing, extracts relatively high amounts of aluminium from acid soils. The mean values of acetate-extractable aluminium at pH 4.65, 1.75 meq Al/100 g of soil, and of exchangeable aluminium (M KCI extraction, 0.41 meq Al were obtained from a material of 30 samples of acid soils (Table 2. Several other acetic acid ammonium acetate extractants, from M acetic acid to M ammonium acetate solution were also used for studying the extractability of soil aluminium. The soil-testing extractant can be used for the estimation of the soluble amounts of aluminium in acid soils, however, further studies are needed for a better interpretation of the ammonium acetate extractable (at pH 4.65 aluminium in our soils.

  10. Cr(VI) generation during sample preparation of solid samples – A ...

    African Journals Online (AJOL)

    Cr(VI) generation during sample preparation of solid samples – A chromite ore case study. R.I Glastonbury, W van der Merwe, J.P Beukes, P.G van Zyl, G Lachmann, C.J.H Steenkamp, N.F Dawson, M.H Stewart ...

  11. Laboratory and Airborne BRDF Analysis of Vegetation Leaves and Soil Samples

    Science.gov (United States)

    Georgiev, Georgi T.; Gatebe, Charles K.; Butler, James J.; King, Michael D.

    2008-01-01

    Laboratory-based Bidirectional Reflectance Distribution Function (BRDF) analysis of vegetation leaves, soil, and leaf litter samples is presented. The leaf litter and soil samples, numbered 1 and 2, were obtained from a site located in the savanna biome of South Africa (Skukuza: 25.0degS, 31.5degE). A third soil sample, number 3, was obtained from Etosha Pan, Namibia (19.20degS, 15.93degE, alt. 1100 m). In addition, BRDF of local fresh and dry leaves from tulip tree (Liriodendron tulipifera) and acacia tree (Acacia greggii) were studied. It is shown how the BRDF depends on the incident and scatter angles, sample size (i.e. crushed versus whole leaf,) soil samples fraction size, sample status (i.e. fresh versus dry leaves), vegetation species (poplar versus acacia), and vegetation s biochemical composition. As a demonstration of the application of the results of this study, airborne BRDF measurements acquired with NASA's Cloud Absorption Radiometer (CAR) over the same general site where the soil and leaf litter samples were obtained are compared to the laboratory results. Good agreement between laboratory and airborne measured BRDF is reported.

  12. Towards quantitative laser-induced breakdown spectroscopy analysis of soil samples

    International Nuclear Information System (INIS)

    Bousquet, B.; Sirven, J.-B.; Canioni, L.

    2007-01-01

    A quantitative analysis of chromium in soil samples is presented. Different emission lines related to chromium are studied in order to select the best one for quantitative features. Important matrix effects are demonstrated from one soil to the other, preventing any prediction of concentration in different soils on the basis of a univariate calibration curve. Finally, a classification of the LIBS data based on a series of Principal Component Analyses (PCA) is applied to a reduced dataset of selected spectral lines related to the major chemical elements in the soils. LIBS data of heterogeneous soils appear to be widely dispersed, which leads to a reconsideration of the sampling step in the analysis process

  13. An inter-lab comparison determination of radionuclides in soil samples by γ-apectrometry

    International Nuclear Information System (INIS)

    Pan Jingquan; Zhang Shurong; Xu Cuihua

    1986-01-01

    The results of an inter-lab comparison of quantitative determination of radionuclides in two soil samples and in an imitated one used as standard reference material by direct γ-spectrometry are presented and discussed. The methods of preparation of the three samples, its homogeneity and the procedures used in this inter-lab comparison are also described. Fifteen laboratories in China participated in this program. The contents of main radionuclides in the samples were estimated by statistical treatment of the reproted data. More than 91% of these laboratories obtained mean values with relative standard deviation below 20%, and in 88% of them the average values we e within the range of the standard reference values with deviation less than 10%. Statistical analysis showed that random error might be underestimated or systematic error might exist in a few laboratories

  14. Micro-PIXE evaluation of radioactive cesium transfer in contaminated soil samples

    International Nuclear Information System (INIS)

    Fujishiro, F.; Ishii, K.; Matsuyama, S.; Arai, H.; Ishizaki, A.; Osada, N.; Sugai, H.; Kusano, K.; Nozawa, Y.; Yamauchi, S.; Karahashi, M.; Oshikawa, S.; Kikuchi, K.; Koshio, S.; Watanabe, K.; Suzuki, Y.

    2014-01-01

    Highlights: • There are radioactively contaminated soils having a radioactive cesium transfer of 0.01. • Micro-PIXE analysis has revealed an existence of phosphorus in a contaminated soil. • Radioactive cesium captured by phosphorus compound would be due to radioactive transfer. -- Abstract: Micro-PIXE analysis has been performed on two soil samples with high cesium activity concentrations. These soil samples were contaminated by fallout from the accident at Fukushima Daiichi Nuclear Power Plant. One exhibits a radioactive cesium transfer of ∼0.01, and the other shows a radioactive cesium transfer of less than 0.001, even though both samples have high cesium activity concentrations exceeding 10,000 Bq/kg. X-ray spectra and elemental images of the soil samples revealed the presence of chlorine, which can react with cesium to produce an inorganic soluble compound, and phosphorus-containing cesium-capturable organic compounds

  15. Transformation mechanism of nutrient elements in the process of biochar preparation for returning biochar to soil

    Institute of Scientific and Technical Information of China (English)

    Shuangshuang Tian; Zhongxin Tan; Alfreda Kasiulienė; Ping Ai

    2017-01-01

    Returning biochar to soil is a heavily researched topic because biochar functions well for soil improvement. There is a significant loss of nutrients, which occurs during biochar preparation before biochar is returned to soil, thereby seriously undermining biochar's efficacy. Therefore, the transformation mechanisms of biochar pH, mass, nutrients and metals during pyrolysis under different atmospheres and temperatures were studied such that the best method for biochar preparation could be developed. Several conclusions can be reached: (1) a CO2 atmosphere is better than a N2 atmosphere for biochar preparation, although preparation in a CO2 atmosphere is not a common practice for biochar producers; (2) 350 ℃ is the best temperature for biochar preparation because the amount of nutrient loss is notably low based on the premise of straw transferred into biochar; and (3) transforming mechanisms of pH, N, P and K are also involved in the biochar preparation process.

  16. Statistical sampling strategies for survey of soil contamination

    NARCIS (Netherlands)

    Brus, D.J.

    2011-01-01

    This chapter reviews methods for selecting sampling locations in contaminated soils for three situations. In the first situation a global estimate of the soil contamination in an area is required. The result of the surey is a number or a series of numbers per contaminant, e.g. the estimated mean

  17. Soil sampling in emergency situations; Amostragem de solos em situacoes de emergencia

    Energy Technology Data Exchange (ETDEWEB)

    Carvalho, Zenildo Lara de [Instituto de Radioprotecao e Dosimetria (IRD), Rio de Janeiro, RJ (Brazil); Ramos Junior, Anthenor Costa [Comissao Nacional de Energia Nuclear (CNEN), Rio de Janeiro, RJ (Brazil). Superintendencia de Licenciamento e Controle

    1997-12-31

    The soil sampling methods used in Goiania`s accident (1987) by the environmental team of Brazilian Nuclear Energy Commission (CNEN) are described. The development of this method of soil sampling to a emergency sampling method used in a Nuclear Emergency Exercise in Angra dos Reis Reactor Site (1991) is presented. A new method for soil sampling based on a Chernobyl environmental monitoring experience (1995) is suggested. (author) 15 refs.

  18. Assessment of soil sample quality used for density evaluations through computed tomography

    International Nuclear Information System (INIS)

    Pires, Luiz F.; Arthur, Robson C.J.; Bacchi, Osny O.S.

    2005-01-01

    There are several methods to measure soil bulk density (ρ s ) like the paraffin sealed clod (PS), the volumetric ring (VR), the computed tomography (CT), and the neutron-gamma surface gauge (SG). In order to evaluate by a non-destructive way the possible modifications in soil structure caused by sampling for the PS and VR methods of ρ s evaluation we proposed to use the gamma ray CT method. A first generation tomograph was used having a 241 Am source and a 3 in x 3 in NaI(Tl) scintillation crystal detector coupled to a photomultiplier tube. Results confirm the effect of soil sampler devices on the structure of soil samples, and that the compaction caused during sampling causes significant alterations of soil bulk density. Through the use of CT it was possible to determine the level of compaction and to make a detailed analysis of the soil bulk density distribution within the soil sample. (author)

  19. Activity Concentration for Surface Soil Samples Collected from Arrant, Qena, Egypt

    International Nuclear Information System (INIS)

    Harb, S.; Salahel Din, K.; Abbady, A.; Moustafa, M.

    2010-01-01

    Soil samples were collected from four regions from Armant area. Qena, Upper Egypt for measure their natural radioactivity concentrations due to Ra-226, Th-232 and K-40 radionuclides. Thirty-Four surface soil samples were analyzed by using low-level gamma-spectrometric analysis. The average activity concentration for Ra-226 in (Bq/kg) in the collected soil samples were found to be 27.3 ±3.2, 11.4±1.09, 10.6±1.2, and 11.4±1.02 while the average value for Th-232 were 15.1±1.4, 11.1±0.77, 10.8 ± 0.72 and 11.1 ± 0.8 (Bq/kg) for soil samples from North, South, West and East. The corresponding average values for K-40 were 521.4±16.8, 463±14.8, 488.9±15.6 and 344.5±10.7 (Bq/kg), respectively. Based on radionuclides concentration in surface soil samples the radiological effects can be assessed

  20. Soil classification basing on the spectral characteristics of topsoil samples

    Science.gov (United States)

    Liu, Huanjun; Zhang, Xiaokang; Zhang, Xinle

    2016-04-01

    Soil taxonomy plays an important role in soil utility and management, but China has only course soil map created based on 1980s data. New technology, e.g. spectroscopy, could simplify soil classification. The study try to classify soils basing on the spectral characteristics of topsoil samples. 148 topsoil samples of typical soils, including Black soil, Chernozem, Blown soil and Meadow soil, were collected from Songnen plain, Northeast China, and the room spectral reflectance in the visible and near infrared region (400-2500 nm) were processed with weighted moving average, resampling technique, and continuum removal. Spectral indices were extracted from soil spectral characteristics, including the second absorption positions of spectral curve, the first absorption vale's area, and slope of spectral curve at 500-600 nm and 1340-1360 nm. Then K-means clustering and decision tree were used respectively to build soil classification model. The results indicated that 1) the second absorption positions of Black soil and Chernozem were located at 610 nm and 650 nm respectively; 2) the spectral curve of the meadow is similar to its adjacent soil, which could be due to soil erosion; 3) decision tree model showed higher classification accuracy, and accuracy of Black soil, Chernozem, Blown soil and Meadow are 100%, 88%, 97%, 50% respectively, and the accuracy of Blown soil could be increased to 100% by adding one more spectral index (the first two vole's area) to the model, which showed that the model could be used for soil classification and soil map in near future.

  1. Current trends in sample preparation for cosmetic analysis.

    Science.gov (United States)

    Zhong, Zhixiong; Li, Gongke

    2017-01-01

    The widespread applications of cosmetics in modern life make their analysis particularly important from a safety point of view. There is a wide variety of restricted ingredients and prohibited substances that primarily influence the safety of cosmetics. Sample preparation for cosmetic analysis is a crucial step as the complex matrices may seriously interfere with the determination of target analytes. In this review, some new developments (2010-2016) in sample preparation techniques for cosmetic analysis, including liquid-phase microextraction, solid-phase microextraction, matrix solid-phase dispersion, pressurized liquid extraction, cloud point extraction, ultrasound-assisted extraction, and microwave digestion, are presented. Furthermore, the research and progress in sample preparation techniques and their applications in the separation and purification of allowed ingredients and prohibited substances are reviewed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. The Recent Developments in Sample Preparation for Mass Spectrometry-Based Metabolomics.

    Science.gov (United States)

    Gong, Zhi-Gang; Hu, Jing; Wu, Xi; Xu, Yong-Jiang

    2017-07-04

    Metabolomics is a critical member in systems biology. Although great progress has been achieved in metabolomics, there are still some problems in sample preparation, data processing and data interpretation. In this review, we intend to explore the roles, challenges and trends in sample preparation for mass spectrometry- (MS-) based metabolomics. The newly emerged sample preparation methods were also critically examined, including laser microdissection, in vivo sampling, dried blood spot, microwave, ultrasound and enzyme-assisted extraction, as well as microextraction techniques. Finally, we provide some conclusions and perspectives for sample preparation in MS-based metabolomics.

  3. CRADA Carbon Sequestration in Soils and Commercial Products

    Energy Technology Data Exchange (ETDEWEB)

    Jacobs, G.K.

    2002-01-31

    ORNL, through The Consortium for Research on Enhancing Carbon Sequestration in Terrestrial Ecosystems (CSiTE), collaborated with The Village Botanica, Inc. (VB) on a project investigating carbon sequestration in soils and commercial products from a new sustainable crop developed from perennial Hibiscus spp. Over 500 pre-treated samples were analyzed for soil carbon content. ORNL helped design a sampling scheme for soils during the planting phase of the project. Samples were collected and prepared by VB and analyzed for carbon content by ORNL. The project did not progress to a Phase II proposal because VB declined to prepare the required proposal.

  4. Characterisation of a reference site for quantifying uncertainties related to soil sampling

    International Nuclear Information System (INIS)

    Barbizzi, Sabrina; Zorzi, Paolo de; Belli, Maria; Pati, Alessandra; Sansone, Umberto; Stellato, Luisa; Barbina, Maria; Deluisa, Andrea; Menegon, Sandro; Coletti, Valter

    2004-01-01

    An integrated approach to quality assurance in soil sampling remains to be accomplished. - The paper reports a methodology adopted to face problems related to quality assurance in soil sampling. The SOILSAMP project, funded by the Environmental Protection Agency of Italy (APAT), is aimed at (i) establishing protocols for soil sampling in different environments; (ii) assessing uncertainties associated with different soil sampling methods in order to select the 'fit-for-purpose' method; (iii) qualifying, in term of trace elements spatial variability, a reference site for national and international inter-comparison exercises. Preliminary results and considerations are illustrated

  5. Decision support tool for soil sampling of heterogeneous pesticide (chlordecone) pollution.

    Science.gov (United States)

    Clostre, Florence; Lesueur-Jannoyer, Magalie; Achard, Raphaël; Letourmy, Philippe; Cabidoche, Yves-Marie; Cattan, Philippe

    2014-02-01

    When field pollution is heterogeneous due to localized pesticide application, as is the case of chlordecone (CLD), the mean level of pollution is difficult to assess. Our objective was to design a decision support tool to optimize soil sampling. We analyzed the CLD heterogeneity of soil content at 0-30- and 30-60-cm depth. This was done within and between nine plots (0.4 to 1.8 ha) on andosol and ferralsol. We determined that 20 pooled subsamples per plot were a satisfactory compromise with respect to both cost and accuracy. Globally, CLD content was greater for andosols and the upper soil horizon (0-30 cm). Soil organic carbon cannot account for CLD intra-field variability. Cropping systems and tillage practices influence the CLD content and distribution; that is CLD pollution was higher under intensive banana cropping systems and, while upper soil horizon was more polluted than the lower one with shallow tillage (pollution in the soil profile. The decision tool we proposed compiles and organizes these results to better assess CLD soil pollution in terms of sampling depth, distance, and unit at field scale. It accounts for sampling objectives, farming practices (cropping system, tillage), type of soil, and topographical characteristics (slope) to design a relevant sampling plan. This decision support tool is also adaptable to other types of heterogeneous agricultural pollution at field level.

  6. Study of Organochlorinated Pesticide Residues and Polychlorinated Biphenyls in Soil Samples

    Directory of Open Access Journals (Sweden)

    MSc. Vlora Gashi

    2013-12-01

    Full Text Available This paper presents and discusses the data obtained for organochlorinated pesticides and their residues in the soil samples of agricultural areas. Soil contamination is one of most important factors influencing the quality of agricultural products. Usage of heavy farm equipment, the land drainage, an exces­sive application of agrochemicals, emissions originating from mining, metallurgical, and chemical and coal power plants and transport, all generate a number of undesired substances (nitric and sulphur oxides, PAHs, heavy metals, pesticides, which after deposition in soil may influence crop quality. Thus, input of these contaminants into the environment should be carefully monitored. Levels of organochlorinated pesticides contamination were evaluated in agriculture areas that are in use. 10 soil samples were taken in agricultural areas  Plane of  Dugagjini , Kosovo. Representa­tive soil samples were collected from 0-30 cm top layer of the soil. In the analytical method we combined ultrasonic bath extraction and a Florisil column for samples clean-up. The analysis of the organochlorinated pesticides in soil samples was performed by gas chromatography technique using electron capture detector (GC/ECD. Optima-5 (low/mid polarity, 5% phenyl methyl siloxane 60 m x 0.33 mm x 0.25μm film capillary column was used for isolation and determination of organochlorinated pesticides. Low concentrations of organochlorinated pesticide and their metabolites were found in the studied samples. The presence of organochlorinated pesticides and their residues is probably resulting of their previous uses for agricultural purposes.

  7. Micro-PIXE evaluation of radioactive cesium transfer in contaminated soil samples

    Science.gov (United States)

    Fujishiro, F.; Ishii, K.; Matsuyama, S.; Arai, H.; Ishizaki, A.; Osada, N.; Sugai, H.; Kusano, K.; Nozawa, Y.; Yamauchi, S.; Karahashi, M.; Oshikawa, S.; Kikuchi, K.; Koshio, S.; Watanabe, K.; Suzuki, Y.

    2014-01-01

    Micro-PIXE analysis has been performed on two soil samples with high cesium activity concentrations. These soil samples were contaminated by fallout from the accident at Fukushima Daiichi Nuclear Power Plant. One exhibits a radioactive cesium transfer of ˜0.01, and the other shows a radioactive cesium transfer of less than 0.001, even though both samples have high cesium activity concentrations exceeding 10,000 Bq/kg. X-ray spectra and elemental images of the soil samples revealed the presence of chlorine, which can react with cesium to produce an inorganic soluble compound, and phosphorus-containing cesium-capturable organic compounds.

  8. Method validation and dissipation kinetics of four herbicides in maize and soil using QuEChERS sample preparation and liquid chromatography tandem mass spectrometry.

    Science.gov (United States)

    Pang, Nannan; Wang, Tielong; Hu, Jiye

    2016-01-01

    A versatile liquid chromatography tandem mass spectrometry method with modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) sample preparation was developed for the determination of rimsulfuron, mesotrione, fluroxypyr-meptyl, and fluroxypyr. By adjusting the amount of graphitized carbon black, the herbicide analytes could be quantified with satisfactory recoveries in the range of 80-110%. A dissipation kinetics study conducted under open field conditions at two sites during 2014 showed first order equations with half-lives between 0.6d and 3.6d, illustrating an appropriate degree of stability and safety. The dissipation kinetics were different in the different matrices. Although the herbicides had higher initial residues in straw than those in soil, they degraded faster in straw. The terminal residues for the herbicides formulated in two water dispersible granules were all below maximum residue limits. These results not only gave insights about the analytes but also contributed to environmental protection and food safety. Copyright © 2015 Elsevier Ltd. All rights reserved.

  9. 7 CFR 61.34 - Drawing and preparation of sample.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Drawing and preparation of sample. 61.34 Section 61.34 Agriculture Regulations of the Department of Agriculture (Continued) AGRICULTURAL MARKETING SERVICE (Standards... Cottonseed Samplers § 61.34 Drawing and preparation of sample. Each licensed cottonseed sampler shall draw...

  10. Measurement of technetium-99 in Marshall Islands soil samples by ICP-MS

    Science.gov (United States)

    Tagami; Uchida; Hamilton; Robison

    2000-07-01

    Extraction techniques for recovery of technetium-99 (99Tc) for Inductively Coupled Plasma Mass Spectrometry (ICP-MS) measurements were evaluated using soil samples collected from the Marshall Islands. The results of three different extraction techniques were compared: (MI) acid leaching of Tc from ashed soil; (M2) acid leaching of Tc from raw dry soil; and (M3) Tc volatilization from ashed soil using a combustion apparatus. Total Tc recoveries varied considerably between the extraction techniques but each method yielded similar analytical results for 99Tc. Applications of these extraction techniques to a series of environmental samples and ICP-MS measurements have yielded first data on the 99Tc content of Marshall Islands soil samples contaminated with close-in radioactive fallout from nuclear weapons testing. The 99Tc activity concentration in the soil samples ranged between 0.1 and 1.1 mBq g(-1) dry weight (dw). The limit of detection for 99Tc by ICP-MS was 0.17 mBq per sample or 0.014 mBq g(-1) dw under standard operating conditions.

  11. Measurement of technetium-99 in Marshall Islands soil samples by ICP-MS

    International Nuclear Information System (INIS)

    Tagami, K.; Uchida, S.; Hamilton, T.; Robison, W.

    2000-01-01

    Extraction techniques for recovery of technetium-99 ( 99 Tc) for Inductively Coupled Plasma Mass Spectrometry (ICP-MS) measurements were evaluated using soil samples collected from the Marshall Islands. The results of three different extraction techniques were compared: (M1) acid leaching of Tc from ashed soil; (M2) acid leaching of Tc from raw dry soil; and (M3) Tc volatilization from ashed soil using a combustion apparatus. Total Tc recoveries varied considerably between the extraction techniques but each method yielded similar analytical results for 99 Tc. Applications of these extraction techniques to a series of environmental samples and ICP-MS measurements have yielded first data on the 99 Tc content of Marshall Islands soil samples contaminated with close-in radioactive fallout from nuclear weapons testing. The 99 Tc activity concentration in the soil samples ranged between 0.1 and 1.1 mBq g -1 dry weight (dw). The limit of detection for 99 Tc by ICP-MS was 0.17 mBq per sample or 0.014 mBq g -1 dw under standard operating conditions

  12. How much will afforestation of former cropland influence soil C stocks? A synthesis of paired sampling, chronosequence sampling and repeated sampling studies

    Science.gov (United States)

    Vesterdal, Lars; Hansen, K.; Stupak, I.; Don, Axel; Poeplau, C.; Leifeld, Jens; van Wesemael, Bas

    2010-05-01

    The need for documentation of land-use change effects on soil C is high on the agenda in most signatory countries to the Kyoto Protocol. Large land areas in Europe have experienced land-use change from cropland to forest since 1990 by direct afforestation as well as abandonment and regrowth of marginally productive cropland. Soil C dynamics following land-use change remain highly uncertain due to a limited number of available studies and due to influence of interacting factors such as land use history, soil type, and climate. Common approaches for estimation of potential soil C changes following land-use change are i) paired sampling of plots with a long legacy of different land uses, ii) chronosequence studies of land-use change, and lastly iii) repeated sampling of plots subject to changed land use. This paper will synthesize the quantitative effects of cropland afforestation on soil C sequestration based on all three approaches and will report on related work within Cost 639. Paired plots of forest and cropland were used to study the general differences between soil C stocks in the two land uses. At 27 sites in Denmark distributed among different regions and soil types forest floor and mineral soil were sampled in and around soil pits. Soil C stocks were higher in forest than cropland (mean difference 22 Mg C ha-1 to 1 m depth). This difference was caused solely by the presence of a forest floor in forests; mineral soil C stocks were similar (108 vs. 109 Mg C ha-1) in the two land uses regardless of soil type and the soil layers considered. The chronosequence approach was employed in the AFFOREST project for evaluation of C sequestration in biomass and soils following afforestation of cropland. Two oak (Quercus robur) and four Norway spruce (Picea abies) afforestation chronosequences (age range 1 to 90 years) were studied in Denmark, Sweden and the Netherlands. Forest floor and mineral soil (0-25 cm) C contents were as a minimum unchanged and in most cases there

  13. 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).

  14. Composite Sampling Approaches for Bacillus anthracis Surrogate Extracted from Soil.

    Directory of Open Access Journals (Sweden)

    Brian France

    Full Text Available Any release of anthrax spores in the U.S. would require action to decontaminate the site and restore its use and operations as rapidly as possible. The remediation activity would require environmental sampling, both initially to determine the extent of contamination (hazard mapping and post-decon to determine that the site is free of contamination (clearance sampling. Whether the spore contamination is within a building or outdoors, collecting and analyzing what could be thousands of samples can become the factor that limits the pace of restoring operations. To address this sampling and analysis bottleneck and decrease the time needed to recover from an anthrax contamination event, this study investigates the use of composite sampling. Pooling or compositing of samples is an established technique to reduce the number of analyses required, and its use for anthrax spore sampling has recently been investigated. However, use of composite sampling in an anthrax spore remediation event will require well-documented and accepted methods. In particular, previous composite sampling studies have focused on sampling from hard surfaces; data on soil sampling are required to extend the procedure to outdoor use. Further, we must consider whether combining liquid samples, thus increasing the volume, lowers the sensitivity of detection and produces false negatives. In this study, methods to composite bacterial spore samples from soil are demonstrated. B. subtilis spore suspensions were used as a surrogate for anthrax spores. Two soils (Arizona Test Dust and sterilized potting soil were contaminated and spore recovery with composites was shown to match individual sample performance. Results show that dilution can be overcome by concentrating bacterial spores using standard filtration methods. This study shows that composite sampling can be a viable method of pooling samples to reduce the number of analysis that must be performed during anthrax spore remediation.

  15. Tooth enamel sample preparation using alkaline treatment in ESR dosimetry

    International Nuclear Information System (INIS)

    Yongzeng, Zhou; Jiadong, Wang; Xiaomei, Jia; Ke, Wu; Jianbo, Cong

    2002-01-01

    Tooth enamel sample preparation using alkaline treatment was studied and compared with traditional mechanical method in this paper. 20 adult teeth were used. Samples were placed into NaOH solution. This method requires 4-5 weeks and the enamel was separated from dentin. Experimental results show that 8M NaOH was appropriate for separating enamel from dentin and that there is no difference in background signal relative intensity between samples prepared by mechanical and by chemical methods. There is also no difference in radiosensitivity between samples prepared by two methods mentioned above. Dose response curve for tooth enamel samples isolated by 8M NaOH solution was obtained

  16. Sample preparation for special PIE-techniques at ITU

    International Nuclear Information System (INIS)

    Toscano, E.H.; Manzel, R.

    2002-01-01

    Several sample preparation techniques were developed and installed in hot cells. The techniques were conceived to evaluate the performance of highly burnt fuel rods and include: (a) a device for the removal of the fuel, (b) a method for the preparation of the specimen ends for the welding of new end caps and for the careful cleaning of samples for Transmission Electron Microscopy and Glow Discharge Mass Spectroscopy, (c) a sample pressurisation device for long term creep tests, and (d) a diameter measuring device for creep or burst samples. Examples of the determination of the mechanical properties, the behaviour under transient conditions and for the assessment of the corrosion behaviour of high burnup cladding materials are presented. (author)

  17. Mixed functional monomers-based monolithic adsorbent for the effective extraction of sulfonylurea herbicides in water and soil samples.

    Science.gov (United States)

    Pei, Miao; Zhu, Xiangyu; Huang, Xiaojia

    2018-01-05

    Effective extraction is a key step in the determination of sulfonylurea herbicides (SUHs) in complicated samples. According to the chemical properties of SUHs, a new monolithic adsorbent utilizing acrylamidophenylboronic acid and vinylimidazole as mixed functional monomers was synthesized. The new adsorbent was employed as the extraction phase of multiple monolithic fiber solid-phase microextraction (MMF-SPME) of SUHs, and the extracted SUHs were determined by high-performance liquid chromatography with diode array detection (HPLC-DAD). Results well evidence that the prepared adsorbent could extract SUHs in environmental waters and soil effectively through multiply interactions such as boronate affinity, dipole-dipole and π-π interactions. Under the optimized extraction conditions, the limits of detection for target SUHs in environmental water and soil samples were 0.018-0.17μg/L and 0.14-1.23μg/kg, respectively. At the same time, the developed method also displayed some analytical merits including wide linear dynamic ranges, good method reproducibility, satisfactory sensitivity and low consume of organic solvent. Finally, the developed were successfully applied to monitor trace SUHs in environmental water and soil samples. The recoveries at three fortified concentrations were in the range of 70.6-119% with RSD below 11% in all cases. The obtained results well demonstrate the excellent practical applicability of the developed MMF-SPME-HPLC-DAD method for the monitoring of SUHs in water and soil samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Planning Considerations Related to Collecting and Analyzing Samples of the Martian Soils

    Science.gov (United States)

    Liu, Yang; Mellon, Mike T.; Ming, Douglas W.; Morris, Richard V.; Noble, Sarah K.; Sullivan, Robert J.; Taylor, Lawrence A.; Beaty, David W.

    2014-01-01

    The Mars Sample Return (MSR) End-to-End International Science Analysis Group (E2E-iSAG [1]) established scientific objectives associ-ated with Mars returned-sample science that require the return and investigation of one or more soil samples. Soil is defined here as loose, unconsolidated materials with no implication for the presence or absence of or-ganic components. The proposed Mars 2020 (M-2020) rover is likely to collect and cache soil in addition to rock samples [2], which could be followed by future sample retrieval and return missions. Here we discuss key scientific consid-erations for sampling and caching soil samples on the proposed M-2020 rover, as well as the state in which samples would need to be preserved when received by analysts on Earth. We are seeking feedback on these draft plans as input to mission requirement formulation. A related planning exercise on rocks is reported in an accompanying abstract [3].

  19. A generalized transmission method for gamma-efficiency determinations in soil samples

    International Nuclear Information System (INIS)

    Bolivar, J.P.; Garcia-Tenorio, R.; Garcia-Leon, M.

    1994-01-01

    In this paper, a generalization of the γ-ray transmission method which is useful for measurements on soil samples, for example, is presented. The correction factor, f, is given, which is a function of the apparent density of the soil and the γ-ray energy. With this method, the need for individual determinations of f, for each energy and apparent soil density is avoided. Although the method has been developed for soils, the general philosophy can be applied to other sample matrices, such as water or vegetables for example. (author)

  20. Use of passive sampling devices to determine soil contaminant concentrations

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, K.A. [Clemson Univ., Pendleton, SC (United States)]|[Washington State Univ., Richland, WA (United States); Hooper, M.J. [Clemson Univ., Pendleton, SC (United States); Weisskopf, C.P. [Washington State Univ., Richland, WA (United States)

    1996-12-31

    The effective remediation of contaminated sites requires accurate identification of chemical distributions. A rapid sampling method using passive sampling devices (PSDs) can provide a thorough site assessment. We have been pursuing their application in terrestrial systems and have found that they increase the ease and speed of analysis, decrease solvent usage and overall cost, and minimize the transport of contaminated soils. Time and cost savings allow a higher sampling frequency than is generally the case using traditional methods. PSDs have been used in the field in soils of varying physical properties and have been successful in estimating soil concentrations ranging from 1 {mu}g/kg (parts per billion) to greater than 200 mg/kg (parts per million). They were also helpful in identifying hot spots within the sites. Passive sampling devices show extreme promise as an analytical tool to rapidly characterize contaminant distributions in soil. There are substantial time and cost savings in laboratory personnel and supplies. By selectively excluding common interferences that require sample cleanup, PSDs can be retrieved from the field and processed rapidly (one technician can process approximately 90 PSDs in an 8-h work day). The results of our studies indicate that PSDs can be used to accurately estimate soil contaminant concentrations and provide lower detection limits. Further, time and cost savings will allow a more thorough and detailed characterization of contaminant distributions. 13 refs., 4 figs., 2 tabs.

  1. Statistical sampling approaches for soil monitoring

    NARCIS (Netherlands)

    Brus, D.J.

    2014-01-01

    This paper describes three statistical sampling approaches for regional soil monitoring, a design-based, a model-based and a hybrid approach. In the model-based approach a space-time model is exploited to predict global statistical parameters of interest such as the space-time mean. In the hybrid

  2. Cesium-137 and natural radionuclides in soils from southern Brazil and soils and others environmental samples from Antarctic

    International Nuclear Information System (INIS)

    Schuch, L.A.

    1993-04-01

    This work presents a study of environmental artificial and natural radioactivity levels in soil samples from the Southern Brazil and in soils and other environmental samples form Antarctica. Artificial radioactivity was determined by measuring Cs-137 which is a 30.1 year half-life man-made radionuclide produced in the past by atmospheric tests of nuclear weapons. Natural radioactivity was determined by measuring some radionuclides belonging to Th-232 and U-238 natural radioactive families, and of K-40 concentrations. Several types of soils from Southern Brazil; and soil samples, marine sediments, lichens, mosses and algae collected at King George and other nearby islands (South Shetland Archipelago, Antarctica) were analyzed. A gamma-ray spectrometer was used to measure radioactivity levels of the collected samples and its overall characteristics are analyzed in this work. (author)

  3. Report on the NAT-9 quality control exercise on uranium isotopes in two soil samples

    International Nuclear Information System (INIS)

    Bleise, Andreas

    2001-04-01

    The International Atomic Energy Agency (IAEA) section of Nutritional and Health related Environmental Studies (NAHRES) organized a quality control study for laboratories analysing samples from the UNEP field mission to Kosovo. Quality control was the major responsibility of the IAEA in the UN field assessment team. The NAT-9 quality control study consists of two soil materials from the IAEA Laboratories in Seibersdorf. The scope of this exercise was to determine the content of the uranium isotopes U-234, U-235 and U-238. The IAEA did not provide specific instructions, the participants were encouraged to apply their established analytical procedures to the samples. Five laboratories were invited to participate, four laboratories submitted results. For each soil sample 10 laboratory mean values were reported, using ICP-MS (3 laboratories) and α-spectrometry (1 laboratory). The participating laboratories were capable to distinguish the different uranium isotopes. All laboratories obtained the natural uranium ratio between U-235 and U-238. However, the results highlight a particular analytical weak spot. Although the methods of measuring the analytical signals are highly dependable, the sample preparation steps, in particular the sample dissolution procedure, appears to be lacking total quality control and has contributed to the deviations from the reported target values. One laboratory has documented evidence that extensive and well-controlled digestion methods can yield measurement results close to the target values. (author)

  4. Using Environmental Variables for Studying of the Quality of Sampling in Soil Mapping

    Directory of Open Access Journals (Sweden)

    A. Jafari

    2016-02-01

    Full Text Available Introduction: Methods of soil survey are generally empirical and based on the mental development of the surveyor, correlating soil with underlying geology, landforms, vegetation and air-photo interpretation. Since there are no statistical criteria for traditional soil sampling; this may lead to bias in the areas being sampled. In digital soil mapping, soil samples may be used to elaborate quantitative relationships or models between soil attributes and soil covariates. Because the relationships are based on the soil observations, the quality of the resulting soil map depends also on the soil observation quality. An appropriate sampling design for digital soil mapping depends on how much data is available and where the data is located. Some statistical methods have been developed for optimizing data sampling for soil surveys. Some of these methods deal with the use of ancillary information. The purpose of this study was to evaluate the quality of sampling of existing data. Materials and Methods: The study area is located in the central basin of the Iranian plateau (Figure 1. The geologic infrastructure of the area is mainly Cretaceous limestone, Mesozoic shale and sandstone. Air photo interpretation (API was used to differentiate geomorphic patterns based on their formation processes, general structure and morphometry. The patterns were differentiated through a nested geomorphic hierarchy (Fig. 2. A four-level geomorphic hierarchy is used to breakdown the complexity of different landscapes of the study area. In the lower level of the hierarchy, the geomorphic surfaces, which were formed by a unique process during a specific geologic time, were defined. A stratified sampling scheme was designed based on geomorphic mapping. In the stratified simple random sampling, the area was divided into sub-areas referred to as strata based on geomorphic surfaces, and within each stratum, sampling locations were randomly selected (Figure 2. This resulted in 191

  5. Measurement of technetium-99 in Marshall Islands soil samples by ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Tagami, K. E-mail: k_tagami@nirs.go.jp; Uchida, S.; Hamilton, T.; Robison, W

    2000-07-15

    Extraction techniques for recovery of technetium-99 ({sup 99}Tc) for Inductively Coupled Plasma Mass Spectrometry (ICP-MS) measurements were evaluated using soil samples collected from the Marshall Islands. The results of three different extraction techniques were compared: (M1) acid leaching of Tc from ashed soil; (M2) acid leaching of Tc from raw dry soil; and (M3) Tc volatilization from ashed soil using a combustion apparatus. Total Tc recoveries varied considerably between the extraction techniques but each method yielded similar analytical results for {sup 99}Tc. Applications of these extraction techniques to a series of environmental samples and ICP-MS measurements have yielded first data on the {sup 99}Tc content of Marshall Islands soil samples contaminated with close-in radioactive fallout from nuclear weapons testing. The {sup 99}Tc activity concentration in the soil samples ranged between 0.1 and 1.1 mBq g{sup -1} dry weight (dw). The limit of detection for {sup 99}Tc by ICP-MS was 0.17 mBq per sample or 0.014 mBq g{sup -1} dw under standard operating conditions.

  6. Removal of fission products from waste solutions using 16 different soil samples

    International Nuclear Information System (INIS)

    Bangash, M.A.; Hanif, J.

    1997-01-01

    Most of the nuclear sites use pits in the surrounding soils for the storage/disposal of low active waste (LAW) solutions. The characteristics of the soil if not suitable for the fixation or adsorption of the radioactive nuclides, may cause migration of these nuclides to hydrosphere. The phenomenon has the risk of radio toxic pollution for the living bodies therefore minerals composing the soil and their adsorption properties need to be investigated. For this purpose 16 different soil samples were collected from all over Pakistan. Mineralogical composition of the soils was determined by X-ray diffraction analysis. It was found that most of the samples contained clay minerals, illite, kaolinite and montmorillonite. Studies for the removal of fission products like, /sup 137/Cs. /sup 60/Sr and activation product /sup 60/CO from solution were carried out on these samples. The sorption experiments were performed by batch technique using radioactive as tracers. Distribution co-efficient were determined by mixing he element solution at pH 3 with the soil at soil solution ratios of 1 to 20. It is revealed from the experimental data that efficient removal of fission products from solutions is achieved by soil samples containing clay mineral montmorillonite, followed by little and kaolinite. These soils thus can be effectively used for the disposal of low level radioactive waste solutions without causing any environmental hazard. (author)

  7. The standardization of an apparatus for the mixing of soil samples ...

    African Journals Online (AJOL)

    Quantitative determination of nematode populations in soils frequently necessitates the mixing of representative soil samples to form a homogeneous, compound sample from which the nematodes are extracted. A mixing apparatus was developed and standardized with the aid of a spectrophotometric technique by which ...

  8. Sample preparations for spark source mass spectrography

    International Nuclear Information System (INIS)

    Catlett, C.W.; Rollins, M.B.; Griffin, E.B.; Dorsey, J.G.

    1977-10-01

    Methods have been developed for the preparation of various materials for spark source mass spectrography. The essential features of these preparations (all which can provide adequate precision in a cost-effective manner) consist in obtaining spark-stable electrode sample pieces, a common matrix, a reduction of anomolous effects in the spark, the incorporation of a suitable internal standard for plate response normalization, and a reduction in time

  9. Present status of NMCC and sample preparation method for bio-samples

    International Nuclear Information System (INIS)

    Futatsugawa, S.; Hatakeyama, S.; Saitou, S.; Sera, K.

    1993-01-01

    In NMCC(Nishina Memorial Cyclotron Center) we are doing researches on PET of nuclear medicine (Positron Emission Computed Tomography) and PIXE analysis (Particle Induced X-ray Emission) using a small cyclotron of compactly designed. The NMCC facilities have been opened to researchers of other institutions since April 1993. The present status of NMCC is described. Bio-samples (medical samples, plants, animals and environmental samples) have mainly been analyzed by PIXE in NMCC. Small amounts of bio-samples for PIXE are decomposed quickly and easily in a sealed PTFE (polytetrafluoroethylene) vessel with a microwave oven. This sample preparation method of bio-samples also is described. (author)

  10. Soil map disaggregation improved by soil-landscape relationships, area-proportional sampling and random forest implementation

    DEFF Research Database (Denmark)

    Møller, Anders Bjørn; Malone, Brendan P.; Odgers, Nathan

    implementation generally improved the algorithm’s ability to predict the correct soil class. The implementation of soil-landscape relationships and area-proportional sampling generally increased the calculation time, while the random forest implementation reduced the calculation time. In the most successful......Detailed soil information is often needed to support agricultural practices, environmental protection and policy decisions. Several digital approaches can be used to map soil properties based on field observations. When soil observations are sparse or missing, an alternative approach...... is to disaggregate existing conventional soil maps. At present, the DSMART algorithm represents the most sophisticated approach for disaggregating conventional soil maps (Odgers et al., 2014). The algorithm relies on classification trees trained from resampled points, which are assigned classes according...

  11. Investigation of the uranium content in sediment and soil samples from the Santos and Sao Vicente estuary region, SP, Brazil

    International Nuclear Information System (INIS)

    Serafim, Ricardo A.M.; Correa, Bianca A.M.; Primi, M.C.; Geraldo, Luiz P.; Yamazaki, Yone M.

    2009-01-01

    In this work the uranium (U) content in sediment and soil samples collected near the Santos and Sao Vicente estuary was determined using the fission track registration technique (SSNTD). The sediment and soil samples after oven-dried and pulverized were prepared in the solution form. Around 10 μL of this solution was deposited on the plastic detector (PCLIGHT) and irradiated at the IEA-R1 (3.5 MW) nuclear reactor. After the irradiation and chemical etching of the plastic foils, the fission tracks were counted with a system consisting of an optical microscope together with a video camera and a PC computer. The U content in the analyzed samples ranged from 3.12 ± 0.55 to 18.3 ± 1.2 ppm for sediments and from 3.21 ± 0.63 to 11.5 ± 1.1 ppm for soils. These results were compared to other values reported in the literature for sediments and soils collected in environments similar to the ones studied in this work The average values for the U content obtained in this work are significant higher (above twice) than the world mean and are in reasonable agreement with results found by other authors for sediments and soils from regions considered as polluted or with a high level of radioactivity. (author)

  12. Specification for soil multisensor and soil sampling cone penetrometer probes

    International Nuclear Information System (INIS)

    Iwatate, D.F.

    1997-01-01

    Specification requirements for engineering, fabrication, and performance of cone penetrometer (CP) soil multisensor and sampling probes (CP-probes) which are required to support contract procurement for services are presented. The specification provides a documented technical basis of quality assurance that is required to use the probes in an operating Hanford tank farm. The documentation cited in this specification will be incorporated into an operational fielding plan that will address all activities associated with the use of the CP-probes. The probes discussed in this specification support the Hanford Tanks Initiative AX-104 Tank Plume Characterization Sub-task. The probes will be used to interrogate soils and vadose zone surrounding tank AX-104

  13. 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

  14. Influences of different sample preparation methods on tooth enamel ESR signals

    International Nuclear Information System (INIS)

    Zhang Wenyi; Jiao Ling; Zhang Liang'an; Pan Zhihong; Zeng Hongyu

    2005-01-01

    Objective: To study the influences of different sample preparation methods on tooth enamel ESR signals in order to reduce the effect of dentine on their sensitivities to radiation. Methods: The enamel was separated from dentine of non-irradiated adult teeth by mechanical, chemical, or both methods. The samples of different preparations were scanned by an ESR spectrometer before and after irradiation. Results: The response of ESR signals of samples prepared with different methods to radiation dose was significantly different. Conclusion: The selection of sample preparation method is very important for dose reconstruction by tooth enamel ESR dosimetry, especially in the low dose range. (authors)

  15. Microbiological evaluation on toxicity amelioration of soil samples contaminated with petroleum-based products

    International Nuclear Information System (INIS)

    Khairuddin Abdul Rahim; Pauline Liew Woan Ying; Ahmad Nazrul Abd Wahid; Shamsiah Abdul Rahman; Mohd Suhaimi Hamzah; Abdul Khalik Wood; Muhamat Omar

    2004-01-01

    Samples of soil materials from oil sludge landfarm in Melaka and petroleum sludge ready for disposal were analysed on their potentially toxic elements and compounds and their microbial population. These were compared against uncontaminated soil samples from agricultural plots and fresh crude petroleum samples obtained from an oil refinery in Kerteh, Terengganu. Enumeration and isolation of culturable microbial populations in the above samples were conducted using standard plate counts and screening methods. Populations of microorganisms from uncontaminated soils were tested on its potential to degrade petroleum derived products on contaminated soil samples and crude petroleum samples in a laboratory experiment. Microorganisms with great potential to degrade petroleum sludge will be further screened in further bioremediation studies in the field. (Author)

  16. Determination of metals in scots pine (Pinus Sylvestris) needles and soil samples

    International Nuclear Information System (INIS)

    Ludborzs, A.; Viksna, A.

    2000-01-01

    Current report is the finding to apply two modern and powerful methods of microanalysis - Total Reflection X-ray Fluorescence Spectrometry (TXRF) and Graphite Furnace Atomic Absorption Spectrometry - for the analysis of biological and geological materials. For some of the measurements Instrumental Neutron Activation Analysis (INAA) has been used as an arbitrary method. The goal of the research project is to find possible relationships between metals content in the Scots pine (Pinus sylvestris) needles and the soil samples, which have been taken under the trees. The objectives of the work are analysis of both needles and soils, pH measurements of the soil samples, and handling of a simplified metal speciation analysis in the soil samples. For statistical reliability of the project, seven pine trees from different locations in Latvia have been chosen as the analysis objects. Samples of 20 different age class needles have been collected from the trees and 21 soil sample has been sampled under the trees. K, Ca, Mn, Fe, Zn, Rb, Sr, Pb, and Cd content have been analysed in both samples of the needles and the soils. The obtained measurement data have been processed according to the aim of the project. Relevant questions about causal differences of metal concentrations in different age classes of needles, about subtle working principles of the plant's root system, about the role of some elements in the plant's living processes still remain unanswered. (author)

  17. Global metabolite analysis of yeast: evaluation of sample preparation methods

    DEFF Research Database (Denmark)

    Villas-Bôas, Silas Granato; Højer-Pedersen, Jesper; Åkesson, Mats Fredrik

    2005-01-01

    Sample preparation is considered one of the limiting steps in microbial metabolome analysis. Eukaryotes and prokaryotes behave very differently during the several steps of classical sample preparation methods for analysis of metabolites. Even within the eukaryote kingdom there is a vast diversity...

  18. 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

  19. Sample collection and sample analysis plan in support of the 105-C/190-C concrete and soil sampling activities

    International Nuclear Information System (INIS)

    Marske, S.G.

    1996-07-01

    This sampling and analysis plan describes the sample collection and sample analysis in support of the 105-C water tunnels and 190-C main pumphouse concrete and soil sampling activities. These analytical data will be used to identify the radiological contamination and presence of hazardous materials to support the decontamination and disposal activities

  20. Research on self-absorption corrections for laboratory γ spectral analysis of soil samples

    International Nuclear Information System (INIS)

    Tian Zining; Jia Mingyan; Li Huibin; Cheng Ziwei; Ju Lingjun; Shen Maoquan; Yang Xiaoyan; Yan Ling; Fen Tiancheng

    2010-01-01

    Based on the calibration results of the point sources,dimensions of HPGe crystal were characterized.Linear attenuation coefficients and detection efficiencies of all kinds of samples were calculated,and the function F(μ) of φ75 mm x 25 mm sample was established. Standard surface source was used to simulate the source of different heights in the soil sample. And the function ε(h) which reflect the relationship between detection efficiencies and heights of the surface sources was determined. The detection efficiency of calibration source can be obtained by integration, F(μ) functions of soil samples established is consistent with the result of MCNP calculation code. Several φ75 mm x 25 mm soil samples were measured by the HPGe spectrometer,and the function F(μ) was used to correct the self absorption. F(μ) functions of soil samples of various dimensions can be calculated by MCNP calculation code established, and self absorption correction can be done. To verify the efficiency of calculation results, φ75 mm x 75 mm soil samples were measured. Several φ75 mm x 25 mm soil samples from aerosphere nuclear testing field was measured by the HPGe spectrometer,and the function F(μ) was used to correct the self absorption. The function F(m) was established, and the technical method which is used to correct the soil samples of unknown area is also given. The correction method of surface source greatly improves the gamma spectrum's metrical accuracy, and it will be widely applied to environmental radioactive investigation. (authors)

  1. Soil sample collection and analysis for the Fugitive Dust Characterization Study

    Science.gov (United States)

    Ashbaugh, Lowell L.; Carvacho, Omar F.; Brown, Michael S.; Chow, Judith C.; Watson, John G.; Magliano, Karen C.

    A unique set of soil samples was collected as part of the Fugitive Dust Characterization Study. The study was carried out to establish whether or not source profiles could be constructed using novel analytical methods that could distinguish soil dust sources from each other. The soil sources sampled included fields planted in cotton, almond, tomato, grape, and safflower, dairy and feedlot facilities, paved and unpaved roads (both urban and rural), an agricultural staging area, disturbed land with salt buildup, and construction areas where the topsoil had been removed. The samples were collected using a systematic procedure designed to reduce sampling bias, and were stored frozen to preserve possible organic signatures. For this paper the samples were characterized by particle size (percent sand, silt, and clay), dry silt content (used in EPA-recommended fugitive dust emission factors), carbon and nitrogen content, and potential to emit both PM 10 and PM 2.5. These are not the "novel analytical methods" referred to above; rather, it was the basic characterization of the samples to use in comparing analytical methods by other scientists contracted to the California Air Resources Board. The purpose of this paper is to document the methods used to collect the samples, the collection locations, the analysis of soil type and potential to emit PM 10, and the sample variability, both within field and between fields of the same crop type.

  2. Comparison of in situ gamma soil analysis and soil sampling data for mapping 241Am and 239Pu soil concentrations at the Nevada Test Site

    International Nuclear Information System (INIS)

    Kirby, J.A.; Anspaugh, L.R.; Phelps, P.L.; Huckabay, G.W.; Markwell, F.; Barnes, M.

    1976-01-01

    Soil sampling and in situ 241 Am-gamma counting with an array of four high purity, planar, Ge detectors are compared as means of determining soil concentration contours of plutonium and their associated uncertainties. Results of this survey, which covered an area of approximately 300,000 m 2 , indicate that with one-third the number of sampling locations, the in situ gamma survey provided soil concentration contours with confidence intervals that were about one-third as wide as those obtained with soil sampling. The methods of the survey are described and a discussion of advantages and limitations of both methods is given

  3. Comparison of in situ gamma soil analysis and soil sampling data for mapping 241Am and 239Pu soil concentrations at the Nevada Test Site

    International Nuclear Information System (INIS)

    Kirby, J.A.; Anspaugh, L.R.; Phelps, P.L.; Huckabay, G.W.; Markwell, F.R.; Barnes, M.G.

    1977-01-01

    Soil sampling and in situ 241 Am-gamma counting with an array of four high-purity, planar, Ge detectors are compared as means of determining soil concentration contours of plutonium and their associated uncertainties. Results of this survey, which covered an area of approximately 300,000 m 2 , indicate that with one-third the number of sampling locations, the in situ gamma survey provided soil concentration contours with confidence intervals that were about one-third as wide as those obtained with soil sampling. The methods of the survey are described and a discussion of advantages and limitations of both methods is given

  4. Fluidics platform and method for sample preparation and analysis

    Science.gov (United States)

    Benner, W. Henry; Dzenitis, John M.; Bennet, William J.; Baker, Brian R.

    2014-08-19

    Herein provided are fluidics platform and method for sample preparation and analysis. The fluidics platform is capable of analyzing DNA from blood samples using amplification assays such as polymerase-chain-reaction assays and loop-mediated-isothermal-amplification assays. The fluidics platform can also be used for other types of assays and analyzes. In some embodiments, a sample in a sealed tube can be inserted directly. The following isolation, detection, and analyzes can be performed without a user's intervention. The disclosed platform may also comprises a sample preparation system with a magnetic actuator, a heater, and an air-drying mechanism, and fluid manipulation processes for extraction, washing, elution, assay assembly, assay detection, and cleaning after reactions and between samples.

  5. The feasible research with measuring radon for taking the soils sample

    International Nuclear Information System (INIS)

    Zeng Bing, Ge Liangquan; Liu Hefan; Li Yeqiang; Zhang Jinzhao; Song Xiao'an

    2010-01-01

    It explains the mechanism of the separation of soil's radon. Through the designed experiment, it confirms the feasibility of measuring radon for taking the soil's sample. It determines the content of the radon and its sub field with indoor and outside through ways of the activated charcoal adsorption, the initiative suction and the diameter mark etching, also the 226 Ra. The paper indicates: it is feasible with measuring radon for taking the soil's sample, and the stability of data is that indoor data are better than outside's. The temperature, the humidity, the rainfall amount, the intensity and so on are the serious influence of the data. If you want to take a soil's sample, you must avoid the rain as far as possible, and avoid the fault zone, the belt of folded strata and complex geologic structure region, and so on. (authors)

  6. Occurrence and species distribution of pathogenic Mucorales in unselected soil samples from France.

    Science.gov (United States)

    Mousavi, B; Costa, J M; Arné, P; Guillot, J; Chermette, R; Botterel, F; Dannaoui, E

    2018-04-01

    Mucormycosis is a life-threatening invasive fungal disease that affects a variety of patient groups. Although Mucorales are mostly opportunistic pathogens originating from soil or decaying vegetation, there are currently few data on prevalence of this group of fungi in the environment. The aim of the present study was to assess the prevalence and diversity of species of Mucorales from soil samples collected in France. Two grams of soil were homogenized in sterile saline and plated on Sabouraud dextrose agar and RPMI agar supplemented with itraconazole or voriconazole. Both media contained chloramphenicol and gentamicin. The plates were incubated at 35 ± 2 °C and checked daily for fungal growth for a maximum of 7 d. Mucorales were subcultured for purity. Each isolate was identified phenotypically and molecular identification was performed by ITS sequencing. A total of 170 soil samples were analyzed. Forty-one isolates of Mucorales were retrieved from 38 culture-positive samples. Among the recovered isolates, 27 Rhizopus arrhizus, 11 Mucor circinelloides, one Lichtheimia corymbifera, one Rhizopus microsporus and one Cunninghamella bertholletiae were found. Positive soil samples came from cultivated fields but also from other types of soil such as flower beds. Mucorales were retrieved from samples obtained in different geographical regions of France. Voriconazole-containing medium improved the recovery of Mucorales compared with other media. The present study showed that pathogenic Mucorales are frequently recovered from soil samples in France. Species diversity should be further analyzed on a larger number of soil samples from different geographic areas in France and in other countries.

  7. Study on natural radioactive elements in soil and rock samples around Mandya district, India

    International Nuclear Information System (INIS)

    Shivakumara, B.C.; Paramesh, L.; Shashikumar, T.S.; Chandrashekara, M.S.

    2012-01-01

    The soil is a complex mixture of different compounds and rocks. In the natural environment, it is an important source of exposure to radiation due to naturally occurring, gamma emitting radionuclides which include 226 Ra, 232 Th and 40 K present in the soil. The study of distribution of these radionuclides in soil and rock is of great importance for radiation protection and measurements. The activity concentrations of 226 Ra, 232 Th, and 40 K in soil and rock samples collected in Mandya District, Karnataka state, India have been measured by gamma ray spectrometry. The average activity concentrations of 226 Ra, 232 Th, and 40 K (Bq/kg) are found to be 40.2, 62.3, and 317.5 Bq/kg, respectively, in soil samples and 30.5, 34.4, and 700.2 Bq/kg, respectively, in rock samples. The concentrations of radionuclides in soil samples are found to higher than in rock samples. The concentrations of radionuclides in soil and rock samples in the study area are slightly higher than Indian average and world average values. (author)

  8. SOIL FERTILITY EVALUATION FOR FERTILISER RECOMMENDATION USING HYPERION DATA

    Directory of Open Access Journals (Sweden)

    Ranendu Ghosh

    2015-12-01

    Full Text Available Soil fertility characterised by nitrogen, phosphorus, potassium, calcium, magnesium and sulphur is traditionally measured from soil samples collected from the field. The process is very cumbersome and time intensive. Hyperspectral data available from Hyperion payload of EO 1 was used for facilitating preparation of soil fertility map of Udaipur district of Rajasthan state, India. Hyperion data was pre-processed for band and area sub setting, atmospheric correction and reflectance data preparation. Spectral analysis in the form of SFF and PPI were carried out for selecting the ground truth sites for soil sample collection. Soil samples collected from forty one sites were analysed for analysis of nutrient composition. Generation of correlogram followed by multiple regressions was done for identifying the most important bands and spectral parameters that can be used for nutrient map generation.

  9. Inter comparison of 90Sr and 137Cs contents in biologic samples and natural U in soil samples

    International Nuclear Information System (INIS)

    Liu Jianfen; Zeng Guangjian; Lu Xuequan

    2001-01-01

    The results of the 90 Sr and 137 Cs contents in biologic samples and the natural U in soil samples obtained in a joint effort by fourteen environmental radiation laboratories in the Chinese environmental protection system were analyzed and compared. Two kinds of biologic samples and one kind of soil samples were used for inter comparison. Of which, one kind of biologic samples (biologic powder samples) and the soil samples came from the IAEA samples were environmental and the reference values were known. The another kind of biologic samples were environmental tea-leaf that were taken from a tea garden near Hangzhou. The mean values obtained by all the joined laboratories was used as the reference. The inter comparison results were expressed in terms of the deviation from the reference value. It was found that the deviation of the 90 Sr and 137 Cs contents of biologic powder samples ranged from -15.4% to 26.5% and -15.0% to 0.4%, respectively. The deviation of the natural U content ranged from -25.5% to 7.3% for the soil samples. For the tea-leaf, the 90 Sr deviation was -22.7% to 19.1%, and the 137 Cs data had a relative large scatter with a ratio of the maximum and the minimum values being about 7. It was pointed out that the analysis results offered by different laboratories might have involved system errors

  10. Amostragem para avaliação da fertilidade do solo em função do instrumento de coleta das amostras e de tipos de preparo do solo Sampling for soil fertility evaluation as influenced by sampling tool and soil tillage

    Directory of Open Access Journals (Sweden)

    Fábio Henrique Tavares de Oliveira

    2007-10-01

    experiment of soil tillage type, planted with corn. In a 81 m² plot under NT 48 simple soil samples were collected, 24 with a cutting shovel (perpendicularly to the furrow and in-between two furrows and 24 with auger hole, in controlled sampling (four samples collected in the planting furrow, 8 to 10 cm away from the furrow and 12 in-between the furrows, close to the points of sampling with the cutting shovel. The procedure was repeated in a second plot under CT. Composite samples of different numbers of simple samples (4, 8, 12, 16 and 24 simple samples/composite samples, with three repetitions were prepared for each combination of soil tillage type - collection tool. The pH and the contents of P, K+ Ca2+, Mg2+ and organic matter (OM were determined in all simple and composite samples. The variability of the evaluated characteristics in samples collected with auger hole was greater than with the cutting shovel, independent of the soil tillage type. For both collection tools, the decreasing order of variability was: P > Mg2+ > K+ > Ca2+ > OM > pH. The medium fertility of a field under NT or under CT after the crop and before subsequent soil preparation can be evaluated with the auger hole, substituting the cutting shovel, if the composite sample consists of 17 % of simple samples collected in the planting furrow, 33 % at a distance of 10 cm from the furrow and 50 % in the middle between the furrows. The mean fertility of a field under NT or CT after the crop and before the subsequent soil preparation, evaluated by the chemical analysis of the composite sample, is similar to that evaluated by the arithmetic average of the chemical analyses of the simple samples collected with cutting shovel or with auger hole in a controlled manner, as used here. In general, a minimum of eight simple samples collected with cutting shovel or hand auger would be enough to form a representative composite sample for evaluation of the soil fertility of a unit of seemingly homogeneous sampling

  11. Combining Electrochemical Sensors with Miniaturized Sample Preparation for Rapid Detection in Clinical Samples

    Science.gov (United States)

    Bunyakul, Natinan; Baeumner, Antje J.

    2015-01-01

    Clinical analyses benefit world-wide from rapid and reliable diagnostics tests. New tests are sought with greatest demand not only for new analytes, but also to reduce costs, complexity and lengthy analysis times of current techniques. Among the myriad of possibilities available today to develop new test systems, amperometric biosensors are prominent players—best represented by the ubiquitous amperometric-based glucose sensors. Electrochemical approaches in general require little and often enough only simple hardware components, are rugged and yet provide low limits of detection. They thus offer many of the desirable attributes for point-of-care/point-of-need tests. This review focuses on investigating the important integration of sample preparation with (primarily electrochemical) biosensors. Sample clean up requirements, miniaturized sample preparation strategies, and their potential integration with sensors will be discussed, focusing on clinical sample analyses. PMID:25558994

  12. 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.

  13. Measurements of Plutonium and Americium in Soil Samples from Project 57 using the Suspended Soil Particle Sizing System (SSPSS)

    International Nuclear Information System (INIS)

    John L. Bowen; Rowena Gonzalez; David S. Shafer

    2001-01-01

    As part of the preliminary site characterization conducted for Project 57, soils samples were collected for separation into several size-fractions using the Suspended Soil Particle Sizing System (SSPSS). Soil samples were collected specifically for separation by the SSPSS at three general locations in the deposited Project 57 plume, the projected radioactivity of which ranged from 100 to 600 pCi/g. The primary purpose in focusing on samples with this level of activity is that it would represent anticipated residual soil contamination levels at the site after corrective actions are completed. Consequently, the results of the SSPSS analysis can contribute to dose calculation and corrective action-level determinations for future land-use scenarios at the site

  14. Uranium content and dose assessment for sediment and soil samples from the estuarine system of Santos and Sao Vicente, SP (Brazil)

    International Nuclear Information System (INIS)

    Geraldo, L. P.; Serafim, R. A. M.; Correa, B. A. M.; Yamazaki, I. M.; Primi, M. C.

    2010-01-01

    In this work, the uranium (U) content in sediment and soil samples collected near the Santos and Sao Vicente estuaries was determined using the fission track registration technique (SSNTD). The sediment and soil samples after oven-dried and pulverised were prepared in the solution form. About 10 ml of this solution was deposited on a plastic detector and irradiated at the IPEN-IEA-R1 (3.5 MW) nuclear reactor. After the irradiation and chemical etching of the plastic foils, the fission tracks were counted with a system consisting of an optical microscope together with a video camera and a PC. The U content in the analysed samples ranged from 3.12±0.55 to 18.3±1.2 ppm for sediments and from 3.21±0.63 to 11.5±1.1 ppm for soils or in terms of 238 U equivalent activity from 38.5±6.8 to 226±15 and 39.6±7.8 to 142±14 Bq kg -1 for sediments and soils, respectively. These results were compared with other values reported in the literature for sediments and soils collected in environments similar to the ones studied in this work. Most of the values obtained in this work are higher than the world mean and are in reasonable agreement with results found by other authors for sediments and soils from regions considered as polluted or with a high level of radioactivity. (authors)

  15. Quantitating morphological changes in biological samples during scanning electron microscopy sample preparation with correlative super-resolution microscopy.

    Science.gov (United States)

    Zhang, Ying; Huang, Tao; Jorgens, Danielle M; Nickerson, Andrew; Lin, Li-Jung; Pelz, Joshua; Gray, Joe W; López, Claudia S; Nan, Xiaolin

    2017-01-01

    Sample preparation is critical to biological electron microscopy (EM), and there have been continuous efforts on optimizing the procedures to best preserve structures of interest in the sample. However, a quantitative characterization of the morphological changes associated with each step in EM sample preparation is currently lacking. Using correlative EM and superresolution microscopy (SRM), we have examined the effects of different drying methods as well as osmium tetroxide (OsO4) post-fixation on cell morphology during scanning electron microscopy (SEM) sample preparation. Here, SRM images of the sample acquired under hydrated conditions were used as a baseline for evaluating morphological changes as the sample went through SEM sample processing. We found that both chemical drying and critical point drying lead to a mild cellular boundary retraction of ~60 nm. Post-fixation by OsO4 causes at least 40 nm additional boundary retraction. We also found that coating coverslips with adhesion molecules such as fibronectin prior to cell plating helps reduce cell distortion from OsO4 post-fixation. These quantitative measurements offer useful information for identifying causes of cell distortions in SEM sample preparation and improving current procedures.

  16. Sample Preparation for Mass Spectrometry Imaging of Plant Tissues: A Review

    Science.gov (United States)

    Dong, Yonghui; Li, Bin; Malitsky, Sergey; Rogachev, Ilana; Aharoni, Asaph; Kaftan, Filip; Svatoš, Aleš; Franceschi, Pietro

    2016-01-01

    Mass spectrometry imaging (MSI) is a mass spectrometry based molecular ion imaging technique. It provides the means for ascertaining the spatial distribution of a large variety of analytes directly on tissue sample surfaces without any labeling or staining agents. These advantages make it an attractive molecular histology tool in medical, pharmaceutical, and biological research. Likewise, MSI has started gaining popularity in plant sciences; yet, information regarding sample preparation methods for plant tissues is still limited. Sample preparation is a crucial step that is directly associated with the quality and authenticity of the imaging results, it therefore demands in-depth studies based on the characteristics of plant samples. In this review, a sample preparation pipeline is discussed in detail and illustrated through selected practical examples. In particular, special concerns regarding sample preparation for plant imaging are critically evaluated. Finally, the applications of MSI techniques in plants are reviewed according to different classes of plant metabolites. PMID:26904042

  17. Sample Preparation for Mass Spectrometry Imaging of Plant Tissues: A Review.

    Science.gov (United States)

    Dong, Yonghui; Li, Bin; Malitsky, Sergey; Rogachev, Ilana; Aharoni, Asaph; Kaftan, Filip; Svatoš, Aleš; Franceschi, Pietro

    2016-01-01

    Mass spectrometry imaging (MSI) is a mass spectrometry based molecular ion imaging technique. It provides the means for ascertaining the spatial distribution of a large variety of analytes directly on tissue sample surfaces without any labeling or staining agents. These advantages make it an attractive molecular histology tool in medical, pharmaceutical, and biological research. Likewise, MSI has started gaining popularity in plant sciences; yet, information regarding sample preparation methods for plant tissues is still limited. Sample preparation is a crucial step that is directly associated with the quality and authenticity of the imaging results, it therefore demands in-depth studies based on the characteristics of plant samples. In this review, a sample preparation pipeline is discussed in detail and illustrated through selected practical examples. In particular, special concerns regarding sample preparation for plant imaging are critically evaluated. Finally, the applications of MSI techniques in plants are reviewed according to different classes of plant metabolites.

  18. 15N sample preparation for mass spectroscopy analysis

    International Nuclear Information System (INIS)

    Trivelin, P.C.O.; Salati, E.; Matsui, E.

    1973-01-01

    Technics for preparing 15 N samples to be analised is presented. Dumas method and oxidation by sodium hypobromite method are described in order to get the appropriate sample. Method to calculate 15 N ratio from mass spectrometry dates is also discussed [pt

  19. Preparation of archaeological samples for its dating by thermoluminescence

    International Nuclear Information System (INIS)

    Mejia F, D.

    2000-01-01

    The present work shows the results of the preparation of archaeological samples for their dating by thermoluminescence (Tl) using the Fine grain technique established by Zimmerman but with the varying of such preparation was realized in normal daylight conditions, only the taking of the Tl readings were realized in dark room and red light. In the chapter 1 basic concepts are described about: matter constitution, radioactivity, units and radiation magnitudes, and thermoluminescence. In the chapter 2 some theoretical aspects on dating are showed. It is described how realizing the samples collection, the fine grain method, the determination of the accumulated dose through the years or paleodoses (P=Q+I) by mean of the increasing to obtain the dose equivalent dose (Q) and the signal regeneration method to obtain the correction factor by supra linearity (1), the determination of the annual dose rate to apply the age equation and the evaluation of the age uncertainty with the error limits. The development of experimental part with samples from the archaeological site named Edzna in Campeche, Mexico is described in the chapter 3. The results are presented in the chapter 4. It was obtained an age for the sample named CH7 it was obtained an age of 389 ± years. In conclusion the preparation of the archaeological samples for their dating by Tl in the conditions before mentioned is reliable, but they must be realized more studies with samples of well known age, preparing them in normal daylight conditions and simultaneously in dark room with red light. In order to observe how respond the minerals present in the sample at different dose rapidity, the same samples must be radiated with radiation sources with different dose rate. (Author)

  20. Optimization of sampling for the determination of the mean Radium-226 concentration in surface soil

    International Nuclear Information System (INIS)

    Williams, L.R.; Leggett, R.W.; Espegren, M.L.; Little, C.A.

    1987-08-01

    This report describes a field experiment that identifies an optimal method for determination of compliance with the US Environmental Protection Agency's Ra-226 guidelines for soil. The primary goals were to establish practical levels of accuracy and precision in estimating the mean Ra-226 concentration of surface soil in a small contaminated region; to obtain empirical information on composite vs. individual soil sampling and on random vs. uniformly spaced sampling; and to examine the practicality of using gamma measurements in predicting the average surface radium concentration and in estimating the number of soil samples required to obtain a given level of accuracy and precision. Numerous soil samples were collected on each six sites known to be contaminated with uranium mill tailings. Three types of samples were collected on each site: 10-composite samples, 20-composite samples, and individual or post hole samples; 10-composite sampling is the method of choice because it yields a given level of accuracy and precision for the least cost. Gamma measurements can be used to reduce surface soil sampling on some sites. 2 refs., 5 figs., 7 tabs

  1. Comparison of soil solution sampling techniques to assess metal fluxes from contaminated soil to groundwater.

    Science.gov (United States)

    Coutelot, F; Sappin-Didier, V; Keller, C; Atteia, O

    2014-12-01

    The unsaturated zone plays a major role in elemental fluxes in terrestrial ecosystems. A representative chemical analysis of soil pore water is required for the interpretation of soil chemical phenomena and particularly to assess Trace Elements (TEs) mobility. This requires an optimal sampling system to avoid modification of the extracted soil water chemistry and allow for an accurate estimation of solute fluxes. In this paper, the chemical composition of soil solutions sampled by Rhizon® samplers connected to a standard syringe was compared to two other types of suction probes (Rhizon® + vacuum tube and Rhizon® + diverted flow system). We investigated the effects of different vacuum application procedures on concentrations of spiked elements (Cr, As, Zn) mixed as powder into the first 20 cm of 100-cm columns and non-spiked elements (Ca, Na, Mg) concentrations in two types of columns (SiO2 sand and a mixture of kaolinite + SiO2 sand substrates). Rhizon® was installed at different depths. The metals concentrations showed that (i) in sand, peak concentrations cannot be correctly sampled, thus the flux cannot be estimated, and the errors can easily reach a factor 2; (ii) in sand + clay columns, peak concentrations were larger, indicating that they could be sampled but, due to sorption on clay, it was not possible to compare fluxes at different depths. The different samplers tested were not able to reflect the elemental flux to groundwater and, although the Rhizon® + syringe device was more accurate, the best solution remains to be the use of a lysimeter, whose bottom is kept continuously at a suction close to the one existing in the soil.

  2. Chemical and geotechnical analyses of soil samples from Olkiluoto for studies on sorption in soils

    International Nuclear Information System (INIS)

    Lusa, M.; Aemmaelae, K.; Hakanen, M.; Lehto, J.; Lahdenperae, A.-M.

    2009-05-01

    The safety assessment of disposal of spent nuclear fuel will include an estimate on the behavior of nuclear waste nuclides in the biosphere. As a part of this estimate also the transfer of nuclear waste nuclides in the soil and sediments is to be considered. In this study soil samples were collected from three excavator pits in Olkiluoto and the geotechnical and chemical characteristics of the samples were determined. In later stage these results will be used in sorption tests. Aim of these tests is to determine the Kd-values for Cs, Tc and I and later for Mo, Nb and Cl. Results of these sorption tests will be reported later. The geotechnical characteristics studied included dry weight and organic matter content as well as grain size distribution and mineralogy analyses. Selective extractions were carried out to study the sorption of cations into different mineral types. The extractions included five steps in which the cations bound to exchangeable, carbonate, oxides of Fe and Mn, organic matter and residual fractions were determined. For all fractions ICPMS analyses were carried out. In these analyses Li, Na, Mg, K, Ca, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Sr, Mo, Cd, Cs and Pb were determined. In addition six profiles were taken from the surroundings of two excavator pits for the 137 Cs determination. Besides the samples taken for the characterization of soil, supplement samples were taken from the same layers for the separation of soil water. From the soil water pH, DOC, anions (F, Cl, NO 3 , SO 4 ) and cations (Na, Mg, K, Ca, Al, Cr, Mn, Fe, Ni, Cu, Zn, As, S, Cd, Cs, Pb, U) were determined. (orig.)

  3. Effects of soil water saturation on sampling equilibrium and kinetics of selected polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Kim, Pil-Gon; Roh, Ji-Yeon; Hong, Yongseok; Kwon, Jung-Hwan

    2017-10-01

    Passive sampling can be applied for measuring the freely dissolved concentration of hydrophobic organic chemicals (HOCs) in soil pore water. When using passive samplers under field conditions, however, there are factors that might affect passive sampling equilibrium and kinetics, such as soil water saturation. To determine the effects of soil water saturation on passive sampling, the equilibrium and kinetics of passive sampling were evaluated by observing changes in the distribution coefficient between sampler and soil (K sampler/soil ) and the uptake rate constant (k u ) at various soil water saturations. Polydimethylsiloxane (PDMS) passive samplers were deployed into artificial soils spiked with seven selected polycyclic aromatic hydrocarbons (PAHs). In dry soil (0% water saturation), both K sampler/soil and k u values were much lower than those in wet soils likely due to the contribution of adsorption of PAHs onto soil mineral surfaces and the conformational changes in soil organic matter. For high molecular weight PAHs (chrysene, benzo[a]pyrene, and dibenzo[a,h]anthracene), both K sampler/soil and k u values increased with increasing soil water saturation, whereas they decreased with increasing soil water saturation for low molecular weight PAHs (phenanthrene, anthracene, fluoranthene, and pyrene). Changes in the sorption capacity of soil organic matter with soil water content would be the main cause of the changes in passive sampling equilibrium. Henry's law constant could explain the different behaviors in uptake kinetics of the selected PAHs. The results of this study would be helpful when passive samplers are deployed under various soil water saturations. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Forensic Comparison of Soil Samples Using Nondestructive Elemental Analysis.

    Science.gov (United States)

    Uitdehaag, Stefan; Wiarda, Wim; Donders, Timme; Kuiper, Irene

    2017-07-01

    Soil can play an important role in forensic cases in linking suspects or objects to a crime scene by comparing samples from the crime scene with samples derived from items. This study uses an adapted ED-XRF analysis (sieving instead of grinding to prevent destruction of microfossils) to produce elemental composition data of 20 elements. Different data processing techniques and statistical distances were evaluated using data from 50 samples and the log-LR cost (C llr ). The best performing combination, Canberra distance, relative data, and square root values, is used to construct a discriminative model. Examples of the spatial resolution of the method in crime scenes are shown for three locations, and sampling strategy is discussed. Twelve test cases were analyzed, and results showed that the method is applicable. The study shows how the combination of an analysis technique, a database, and a discriminative model can be used to compare multiple soil samples quickly. © 2016 American Academy of Forensic Sciences.

  5. Pecan growth under different soil preparation and hole sizes: coleopterans as bioindicators

    Directory of Open Access Journals (Sweden)

    Jardel Boscardin

    2017-12-01

    Full Text Available The study aimed to evaluate the effects of different soil preparation and hole sizes in an orchard of Carya illinoinensis pecan (Wangenh. K. Koch (Juglandaceae by the Order Coleoptera fauna. A pecan orchard was established in spacing 7 m x 7 m, in Santa Maria, Rio Grande do Sul State, Brazil in randomized block design, with five blocks and four treatments, using: small pit 20 m x 60 cm (Cp; more harrowing subsoiler and small pit (Scp; rotary hoe and small pit (Ecp; and large pit 40 m x 60 cm (Cg. From March 2014 to November 2015, eight samples were taken from Coleoptera fauna, one per season, with four pitfall traps distributed in each treatment and the surrounding area, totaling 100 samples per collection. The Ecp treatment had the lowest diversity values and evenness for Coleoptera fauna, while the Cp and Cg treatments presented the highest indices. The species Diloboderus abderus (Sturm was as very common. It was concluded that Cg treatment does not interfere with coleopteran and promotes the highest growth in diameter of pecan plants.

  6. Sample preparation and EFTEM of Meat Samples for Nanoparticle Analysis in Food

    International Nuclear Information System (INIS)

    Lari, L; Dudkiewicz, A

    2014-01-01

    Nanoparticles are used in industry for personal care products and the preparation of food. In the latter application, their functions include the prevention of microbes' growth, increase of the foods nutritional value and sensory quality. EU regulations require a risk assessment of the nanoparticles used in foods and food contact materials before the products can reach the market. However, availability of validated analytical methodologies for detection and characterisation of the nanoparticles in food hampers appropriate risk assessment. As part of a research on the evaluation of the methods for screening and quantification of Ag nanoparticles in meat we have tested a new TEM sample preparation alternative to resin embedding and cryo-sectioning. Energy filtered TEM analysis was applied to evaluate thickness and the uniformity of thin meat layers acquired at increasing input of the sample demonstrating that the protocols used ensured good stability under the electron beam, reliable sample concentration and reproducibility

  7. Sample preparation and EFTEM of Meat Samples for Nanoparticle Analysis in Food

    Science.gov (United States)

    Lari, L.; Dudkiewicz, A.

    2014-06-01

    Nanoparticles are used in industry for personal care products and the preparation of food. In the latter application, their functions include the prevention of microbes' growth, increase of the foods nutritional value and sensory quality. EU regulations require a risk assessment of the nanoparticles used in foods and food contact materials before the products can reach the market. However, availability of validated analytical methodologies for detection and characterisation of the nanoparticles in food hampers appropriate risk assessment. As part of a research on the evaluation of the methods for screening and quantification of Ag nanoparticles in meat we have tested a new TEM sample preparation alternative to resin embedding and cryo-sectioning. Energy filtered TEM analysis was applied to evaluate thickness and the uniformity of thin meat layers acquired at increasing input of the sample demonstrating that the protocols used ensured good stability under the electron beam, reliable sample concentration and reproducibility.

  8. Final LDRD report : development of sample preparation methods for ChIPMA-based imaging mass spectrometry of tissue samples.

    Energy Technology Data Exchange (ETDEWEB)

    Maharrey, Sean P.; Highley, Aaron M.; Behrens, Richard, Jr.; Wiese-Smith, Deneille

    2007-12-01

    The objective of this short-term LDRD project was to acquire the tools needed to use our chemical imaging precision mass analyzer (ChIPMA) instrument to analyze tissue samples. This effort was an outgrowth of discussions with oncologists on the need to find the cellular origin of signals in mass spectra of serum samples, which provide biomarkers for ovarian cancer. The ultimate goal would be to collect chemical images of biopsy samples allowing the chemical images of diseased and nondiseased sections of a sample to be compared. The equipment needed to prepare tissue samples have been acquired and built. This equipment includes an cyro-ultramicrotome for preparing thin sections of samples and a coating unit. The coating unit uses an electrospray system to deposit small droplets of a UV-photo absorbing compound on the surface of the tissue samples. Both units are operational. The tissue sample must be coated with the organic compound to enable matrix assisted laser desorption/ionization (MALDI) and matrix enhanced secondary ion mass spectrometry (ME-SIMS) measurements with the ChIPMA instrument Initial plans to test the sample preparation using human tissue samples required development of administrative procedures beyond the scope of this LDRD. Hence, it was decided to make two types of measurements: (1) Testing the spatial resolution of ME-SIMS by preparing a substrate coated with a mixture of an organic matrix and a bio standard and etching a defined pattern in the coating using a liquid metal ion beam, and (2) preparing and imaging C. elegans worms. Difficulties arose in sectioning the C. elegans for analysis and funds and time to overcome these difficulties were not available in this project. The facilities are now available for preparing biological samples for analysis with the ChIPMA instrument. Some further investment of time and resources in sample preparation should make this a useful tool for chemical imaging applications.

  9. Analysis on soil compressibility changes of samples stabilized with lime

    Directory of Open Access Journals (Sweden)

    Elena-Andreea CALARASU

    2016-12-01

    Full Text Available In order to manage and control the stability of buildings located on difficult foundation soils, several techniques of soil stabilization were developed and applied worldwide. Taking into account the major significance of soil compressibility on construction durability and safety, the soil stabilization with a binder like lime is considered one of the most used and traditional methods. The present paper aims to assess the effect of lime content on soil geotechnical parameters, especially on compressibility ones, based on laboratory experimental tests, for several soil categories in admixture with different lime dosages. The results of this study indicate a significant improvement of stabilized soil parameters, such as compressibility and plasticity, in comparison with natural samples. The effect of lime stabilization is related to an increase of soil structure stability by increasing the bearing capacity.

  10. The Impact of Soil Sampling Errors on Variable Rate Fertilization

    Energy Technology Data Exchange (ETDEWEB)

    R. L. Hoskinson; R C. Rope; L G. Blackwood; R D. Lee; R K. Fink

    2004-07-01

    Variable rate fertilization of an agricultural field is done taking into account spatial variability in the soil’s characteristics. Most often, spatial variability in the soil’s fertility is the primary characteristic used to determine the differences in fertilizers applied from one point to the next. For several years the Idaho National Engineering and Environmental Laboratory (INEEL) has been developing a Decision Support System for Agriculture (DSS4Ag) to determine the economically optimum recipe of various fertilizers to apply at each site in a field, based on existing soil fertility at the site, predicted yield of the crop that would result (and a predicted harvest-time market price), and the current costs and compositions of the fertilizers to be applied. Typically, soil is sampled at selected points within a field, the soil samples are analyzed in a lab, and the lab-measured soil fertility of the point samples is used for spatial interpolation, in some statistical manner, to determine the soil fertility at all other points in the field. Then a decision tool determines the fertilizers to apply at each point. Our research was conducted to measure the impact on the variable rate fertilization recipe caused by variability in the measurement of the soil’s fertility at the sampling points. The variability could be laboratory analytical errors or errors from variation in the sample collection method. The results show that for many of the fertility parameters, laboratory measurement error variance exceeds the estimated variability of the fertility measure across grid locations. These errors resulted in DSS4Ag fertilizer recipe recommended application rates that differed by up to 138 pounds of urea per acre, with half the field differing by more than 57 pounds of urea per acre. For potash the difference in application rate was up to 895 pounds per acre and over half the field differed by more than 242 pounds of potash per acre. Urea and potash differences

  11. Sample preparation composite and replicate strategy for assay of solid oral drug products.

    Science.gov (United States)

    Harrington, Brent; Nickerson, Beverly; Guo, Michele Xuemei; Barber, Marc; Giamalva, David; Lee, Carlos; Scrivens, Garry

    2014-12-16

    In pharmaceutical analysis, the results of drug product assay testing are used to make decisions regarding the quality, efficacy, and stability of the drug product. In order to make sound risk-based decisions concerning drug product potency, an understanding of the uncertainty of the reportable assay value is required. Utilizing the most restrictive criteria in current regulatory documentation, a maximum variability attributed to method repeatability is defined for a drug product potency assay. A sampling strategy that reduces the repeatability component of the assay variability below this predefined maximum is demonstrated. The sampling strategy consists of determining the number of dosage units (k) to be prepared in a composite sample of which there may be a number of equivalent replicate (r) sample preparations. The variability, as measured by the standard error (SE), of a potency assay consists of several sources such as sample preparation and dosage unit variability. A sampling scheme that increases the number of sample preparations (r) and/or number of dosage units (k) per sample preparation will reduce the assay variability and thus decrease the uncertainty around decisions made concerning the potency of the drug product. A maximum allowable repeatability component of the standard error (SE) for the potency assay is derived using material in current regulatory documents. A table of solutions for the number of dosage units per sample preparation (r) and number of replicate sample preparations (k) is presented for any ratio of sample preparation and dosage unit variability.

  12. PIXE Analysis of Aerosol and Soil Samples Collected in the Adirondack Mountains

    Science.gov (United States)

    Yoskowitz, Joshua; Ali, Salina; Nadareski, Benjamin; Labrake, Scott; Vineyard, Michael

    2014-09-01

    We have performed an elemental analysis of aerosol and soil samples collected at Piseco Lake in Upstate New York using proton induced X-ray emission spectroscopy (PIXE). This work is part of a systematic study of airborne pollution in the Adirondack Mountains. Of particular interest is the sulfur content that can contribute to acid rain, a well-documented problem in the Adirondacks. We used a nine-stage cascade impactor to collect the aerosol samples near Piseco Lake and distribute the particulate matter onto Kapton foils by particle size. The soil samples were also collected at Piseco Lake and pressed into cylindrical pellets for experimentation. PIXE analysis of the aerosol and soil samples were performed with 2.2-MeV proton beams from the 1.1-MV Pelletron accelerator in the Union College Ion-Beam Analysis Laboratory. There are higher concentrations of sulfur at smaller particle sizes (0.25-1 μm), suggesting that it could be suspended in the air for days and originate from sources very far away. Other elements with significant concentrations peak at larger particle sizes (1-4 μm) and are found in the soil samples, suggesting that these elements could originate in the soil. The PIXE analysis will be described and the resulting data will be presented.

  13. Effect of the grain size of the soil on the measured activity and variation in activity in surface and subsurface soil samples

    International Nuclear Information System (INIS)

    Sulaiti, H.A.; Rega, P.H.; Bradley, D.; Dahan, N.A.; Mugren, K.A.; Dosari, M.A.

    2014-01-01

    Correlation between grain size and activity concentrations of soils and concentrations of various radionuclides in surface and subsurface soils has been measured for samples taken in the State of Qatar by gamma-spectroscopy using a high purity germanium detector. From the obtained gamma-ray spectra, the activity concentrations of the 238U (226Ra) and /sup 232/ Th (/sup 228/ Ac) natural decay series, the long-lived naturally occurring radionuclide 40 K and the fission product radionuclide 137CS have been determined. Gamma dose rate, radium equivalent, radiation hazard index and annual effective dose rates have also been estimated from these data. In order to observe the effect of grain size on the radioactivity of soil, three grain sizes were used i.e., smaller than 0.5 mm; smaller than 1 mm and greater than 0.5 mm; and smaller than 2 mm and greater than 1 mm. The weighted activity concentrations of the 238U series nuclides in 0.5-2 mm grain size of sample numbers was found to vary from 2.5:f:0.2 to 28.5+-0.5 Bq/kg, whereas, the weighted activity concentration of 4 degree K varied from 21+-4 to 188+-10 Bq/kg. The weighted activity concentrations of 238U series and 4 degree K have been found to be higher in the finest grain size. However, for the 232Th series, the activity concentrations in the 1-2 mm grain size of one sample were found to be higher than in the 0.5-1 mm grain size. In the study of surface and subsurface soil samples, the activity concentration levels of 238 U series have been found to range from 15.9+-0.3 to 24.1+-0.9 Bq/kg, in the surface soil samples (0-5 cm) and 14.5+-0.3 to 23.6+-0.5 Bq/kg in the subsurface soil samples (5-25 cm). The activity concentrations of 232Th series have been found to lie in the range 5.7+-0.2 to 13.7+-0.5 Bq/kg, in the surface soil samples (0-5 cm)and 4.1+-0.2 to 15.6+-0.3 Bq/kg in the subsurface soil samples (5-25 cm). The activity concentrations of 4 degree K were in the range 150+-8 to 290+-17 Bq/kg, in the surface

  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. Analysis of PAH in soil samples

    International Nuclear Information System (INIS)

    Haeufel, J.; Weisweiler, W.

    1994-01-01

    The supercritical fluid extraction of polycyclic aromatic hydrocarbons (PAH) from soil samples is described. Carbon dioxide mixed with a small amount of methanol is used for solvent. The results are compared with those obtained by a classical extraction method (that means with the use of organic liquids). The extracted PAH from both procedures can be separated by HPLC and analyzed with UV- and fluorescence detection. (orig.) [de

  16. Kinetics of exchange of a tracer in soil and clay samples

    Energy Technology Data Exchange (ETDEWEB)

    Zanotti, J C; Facetti, J F [Asuncion Nacional Univ. (Paraguay). Inst. de Ciencias

    1971-01-01

    The kinetics of exchange of a Na tracer in soil and clay samples, provides with a reliable and convenient method for the determination of the different soil fraction ahd their CEC values, In addition, the analysis of the exchanges curves can be used for the identification of the clay present in the soil.

  17. Kinetics of exchange of a tracer in soil and clay samples

    International Nuclear Information System (INIS)

    Zanotti, J.C.; Facetti, J.F.

    1971-01-01

    The kinetics of exchange of a Na tracer in soil and clay samples, provides with a reliable and convenient method for the determination of the different soil fraction ahd their CEC values, In addition, the analysis of the exchanges curves can be used for the identification of the clay present in the soil

  18. Sample preparation of energy materials for X-ray nanotomography with micromanipulation.

    Science.gov (United States)

    Chen-Wiegart, Yu-chen Karen; Camino, Fernando E; Wang, Jun

    2014-06-06

    X-ray nanotomography presents an unprecedented opportunity to study energy storage/conversion materials at nanometer scales in three dimensions, with both elemental and chemical sensitivity. A critical step in obtaining high-quality X-ray nanotomography data is reliable sample preparation to ensure that the entire sample fits within the field of view of the X-ray microscope. Although focused-ion-beam lift-out has previously been used for large sample (few to tens of microns) preparation, a difficult undercut and lift-out procedure results in a time-consuming sample preparation process. Herein, we propose a much simpler and direct sample preparation method to resolve the issues that block the view of the sample base after milling and during the lift-out process. This method is applied on a solid-oxide fuel cell and a lithium-ion battery electrode, before numerous critical 3D morphological parameters are extracted, which are highly relevant to their electrochemical performance. A broad application of this method for microstructure study with X-ray nanotomography is discussed and presented. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Pore water sampling in acid sulfate soils: a new peeper method.

    Science.gov (United States)

    Johnston, Scott G; Burton, Edward D; Keene, Annabelle F; Bush, Richard T; Sullivan, Leigh A; Isaacson, Lloyd

    2009-01-01

    This study describes the design, deployment, and application of a modified equilibration dialysis device (peeper) optimized for sampling pore waters in acid sulfate soils (ASS). The modified design overcomes the limitations of traditional-style peepers, when sampling firm ASS materials over relatively large depth intervals. The new peeper device uses removable, individual cells of 25 mL volume housed in a 1.5 m long rigid, high-density polyethylene rod. The rigid housing structure allows the device to be inserted directly into relatively firm soils without requiring a supporting frame. The use of removable cells eliminates the need for a large glove-box after peeper retrieval, thus simplifying physical handling. Removable cells are easily maintained in an inert atmosphere during sample processing and the 25-mL sample volume is sufficient for undertaking multiple analyses. A field evaluation of equilibration times indicates that 32 to 38 d of deployment was necessary. Overall, the modified method is simple and effective and well suited to acquisition and processing of redox-sensitive pore water profiles>1 m deep in acid sulfate soil or any other firm wetland soils.

  20. Determination of technetium-99 in soil samples by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Muto, Toshio; Shimokawa, Toshinari

    1997-01-01

    A new powerful analytical technique viz. high performance liquid chromatography(HPLC) coupled to inductively coupled plasma mass spectrometry(HPLC/ICP-MS) has been applied to the determination of technetium-99( 99 Tc) in soils as a typical environmental sample. Technetium was enriched in a solution from incinerated soil samples by leaching in HNO 3 and passed through 'TEVA resin' column. The solution was injected into HPLC/ICP-MS system to eliminate the interfering elements (i.e. Ru and Mo) and to determine the 99 Tc concentration at the same time. The concentrations of 99 Tc in the incinerated soils were found to be 0.49Bq/kg(0.77ng/kg)-1.4Bq/kg(2.2ng/kg) with the determination limit of 0.02Bq/kg(0.03ng/kg(0.03ppt)). The results indicate the following findings; 1) the determination of 99 Tc by ICP-MS after strict elimination of the interfering elements by HPLC brings about the improvement in their reliability; 2) the detection limits identified are much lower compared with those by conventional ICP-MS methods because of the concentration of 99 Tc to smaller volume, which is due to only 100μl of samples could be measured by HPLC/ICP-MS system; 3) sample preparation could be simplified because of strict elimination of the interfering elements by HPLC. This research showed that HPLC/ICP-MS system is very effective to determine 99 Tc in environmental samples. (author)

  1. Sample preparation optimization in fecal metabolic profiling.

    Science.gov (United States)

    Deda, Olga; Chatziioannou, Anastasia Chrysovalantou; Fasoula, Stella; Palachanis, Dimitris; Raikos, Νicolaos; Theodoridis, Georgios A; Gika, Helen G

    2017-03-15

    Metabolomic analysis of feces can provide useful insight on the metabolic status, the health/disease state of the human/animal and the symbiosis with the gut microbiome. As a result, recently there is increased interest on the application of holistic analysis of feces for biomarker discovery. For metabolomics applications, the sample preparation process used prior to the analysis of fecal samples is of high importance, as it greatly affects the obtained metabolic profile, especially since feces, as matrix are diversifying in their physicochemical characteristics and molecular content. However there is still little information in the literature and lack of a universal approach on sample treatment for fecal metabolic profiling. The scope of the present work was to study the conditions for sample preparation of rat feces with the ultimate goal of the acquisition of comprehensive metabolic profiles either untargeted by NMR spectroscopy and GC-MS or targeted by HILIC-MS/MS. A fecal sample pooled from male and female Wistar rats was extracted under various conditions by modifying the pH value, the nature of the organic solvent and the sample weight to solvent volume ratio. It was found that the 1/2 (w f /v s ) ratio provided the highest number of metabolites under neutral and basic conditions in both untargeted profiling techniques. Concerning LC-MS profiles, neutral acetonitrile and propanol provided higher signals and wide metabolite coverage, though extraction efficiency is metabolite dependent. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Comparison of sample preparation procedures on metal(loid) fractionation patterns in lichens.

    Science.gov (United States)

    Kroukamp, E M; Godeto, T W; Forbes, P B C

    2017-08-13

    The effects of different sample preparation strategies and storage on metal(loid) fractionation trends in plant material is largely underresearched. In this study, a bulk sample of lichen Parmotrema austrosinense (Zahlbr.) Hale was analysed for its total extractable metal(loid) content by ICP-MS, and was determined to be adequately homogenous (sample were prepared utilising a range of sample preservation techniques and subjected to a modified sequential extraction procedure or to total metal extraction. Both experiments were repeated after 1-month storage at 4 °C. Cryogenic freezing gave the best reproducibility for total extractable elemental concentrations between months, indicating this to be the most suitable method of sample preparation in such studies. The combined extraction efficiencies were >82% for As, Cu, Mn, Pb, Sr and Zn but poor for other elements, where sample preparation strategies 'no sample preparation' and 'dried in a desiccator' had the best extraction recoveries. Cryogenic freezing procedures had a significantly (p sample cleaning and preservation when species fractionation patterns are of interest. This study also shows that the assumption that species stability can be ensured through cryopreservation and freeze drying techniques needs to be revisited.

  3. The use of gamma ray computed tomography to investigate soil compaction due to core sampling devices

    International Nuclear Information System (INIS)

    Pires, Luiz F.; Arthur, Robson C.J.; Correchel, Vladia; Bacchi, Osny O.S.; Reichardt, Klaus; Brasil, Rene P. Camponez do

    2004-01-01

    Compaction processes can influence soil physical properties such as soil density, porosity, pore size distribution, and processes like soil water and nutrient movements, root system distribution, and others. Soil porosity modification has important consequences like alterations in results of soil water retention curves. These alterations may cause differences in soil water storage calculations and matrix potential values, which are utilized in irrigation management systems. Because of this, soil-sampling techniques should avoid alterations of sample structure. In this work soil sample compaction caused by core sampling devices was investigated using the gamma ray computed tomography technique. A first generation tomograph with fixed source-detector arrangement and translation/rotational movements of the sample was utilized to obtain the images. The radioactive source is 241 Am, with an activity of 3.7 GBq, and the detector consists of a 3 in. x 3 in. NaI(Tl) scintillation crystal coupled to a photomultiplier tube. Soil samples were taken from an experimental field utilizing cylinders 4.0 cm high and 2.6 cm in diameter. Based on image analyses it was possible to detect compacted regions in all samples next to the cylinder wall due to the sampling system. Tomographic unit profiles of the sample permitted to identify higher values of soil density for deeper regions of the sample, and it was possible to determine the average densities and thickness of these layers. Tomographic analyses showed to be a very useful tool for soil compaction characterization and presented many advantages in relation to traditional methods. (author)

  4. Molecular identification of Coccidioides spp. in soil samples from Brazil.

    Science.gov (United States)

    de Macêdo, Regina C L; Rosado, Alexandre S; da Mota, Fabio F; Cavalcante, Maria A S; Eulálio, Kelsen D; Filho, Antônio D; Martins, Liline M S; Lazéra, Márcia S; Wanke, Bodo

    2011-05-16

    Since 1991 several outbreaks of acute coccidioidomycosis (CM) were diagnosed in the semi-arid Northeast of Brazil, mainly related to disturbance of armadillo burrows caused by hunters while digging them for the capture of these animals. This activity causes dust contaminated with arthroconidia of Coccidioides posadasii, which, once inhaled, cause the mycosis. We report on the identification of C. posadasii in soil samples related to outbreaks of CM. Twenty four soil samples had their DNA extracted and subsequently submitted to a semi-nested PCR technique using specific primers. While only 6 (25%) soil samples were positive for C. posadasii by mice inoculation, all (100%) were positive by the molecular tool. This methodology represents a simple, sensitive and specific molecular technique to determine the environmental distribution of Coccidioides spp. in endemic areas, but cannot distinguish the species. Moreover, it may be useful to identify culture isolates. Key-words: 1. Coccidioidomycosis. 2. Coccidioides spp. 3. C. posadasii. 4. Semi-arid. 5. Semi-nested PCR.

  5. 76 FR 11334 - Safety Zone; Soil Sampling; Chicago River, Chicago, IL

    Science.gov (United States)

    2011-03-02

    ...The Coast Guard is establishing a temporary safety zone on the North Branch of the Chicago River near Chicago, Illinois. This zone is intended to restrict vessels from a portion of the North Branch of the Chicago River due to soil sampling in this area. This temporary safety zone is necessary to protect the surrounding public and vessels from the hazards associated with the soil sampling efforts.

  6. Isolation of antimicrobial producing Actinobacteria from soil samples.

    Science.gov (United States)

    Elbendary, Afaf Ahmed; Hessain, Ashgan Mohamed; El-Hariri, Mahmoud Darderi; Seida, Ahmed Adel; Moussa, Ihab Mohamed; Mubarak, Ayman Salem; Kabli, Saleh A; Hemeg, Hassan A; El Jakee, Jakeen Kamal

    2018-01-01

    Emergence of multidrug resistant bacteria has made the search for novel bioactive compounds from natural and unexplored habitats a necessity. Actinobacteria have important bioactive substances. The present study investigated antimicrobial activity of Actinobacteria isolated from soil samples of Egypt. One hundred samples were collected from agricultural farming soil of different governorates. Twelve isolates have produced activity against the tested microorganisms ( S. aureus , Bacillus cereus , E. coli , K. pneumoniae , P. aeruginosa , S. Typhi, C. albicans , A. niger and A. flavus ). By VITEK 2 system version: 07.01 the 12 isolates were identified as Kocuria kristinae , Kocuria rosea , Streptomyces griseus , Streptomyces flaveolus and Actinobacteria . Using ethyl acetate extraction method the isolates culture's supernatants were tested by diffusion method against indicator microorganisms. These results indicate that Actinobacteria isolated from Egypt farms could be sources of antimicrobial bioactive substances.

  7. Field Sample Preparation Method Development for Isotope Ratio Mass Spectrometry

    International Nuclear Information System (INIS)

    Leibman, C.; Weisbrod, K.; Yoshida, T.

    2015-01-01

    Non-proliferation and International Security (NA-241) established a working group of researchers from Los Alamos National Laboratory (LANL), Pacific Northwest National Laboratory (PNNL) and Savannah River National Laboratory (SRNL) to evaluate the utilization of in-field mass spectrometry for safeguards applications. The survey of commercial off-the-shelf (COTS) mass spectrometers (MS) revealed no instrumentation existed capable of meeting all the potential safeguards requirements for performance, portability, and ease of use. Additionally, fieldable instruments are unlikely to meet the International Target Values (ITVs) for accuracy and precision for isotope ratio measurements achieved with laboratory methods. The major gaps identified for in-field actinide isotope ratio analysis were in the areas of: 1. sample preparation and/or sample introduction, 2. size reduction of mass analyzers and ionization sources, 3. system automation, and 4. decreased system cost. Development work in 2 through 4, numerated above continues, in the private and public sector. LANL is focusing on developing sample preparation/sample introduction methods for use with the different sample types anticipated for safeguard applications. Addressing sample handling and sample preparation methods for MS analysis will enable use of new MS instrumentation as it becomes commercially available. As one example, we have developed a rapid, sample preparation method for dissolution of uranium and plutonium oxides using ammonium bifluoride (ABF). ABF is a significantly safer and faster alternative to digestion with boiling combinations of highly concentrated mineral acids. Actinides digested with ABF yield fluorides, which can then be analyzed directly or chemically converted and separated using established column chromatography techniques as needed prior to isotope analysis. The reagent volumes and the sample processing steps associated with ABF sample digestion lend themselves to automation and field

  8. Spiked natural matrix materials as quality assessment samples

    International Nuclear Information System (INIS)

    Feiner, M.S.; Sanderson, C.G.

    1988-01-01

    The Environmental Measurements Laboratory has conducted the Quality Assessment Program since 1976 to evaluate the quality of the environmental radioactivity data, which is reported to the Department of Energy by as many as 42 commercial contractors involved in nuclear work. In this program, matrix materials of known radionuclide concentrations are distributed routinely to the contractors and the reported results are compared. The five matrices used are: soil, vegetation, animal tissue, water and filter paper. Environmental soil, vegetation and animal tissue are used, but the water and filter paper samples are prepared by spiking with known amounts of standard solutions traceable to the National Bureau of Standards. A summary of results is given to illustrate the successful operation of the program. Because of the difficulty and high cost of collecting large samples of natural matrix material and to increase the versatility of the program, an attempt was recently made to prepare the soil, vegetation and animal tissue samples with spiked solutions. A description of the preparation of these reference samples and the results of analyses are presented along with a discussion of the pitfalls and advantages of this approach. 19 refs.; 6 tabs

  9. Exchangeable phosphorus and others parameters in soil samples from Sapucai

    International Nuclear Information System (INIS)

    Facetti, J.F.; Zanotti, J.F.

    1972-01-01

    Soils samples from the alkaline rocks area at Sapucai were studied. The total amount of P in the soils shows to be high, as well as the E value for the 32 P exclangeable phosphorus. Other parameters like V values, TEC, etc., and their relationschip also were analyzed

  10. Exchangeable phosphorus and others parameters in soil samples from Sapucai

    Energy Technology Data Exchange (ETDEWEB)

    Facetti, J F; Zanotti, J F [Asuncion Nacional Univ. (Paraguay). Inst. de Ciencias

    1972-01-01

    Soils samples from the alkaline rocks area at Sapucai were studied. The total amount of P in the soils shows to be high, as well as the E value for the 32 P exclangeable phosphorus. Other parameters like V values, TEC, etc., and their relationschip also were analyzed.

  11. Mobility, bioavailability, and toxic effects of cadmium in soil samples

    International Nuclear Information System (INIS)

    Prokop, Z.; Cupr, P.; Zlevorova-Zlamalikova V.; Komarek, J.; Dusek, L.; Holoubek, I.

    2003-01-01

    Total concentration is not a reliable indicator of metal mobility or bioavailability in soils. The physicochemical form determines the behavior of metals in soils and hence the toxicity toward terrestrial biota. The main objectives of this study were the application and comparison of three approaches for the evaluation of cadmium behavior in soil samples. The mobility and bioavailability of cadmium in five selected soil samples were evaluated using equilibrium speciation (Windermere humic aqueous mode (WHAM)), extraction procedures (Milli-Q water, DMSO, and DTPA), and a number of bioassays (Microtox, growth inhibition test, contact toxicity test, and respiration). The mobility, represented by the water-extractable fraction corresponded well with the amount of cadmium in the soil solution, calculate using the WHAM (r 2 =0.96, P<0.001). The results of the ecotoxicologica evaluation, which represent the bioavailable fraction of cadmium, correlated well with DTPA extractability and also with the concentration of free cadmium ion, which is recognized as the most bioavailable metal form. The results of the WHAM as well as the results of extraction experiments showed a strong binding of cadmium to organic matter and a weak sorption of cadmium to clay minerals

  12. Determination of pyridine in soil and water samples of a polluted area

    International Nuclear Information System (INIS)

    Peters, R.J.B.; Renesse van Duivenbode, J.A.D. van

    1994-01-01

    A method for the analyses of pyridine in environmental samples is described. For soil samples a distillation procedure followed by an extraction, an acidic extraction or a Soxhlet extraction can be used. For water samples a distillation procedure followed by extraction can be employed. Deuterated pyridine is used as an internal standard and the extracts are analyzed by GC-MS. The recoveries of the methods are higher than 80%; the detection limits for pyridine are 0.01 mg/kg for soil samples and 0.2 μg/l for water samples. (orig.)

  13. Choice and preparation of standard samples for X-ray spectral microanalysis

    International Nuclear Information System (INIS)

    Gavrilenko, I.S.; Surzhko, V.F.

    1989-01-01

    Choice, preparation and certification of standard samples for X-ray spectral microanalysis are considered. Requirements for standard samples in terms of concentration and volume, porosity, corrosion, conductivity distribution are formulated. Stages of sample preparation process, including composition choice, heat treatment, section production, certification, are considered in detail. The choice of composition is based on studying phase equilibrium diagrams, subdivided into 6 types

  14. An Open-source Low-cost Portable Apparatus for Soil Fauna Sampling

    Science.gov (United States)

    Daliakopoulos, Ioannis; Wagner, Karl; Grillakis, Manolis; Apostolakis, Antonios; Tsanis, Ioannis

    2016-04-01

    A low-cost apparatus for the extraction of living soil animals from soil or litter samples is presented. The main unit consists of a modular bank system with three horizontal shelves designed to accommodate lamps and soil samples over funnel and jar systems for animal collection, thus serving as a practical and standardized modification of the well-documented Berlese-Tullgren funnel. Shelves are vertically adjustable, sliding on 5 mm threaded rods and securing with wing nuts for easy assembly/disassembly and stability. Shelf material is 4 mm plywood (or similar), laser-cut (or similar) to accommodate lamp sockets, tubes and funnels at respective levels. Soil samples are inserted in 10 cm tubes from standard Ø50 mm PVC piping that can also function as direct collection corers for softer soils. Tubes are fitted in the tube bank shelf, each directly under a 25 W reflector lamp and over a funnel and jar system. Lamps are located 25 mm over the tubes' top creating a relatively constant 10 oC temperature gradient that drives soil animals away from heat and light, and towards the bottom end of the tube which is fitted with a suitable fabric mesh. Standard 106 ml panelled jars, filled with a safe-to-handle preservative (e.g. propylene glycol) to the lower end of the funnel fitted in them, trap and preserve soil organisms until identification. The apparatus offers flat-pack portability and scalability using low-cost standard material. Design specifications and Drawing eXchange Format (dxf) files for apparatus reproduction are provided.

  15. Direct determination of uranium in soil, rock, ore and biological samples by laser-induced fluorometry

    International Nuclear Information System (INIS)

    Li Qingzhen; Zhang Yanan

    1993-03-01

    A laser-induced fluorometric method with modified J-22 anti-interferent fluorescent reagent for directly determining the uranium in soil, rock, ore, geochemical, biological and other samples has been studied. The effects of external ions and dilution law of sample are examined in detail. A method for correcting inner effect is proposed. A mixed solution of 0.25% NaOH-10% J-22 is prepared which can be added to the sample cuvette for direct measurement without any pre-adjustment of acidity. Therefore, it is much simpler for operation and reduces the loss and contamination of uranium. By changing the laser fluorometer sensitivity (400 ∼ 200), up to 3000 ng uranium in the cuvette can be detected. Thus, both analytical accuracy and detectable range are improved. This method is simple, rapid, accurate and applicable to various uranium-bearing samples. The detection limit is better than 0.05 μgU/g. The relative standard deviation is ≤+-5% for the rock reference samples of 0.95, 84.8, 669 and 7240 μgU/g

  16. Novel strategies for sample preparation in forensic toxicology.

    Science.gov (United States)

    Samanidou, Victoria; Kovatsi, Leda; Fragou, Domniki; Rentifis, Konstantinos

    2011-09-01

    This paper provides a review of novel strategies for sample preparation in forensic toxicology. The review initially outlines the principle of each technique, followed by sections addressing each class of abused drugs separately. The novel strategies currently reviewed focus on the preparation of various biological samples for the subsequent determination of opiates, benzodiazepines, amphetamines, cocaine, hallucinogens, tricyclic antidepressants, antipsychotics and cannabinoids. According to our experience, these analytes are the most frequently responsible for intoxications in Greece. The applications of techniques such as disposable pipette extraction, microextraction by packed sorbent, matrix solid-phase dispersion, solid-phase microextraction, polymer monolith microextraction, stir bar sorptive extraction and others, which are rapidly gaining acceptance in the field of toxicology, are currently reviewed.

  17. Regional soil erosion assessment based on a sample survey and geostatistics

    Science.gov (United States)

    Yin, Shuiqing; Zhu, Zhengyuan; Wang, Li; Liu, Baoyuan; Xie, Yun; Wang, Guannan; Li, Yishan

    2018-03-01

    Soil erosion is one of the most significant environmental problems in China. From 2010 to 2012, the fourth national census for soil erosion sampled 32 364 PSUs (Primary Sampling Units, small watersheds) with the areas of 0.2-3 km2. Land use and soil erosion controlling factors including rainfall erosivity, soil erodibility, slope length, slope steepness, biological practice, engineering practice, and tillage practice for the PSUs were surveyed, and the soil loss rate for each land use in the PSUs was estimated using an empirical model, the Chinese Soil Loss Equation (CSLE). Though the information collected from the sample units can be aggregated to estimate soil erosion conditions on a large scale; the problem of estimating soil erosion condition on a regional scale has not been addressed well. The aim of this study is to introduce a new model-based regional soil erosion assessment method combining a sample survey and geostatistics. We compared seven spatial interpolation models based on the bivariate penalized spline over triangulation (BPST) method to generate a regional soil erosion assessment from the PSUs. Shaanxi Province (3116 PSUs) in China was selected for the comparison and assessment as it is one of the areas with the most serious erosion problem. Ten-fold cross-validation based on the PSU data showed the model assisted by the land use, rainfall erosivity factor (R), soil erodibility factor (K), slope steepness factor (S), and slope length factor (L) derived from a 1 : 10 000 topography map is the best one, with the model efficiency coefficient (ME) being 0.75 and the MSE being 55.8 % of that for the model assisted by the land use alone. Among four erosion factors as the covariates, the S factor contributed the most information, followed by K and L factors, and R factor made almost no contribution to the spatial estimation of soil loss. The LS factor derived from 30 or 90 m Shuttle Radar Topography Mission (SRTM) digital elevation model (DEM) data

  18. Radioactivity in Soil Samples Collected in Southern Serbia

    International Nuclear Information System (INIS)

    Jankovic, M.; Nikolic, J.; Pantelic, G.; Rajacic, M.; Sarap, N.; Todorovic, D.

    2013-01-01

    In the attack on the Federal Republic of Yugoslavia (the focus effect was of Kosovo and Metohija and southern Serbia) in 1999, NATO forces used ammunition containing depleted uranium. Cleaning action of depleted uranium was performed by Radiation and Environmental Protection Department of the Vinca Institute of Nuclear Science, during 2002?2007 at locations: Pljackovica, Bratoselce, Borovac and Reljan. At all locations underwent detailed dosimetric screening and decontamination was performed. Because of the loose soil, DU projectils were found to a depth of 1 m. Found missiles, contaminated soil and radioactive material has been collected and stored on radioactive waste. After cleaning the ground is leveled and another dosimetric prospecting was performed. Monitoring of radioactivity in southern Serbia included determination of gamma emitters as well as determination of gross alpha and beta activities in soil, water and plant. Sampling was carried out at Pljackovica, Borovac, Bratoselce and Reljan in July 2011. This paper presents only the results of measurement of gamma emitters in soil samples and showed the presence of natural radionuclides: 226Ra, 232Th, 40K, 235U, 238U and the produced radionuclide 137Cs (from the Chernobyl accident). Also, the ratio between the 235U and 238U is given. In order to evaluate the radiological hazard of the natural radioactivity, the radium equivalent activity, the gamma-absorbed dose rate and the external hazard index have been calculated. (author)

  19. TEM sample preparation by FIB for carbon nanotube interconnects

    International Nuclear Information System (INIS)

    Ke, Xiaoxing; Bals, Sara; Romo Negreira, Ainhoa; Hantschel, Thomas; Bender, Hugo; Van Tendeloo, Gustaaf

    2009-01-01

    A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

  20. TEM sample preparation by FIB for carbon nanotube interconnects

    Energy Technology Data Exchange (ETDEWEB)

    Ke, Xiaoxing, E-mail: xiaoxing.ke@ua.ac.be [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Bals, Sara [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Romo Negreira, Ainhoa [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Metallurgy and Materials Engineering Department, KU Leuven, Kasteelpark Arenberg 44, Leuven B-3001 (Belgium); Hantschel, Thomas; Bender, Hugo [IMEC, Kapeldreef 75, B-3001 Leuven (Belgium); Van Tendeloo, Gustaaf [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium)

    2009-10-15

    A powerful method to study carbon nanotubes (CNTs) grown in patterned substrates for potential interconnects applications is transmission electron microscopy (TEM). However, high-quality TEM samples are necessary for such a study. Here, TEM specimen preparation by focused ion beam (FIB) has been used to obtain lamellae of patterned samples containing CNTs grown inside contact holes. A dual-cap Pt protection layer and an extensive 5 kV cleaning procedure are applied in order to preserve the CNTs and avoid deterioration during milling. TEM results show that the inner shell structure of the carbon nanotubes has been preserved, which proves that focused ion beam is a useful technique to prepare TEM samples of CNT interconnects.

  1. Analysis of arsenic and calcium in soil samples by laser ablation mass spectrometry

    International Nuclear Information System (INIS)

    Beccaglia, Ana M.; Rinaldi, Carlos A.; Ferrero, Juan C.

    2006-01-01

    We present an analytical procedure based on laser ablation mass spectrometry (LAMS) in order to detect and quantify arsenic and calcium in soil samples and we analyze the diverse factors that influence the precision of LAMS, such as laser fluence and matrix effect. The results indicate that a Zn matrix is a good choice for the analysis of those metals in soil samples. This work also provides a method for the direct determination of As in soil samples whose concentrations are lower than 100 ppm with a 70 ppm minimum detection limits (MDL)

  2. Extraction and analysis of 14C-carbofuran radioactivity in soil sample

    International Nuclear Information System (INIS)

    Maizatul Akmam Mhd Nasir; Nashriyah Mat

    2005-01-01

    Carbofuran insecticide or nematicide sprayed onto soil in the agroecosystem will be taken up by plant. Carbofuran residue will pollute the environment and organisms in the food chain. Extraction and analysis of 14 C-carbofuran in soil from lysimeter were carried out. The Liquid Scintillation Counter (LSC) was used to measure radioactivity of 14 C-carbofuran in soil sample. (Author)

  3. Isolation of antimicrobial producing Actinobacteria from soil samples

    Directory of Open Access Journals (Sweden)

    Afaf Ahmed Elbendary

    2018-01-01

    Full Text Available Emergence of multidrug resistant bacteria has made the search for novel bioactive compounds from natural and unexplored habitats a necessity. Actinobacteria have important bioactive substances. The present study investigated antimicrobial activity of Actinobacteria isolated from soil samples of Egypt. One hundred samples were collected from agricultural farming soil of different governorates. Twelve isolates have produced activity against the tested microorganisms (S. aureus, Bacillus cereus, E. coli, K. pneumoniae, P. aeruginosa, S. Typhi, C. albicans, A. niger and A. flavus. By VITEK 2 system version: 07.01 the 12 isolates were identified as Kocuria kristinae, Kocuria rosea, Streptomyces griseus, Streptomyces flaveolus and Actinobacteria. Using ethyl acetate extraction method the isolates culture’s supernatants were tested by diffusion method against indicator microorganisms. These results indicate that Actinobacteria isolated from Egypt farms could be sources of antimicrobial bioactive substances.

  4. Selecting Sample Preparation Workflows for Mass Spectrometry-Based Proteomic and Phosphoproteomic Analysis of Patient Samples with Acute Myeloid Leukemia.

    Science.gov (United States)

    Hernandez-Valladares, Maria; Aasebø, Elise; Selheim, Frode; Berven, Frode S; Bruserud, Øystein

    2016-08-22

    Global mass spectrometry (MS)-based proteomic and phosphoproteomic studies of acute myeloid leukemia (AML) biomarkers represent a powerful strategy to identify and confirm proteins and their phosphorylated modifications that could be applied in diagnosis and prognosis, as a support for individual treatment regimens and selection of patients for bone marrow transplant. MS-based studies require optimal and reproducible workflows that allow a satisfactory coverage of the proteome and its modifications. Preparation of samples for global MS analysis is a crucial step and it usually requires method testing, tuning and optimization. Different proteomic workflows that have been used to prepare AML patient samples for global MS analysis usually include a standard protein in-solution digestion procedure with a urea-based lysis buffer. The enrichment of phosphopeptides from AML patient samples has previously been carried out either with immobilized metal affinity chromatography (IMAC) or metal oxide affinity chromatography (MOAC). We have recently tested several methods of sample preparation for MS analysis of the AML proteome and phosphoproteome and introduced filter-aided sample preparation (FASP) as a superior methodology for the sensitive and reproducible generation of peptides from patient samples. FASP-prepared peptides can be further fractionated or IMAC-enriched for proteome or phosphoproteome analyses. Herein, we will review both in-solution and FASP-based sample preparation workflows and encourage the use of the latter for the highest protein and phosphorylation coverage and reproducibility.

  5. Development of sample preparation method for honey analysis using PIXE

    International Nuclear Information System (INIS)

    Saitoh, Katsumi; Chiba, Keiko; Sera, Koichiro

    2008-01-01

    We developed an original preparation method for honey samples (samples in paste-like state) specifically designed for PIXE analysis. The results of PIXE analysis of thin targets prepared by adding a standard containing nine elements to honey samples demonstrated that the preparation method bestowed sufficient accuracy on quantitative values. PIXE analysis of 13 kinds of honey was performed, and eight mineral components (Si, P, S, K, Ca, Mn, Cu and Zn) were detected in all honey samples. The principal mineral components were K and Ca, and the quantitative value for K accounted for the majority of the total value for mineral components. K content in honey varies greatly depending on the plant source. Chestnuts had the highest K content. In fact, it was 2-3 times that of Manuka, which is known as a high quality honey. K content of false-acacia, which is produced in the greatest abundance, was 1/20 that of chestnuts. (author)

  6. The depth distribution functions of the natural abundances of carbon isotopes in Alfisols thoroughly sampled by thin-layer sampling, and their relation to the dynamics of organic matter in theses soils

    International Nuclear Information System (INIS)

    Becker-Heidmann, P.

    1989-01-01

    The aim of this study was to gain fundamental statements on the relationship between the depth distributions of the natural abundances of 13 C and 14 C isotopes and the dynamics of the organic matter in Alfisols. For this purpose, six Alfisols were investigated: four forest soils from Northern Germany, two of them developed in Loess and two in glacial loam, one West German Loess soil used for fruit-growing and one agricultural granite-gneiss soil from the semiarid part of India. The soil was sampled as succesive horizontal layers of 2 cm depth from an area of 0.5 to 1 m 2 size, starting from the organic down to the C horizon or the lower part of the Bt. This kind of completely thin-layer-wise sampling was applied here for the first time. The carbon content and the natural abundances of the 13 C and the 14 C isotopes of each sample were determined. The δ 13 C value was measured by mass spectrometry. A vacuum preparation line with an electronically controlled cooling unit was constructed thereto. For the determination of the 14 C content, the sample carbon was transferred into benzene, and its activity was measured by liquid scintillation spectrometry. From the combination of the depth distribution functions of the 14 C activity and the δ 13 C value, and with the aid of additional analyses like C/N ratio and particle size distribution, a conclusive interpretation as to the dynamics of the organic matter in the investigated Alfisols is given. (orig./BBR)

  7. Witness sample preparation for measuring antireflection coatings.

    Science.gov (United States)

    Willey, Ronald R

    2014-02-01

    Measurement of antireflection coating of witness samples from across the worldwide industry has been shown to have excess variability from a sampling taken for the OSA Topical Meeting on Optical Interference Coatings: Measurement Problem. Various sample preparation techniques have been discussed with their limitations, and a preferred technique is recommended with its justification, calibration procedures, and limitations. The common practice of grinding the second side to reduce its reflection is less than satisfactory. One recommended practice is to paint the polished second side, which reduces its reflection to almost zero. A method to evaluate the suitability of given paints is also described.

  8. Sample preparation method for scanning force microscopy

    CERN Document Server

    Jankov, I R; Szente, R N; Carreno, M N P; Swart, J W; Landers, R

    2001-01-01

    We present a method of sample preparation for studies of ion implantation on metal surfaces. The method, employing a mechanical mask, is specially adapted for samples analysed by Scanning Force Microscopy. It was successfully tested on polycrystalline copper substrates implanted with phosphorus ions at an acceleration voltage of 39 keV. The changes of the electrical properties of the surface were measured by Kelvin Probe Force Microscopy and the surface composition was analysed by Auger Electron Spectroscopy.

  9. Status report of AMS sample preparation laboratory at GADAM Centre, Gliwice, Poland

    Energy Technology Data Exchange (ETDEWEB)

    Piotrowska, N., E-mail: natalia.piotrowska@polsl.pl [GADAM Centre of Excellence, Department of Radioisotopes, Institute of Physics, Silesian University of Technology, Gliwice (Poland)

    2013-01-15

    The laboratory for {sup 14}C AMS sample preparation in the Gliwice Radiocarbon Laboratory has gradually evolved since its start in 1999 to cater for an increase in volume and variety of radiocarbon dating samples. To date, nearly 2000 graphite targets have been produced from materials such as plant macrofossils, charcoal, peat, bones, shells and wood. The equipment comprises a station for chemical preparation and high vacuum lines for production, purification and graphitization of sample carbon dioxide. The present capacity allows preparation of up to 400 targets annually for the needs of scientific projects and external orders for radiocarbon dating continuously received by the GADAM Centre of Excellence. The laboratory's sample preparation protocols and recent improvements are described and its performance during the 10 years of activity is discussed in terms of parameters obtained from reference materials prepared in this laboratory and demonstrated with a few science applications.

  10. A New Approach To Soil Sampling For Risk Assessment Of Nutrient Mobilisation.

    Science.gov (United States)

    Jonczyk, J. C.; Owen, G. J.; Snell, M. A.; Barber, N.; Benskin, C.; Reaney, S. M.; Haygarth, P.; Quinn, P. F.; Barker, P. A.; Aftab, A.; Burke, S.; Cleasby, W.; Surridge, B.; Perks, M. T.

    2016-12-01

    Traditionally, risks of nutrient and sediment losses from soils are assessed through a combination of field soil nutrient values on soil samples taken over the whole field and the proximity of the field to water courses. The field average nutrient concentration of the soil is used by farmers to determine fertiliser needs. These data are often used by scientists to assess the risk of nutrient losses to water course, though are not really `fit' for this purpose. The Eden Demonstration Test Catchment (http://www.edendtc.org.uk/) is a research project based in the River Eden catchment, NW UK, with the aim of cost effectively mitigating diffuse pollution from agriculture whilst maintaining agricultural productivity. Three instrumented focus catchments have been monitored since 2011, providing high resolution in-stream chemistry and ecological data, alongside some spatial data on soils, land use and nutrient inputs. An approach to mitigation was demonstrated in a small sub-catchment, where surface runoff was identified as the key drivers of nutrient losses, using a suite of runoff attenuation features. Other issues identified were management of hard- standings and soil compaction. A new approach for evaluating nutrient losses from soils is assessed in the Eden DTC project. The Sensitive Catchment Integrated Modelling and Prediction (SCIMAP) model is a risk-mapping framework designed to identify where in the landscape diffuse pollution is most likely to be originating (http://www.scimap.org.uk) and was used to look at the spatial pattern of erosion potential. The aim of this work was to assess if erosion potential identified through the model could be used to inform a new soil sampling strategy, to better assess risk of erosion and risk of transport of sediment-bound phosphorus. Soil samples were taken from areas with different erosion potential. The chemical analysis of these targeted samples are compared to those obtained using more traditional sampling approaches

  11. Sample preparation techniques of biological material for isotope analysis

    International Nuclear Information System (INIS)

    Axmann, H.; Sebastianelli, A.; Arrillaga, J.L.

    1990-01-01

    Sample preparation is an essential step in all isotope-aided experiments but often it is not given enough attention. The methods of sample preparation are very important to obtain reliable and precise analytical data and for further interpretation of results. The size of a sample required for chemical analysis is usually very small (10mg-1500mg). On the other hand the amount of harvested plant material from plots in a field experiment is often bulky (several kilograms) and the entire sample is too large for processing. In addition, while approaching maturity many crops show not only differences in physical consistency but also a non-uniformity in 15 N content among plant parts, requiring a plant fractionation or separation into parts (vegetative and reproductive) e.g. shoots and spikes, in case of small grain cereals, shoots and pods in case of grain legumes and tops and roots or beets (including crown) in case of sugar beet, etc. In any case the ultimate goal of these procedures is to obtain representative subsample harvested from greenhouse or field experiments for chemical analysis. Before harvesting an isotopic-aided experiment the method of sampling has to be selected. It should be based on the type of information required in relation to the objectives of the research and the availability of resources (staff, sample preparation equipment, analytical facilities, chemicals and supplies, etc.). 10 refs, 3 figs, 3 tabs

  12. Molecular identification of Coccidioides spp. in soil samples from Brazil

    Directory of Open Access Journals (Sweden)

    Filho Antônio D

    2011-05-01

    Full Text Available Abstract Background Since 1991 several outbreaks of acute coccidioidomycosis (CM were diagnosed in the semi-arid Northeast of Brazil, mainly related to disturbance of armadillo burrows caused by hunters while digging them for the capture of these animals. This activity causes dust contaminated with arthroconidia of Coccidioides posadasii, which, once inhaled, cause the mycosis. We report on the identification of C. posadasii in soil samples related to outbreaks of CM. Results Twenty four soil samples had their DNA extracted and subsequently submitted to a semi-nested PCR technique using specific primers. While only 6 (25% soil samples were positive for C. posadasii by mice inoculation, all (100% were positive by the molecular tool. Conclusion This methodology represents a simple, sensitive and specific molecular technique to determine the environmental distribution of Coccidioides spp. in endemic areas, but cannot distinguish the species. Moreover, it may be useful to identify culture isolates. Key-words: 1. Coccidioidomycosis. 2. Coccidioides spp. 3. C. posadasii. 4. Semi-arid. 5. Semi-nested PCR

  13. The use of supercritical fluid extraction as a sample preparation technique for soils

    International Nuclear Information System (INIS)

    Levy, J.M.; Dolata, L.A.; Rosselli, A.C.; Ravey, R.M.

    1994-01-01

    Using off-line supercritical fluid extraction (SFE), polynuclear aromatic hydrocarbons (PAHs) were extracted at different levels from various soil and sediment matrices. Based upon GC/MS measurements a number of SFE operational parameters including pressure, temperature and flow rate, were optimized to yield the highest efficiencies with the best precision

  14. [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.

  15. Analysis of soil samples from Gebeng area using NAA technique

    Science.gov (United States)

    Elias, Md Suhaimi; Wo, Yii Mei; Hamzah, Mohd Suhaimi; Shukor, Shakirah Abd; Rahman, Shamsiah Ab; Salim, Nazaratul Ashifa Abdullah; Azman, Muhamad Azfar; Hashim, Azian

    2017-01-01

    Rapid development and urbanization will increase number of residence and industrial area. Without proper management and control of pollution, these will give an adverse effect to environment and human life. The objective of this study to identify and quantify key contaminants into the environment of the Gebeng area as a result of industrial and human activities. Gebeng area was gazetted as one of the industrial estate in Pahang state. Assessment of elemental pollution in soil of Gebeng area base on level of concentration, enrichment factor and geo-accumulation index. The enrichment factors (EFs) were determined by the elemental rationing method, whilst the geo-accumulation index (Igeo) by comparing of current to continental crustal average concentration of element. Twenty-seven of soil samples were collected from Gebeng area. Soil samples were analysed by using Neutron Activation Analyses (NAA) technique. The obtained data showed higher concentration of iron (Fe) due to abundance in soil compared to other elements. The results of enrichment factor showed that Gebeng area have enrich with elements of As, Br, Hf, Sb, Th and U. Base on the geo-accumulation index (Igeo) classification, the soil quality of Gebeng area can be classified as class 0, (uncontaminated) to Class 3, (moderately to heavily contaminated).

  16. Considerations for Sample Preparation Using Size-Exclusion Chromatography for Home and Synchrotron Sources.

    Science.gov (United States)

    Rambo, Robert P

    2017-01-01

    The success of a SAXS experiment for structural investigations depends on two precise measurements, the sample and the buffer background. Buffer matching between the sample and background can be achieved using dialysis methods but in biological SAXS of monodisperse systems, sample preparation is routinely being performed with size exclusion chromatography (SEC). SEC is the most reliable method for SAXS sample preparation as the method not only purifies the sample for SAXS but also almost guarantees ideal buffer matching. Here, I will highlight the use of SEC for SAXS sample preparation and demonstrate using example proteins that SEC purification does not always provide for ideal samples. Scrutiny of the SEC elution peak using quasi-elastic and multi-angle light scattering techniques can reveal hidden features (heterogeneity) of the sample that should be considered during SAXS data analysis. In some cases, sample heterogeneity can be controlled using a small molecule additive and I outline a simple additive screening method for sample preparation.

  17. A Method for Microalgae Proteomics Analysis Based on Modified Filter-Aided Sample Preparation.

    Science.gov (United States)

    Li, Song; Cao, Xupeng; Wang, Yan; Zhu, Zhen; Zhang, Haowei; Xue, Song; Tian, Jing

    2017-11-01

    With the fast development of microalgal biofuel researches, the proteomics studies of microalgae increased quickly. A filter-aided sample preparation (FASP) method is widely used proteomics sample preparation method since 2009. Here, a method of microalgae proteomics analysis based on modified filter-aided sample preparation (mFASP) was described to meet the characteristics of microalgae cells and eliminate the error caused by over-alkylation. Using Chlamydomonas reinhardtii as the model, the prepared sample was tested by standard LC-MS/MS and compared with the previous reports. The results showed mFASP is suitable for most of occasions of microalgae proteomics studies.

  18. Selecting Sample Preparation Workflows for Mass Spectrometry-Based Proteomic and Phosphoproteomic Analysis of Patient Samples with Acute Myeloid Leukemia

    Directory of Open Access Journals (Sweden)

    Maria Hernandez-Valladares

    2016-08-01

    Full Text Available Global mass spectrometry (MS-based proteomic and phosphoproteomic studies of acute myeloid leukemia (AML biomarkers represent a powerful strategy to identify and confirm proteins and their phosphorylated modifications that could be applied in diagnosis and prognosis, as a support for individual treatment regimens and selection of patients for bone marrow transplant. MS-based studies require optimal and reproducible workflows that allow a satisfactory coverage of the proteome and its modifications. Preparation of samples for global MS analysis is a crucial step and it usually requires method testing, tuning and optimization. Different proteomic workflows that have been used to prepare AML patient samples for global MS analysis usually include a standard protein in-solution digestion procedure with a urea-based lysis buffer. The enrichment of phosphopeptides from AML patient samples has previously been carried out either with immobilized metal affinity chromatography (IMAC or metal oxide affinity chromatography (MOAC. We have recently tested several methods of sample preparation for MS analysis of the AML proteome and phosphoproteome and introduced filter-aided sample preparation (FASP as a superior methodology for the sensitive and reproducible generation of peptides from patient samples. FASP-prepared peptides can be further fractionated or IMAC-enriched for proteome or phosphoproteome analyses. Herein, we will review both in-solution and FASP-based sample preparation workflows and encourage the use of the latter for the highest protein and phosphorylation coverage and reproducibility.

  19. Final Report for X-ray Diffraction Sample Preparation Method Development

    Energy Technology Data Exchange (ETDEWEB)

    Ely, T. M. [Hanford Site (HNF), Richland, WA (United States); Meznarich, H. K. [Hanford Site (HNF), Richland, WA (United States); Valero, T. [Hanford Site (HNF), Richland, WA (United States)

    2018-01-30

    WRPS-1500790, “X-ray Diffraction Saltcake Sample Preparation Method Development Plan/Procedure,” was originally prepared with the intent of improving the specimen preparation methodology used to generate saltcake specimens suitable for XRD-based solid phase characterization. At the time that this test plan document was originally developed, packed powder in cavity supports with collodion binder was the established XRD specimen preparation method. An alternate specimen preparation method less vulnerable, if not completely invulnerable to preferred orientation effects, was desired as a replacement for the method.

  20. Soil sealing degree as factor influencing urban soil contamination with polycyclic aromatic hydrocarbons (PAHs

    Directory of Open Access Journals (Sweden)

    Mendyk Łukasz

    2016-03-01

    Full Text Available The objective of the study was to determine role of soil sealing degree as the factor influencing soil contamination with polycyclic aromatic hydrocarbons (PAHs. The study area included four sampling sites located within the administrative boundaries of the Toruń city, Poland. Sampling procedure involved preparing soil pits representing three examples of soil sealing at each site: non-sealed soil as a control one (I and two degrees of soil sealing: semi-pervious surface (II and totally impervious surface (III. Together with basic properties defined with standard procedures (particle size distribution, pH, LOI, content of carbonates content of selected PAHs was determined by dichloromethane extraction using gas chromatography with mass spectrometric detection (GC-MS. Obtained results show that urban soils in the city of Toruń are contaminated with polycyclic aromatic hydrocarbons. Soil sealing degree has a strong influence on the soil contamination with polycyclic aromatic hydrocarbons. Totally sealed soils are better preserved from atmospheric pollution including PAHs. Combustion of grass/wood/coal was the main source of determined PAHs content in examined soils.

  1. Poly-use multi-level sampling system for soil-gas transport analysis in the vadose zone.

    Science.gov (United States)

    Nauer, Philipp A; Chiri, Eleonora; Schroth, Martin H

    2013-10-01

    Soil-gas turnover is important in the global cycling of greenhouse gases. The analysis of soil-gas profiles provides quantitative information on below-ground turnover and fluxes. We developed a poly-use multi-level sampling system (PMLS) for soil-gas sampling, water-content and temperature measurement with high depth resolution and minimal soil disturbance. It is based on perforated access tubes (ATs) permanently installed in the soil. A multi-level sampler allows extraction of soil-gas samples from 20 locations within 1 m depth, while a capacitance probe is used to measure volumetric water contents. During idle times, the ATs are sealed and can be equipped with temperature sensors. Proof-of-concept experiments in a field lysimeter showed good agreement of soil-gas samples and water-content measurements compared with conventional techniques, while a successfully performed gas-tracer test demonstrated the feasibility of the PMLS to determine soil-gas diffusion coefficients in situ. A field application of the PMLS to quantify oxidation of atmospheric CH4 in a field lysimeter and in the forefield of a receding glacier yielded activity coefficients and soil-atmosphere fluxes well in agreement with previous studies. With numerous options for customization, the presented tool extends the methodological choices to investigate soil-gas transport in the vadose zone.

  2. GEMAS: Colours of dry and moist agricultural soil samples of Europe

    Science.gov (United States)

    Klug, Martin; Fabian, Karl; Reimann, Clemens

    2016-04-01

    High resolution HDR colour images of all Ap samples from the GEMAS survey were acquired using a GeoTek Linescan camera. Three measurements of dry and wet samples with increasing exposure time and increasing illumination settings produced a set of colour images at 50μm resolution. Automated image processing was used to calibrate the six images per sample with respect to the synchronously measured X-Rite colorchecker chart. The calibrated images were then fit to Munsell soil colours that were measured in the same way. The results provide overview maps of dry and moist European soil colours. Because colour is closely linked to iron mineralogy, carbonate, silicate and organic carbon content the results can be correlated to magnetic, mineralogical, and geochemical properties. In combination with the full GEMAS chemical and physical measurements, this yields a valuable data set for calibration and interpretation of visible satellite colour data with respect to chemical composition and geological background, soil moisture, and soil degradation. This data set will help to develop new methods for world-wide characterization and monitoring of agricultural soils which is essential for quantifying geologic and human impact on the critical zone environment. It furthermore enables the scientific community and governmental authorities to monitor consequences of climatic change, to plan and administrate economic and ecological land use, and to use the data set for forensic applications.

  3. Sample Preparation (SS): SE51_SS01 [Metabolonote[Archive

    Lifescience Database Archive (English)

    Full Text Available e Master NEO, BMS, Tokyo, Japan), and the seed powder was extracted with 1 mL of extraction buffer (0.1% HCO...trifugation (4 ℃, 10,000 rpm, 5 min), the sample tubes were subjected to sample preparation (buffer transfer

  4. Radionuclides and heavy metal contents in phosphogypsum samples in comparison to cerrado soils

    Energy Technology Data Exchange (ETDEWEB)

    Jacomino, Vanusa Maria Feliciano; Oliveira, Kerley Alberto Pereira de, E-mail: vmfj@cdtn.b, E-mail: kapo@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil); Taddei, Maria Helena Tirollo; Nascimento, Marcos Roberto Lopes, E-mail: mhtaddei@cnen.gov.b, E-mail: pmarcos@cnen.gov.b [Laboratorio de Pocos de Caldas (LAPOC/CNEN-MG), MG (Brazil); Siqueira, Maria Celia, E-mail: mc.ufscar@gmail.co [Universidade Federal de Sao Carlos (UFSCar), SP (Brazil). Dept. de Quimica; Carneiro, Maria Eleonora Deschamps Pires, E-mail: eleonora.deschamps@meioambiente.mg.gov.b [Fundacao Estadual do Meio Ambiente (FEAM), Belo Horizonte, MG (Brazil). Gestao de Residuos Solidos; Silva, David Faria da; Mello, Jaime Wilson Vargas de, E-mail: davidf.agro@hotmail.co, E-mail: jwvmello@ufv.b [Universidade Federal de Vicosa (UFV), MG (Brazil). Dept. de Solos

    2009-09-15

    Phosphogypsum (PG) or agricultural gypsum, a solid waste from the phosphate fertilizer industry, is used as soil amendment, especially on soils in the Cerrado region, in Brazil. This material may however contain natural radionuclides and metals which can be transferred to soils, plants and water sources. This paper presents and discusses the results of physical and chemical analyses that characterized samples of PG and compares them to the results found in two typical soils of the Cerrado, a clayey and sandy one. These analyses included: solid waste classification, evaluation of organic matter content and of P, K, Ca, Mg, and Al concentrations and of the mineralogical composition. Natural radionuclides and metal concentrations in PG and soil samples were also measured. Phosphogypsum was classified as Class II A - not dangerous, not inert, not corrosive and not reactive. The organic matter content in the soil samples was low and potential acidity high. In the mean, the specific {sup 226}Ra activity in the phosphogypsum samples (252 Bq kg{sup -1}) was below the maximum level recommended by USEPA, which is 370 Bq kg{sup -1} for agricultural use. In addition, this study verified that natural radionuclides and metals concentrations in PG were lower than in the clayey Oxisol of Sete Lagoas, Minas Gerais, Brazil. These results indicated that the application of phosphogypsum as soil amendment in agriculture would not cause a significant impact on the environment. (author)

  5. Radionuclides and heavy metal contents in phosphogypsum samples in comparison to cerrado soils

    International Nuclear Information System (INIS)

    Jacomino, Vanusa Maria Feliciano; Oliveira, Kerley Alberto Pereira de; Taddei, Maria Helena Tirollo; Nascimento, Marcos Roberto Lopes; Siqueira, Maria Celia; Carneiro, Maria Eleonora Deschamps Pires; Silva, David Faria da; Mello, Jaime Wilson Vargas de

    2009-01-01

    Phosphogypsum (PG) or agricultural gypsum, a solid waste from the phosphate fertilizer industry, is used as soil amendment, especially on soils in the Cerrado region, in Brazil. This material may however contain natural radionuclides and metals which can be transferred to soils, plants and water sources. This paper presents and discusses the results of physical and chemical analyses that characterized samples of PG and compares them to the results found in two typical soils of the Cerrado, a clayey and sandy one. These analyses included: solid waste classification, evaluation of organic matter content and of P, K, Ca, Mg, and Al concentrations and of the mineralogical composition. Natural radionuclides and metal concentrations in PG and soil samples were also measured. Phosphogypsum was classified as Class II A - not dangerous, not inert, not corrosive and not reactive. The organic matter content in the soil samples was low and potential acidity high. In the mean, the specific 226 Ra activity in the phosphogypsum samples (252 Bq kg -1 ) was below the maximum level recommended by USEPA, which is 370 Bq kg -1 for agricultural use. In addition, this study verified that natural radionuclides and metals concentrations in PG were lower than in the clayey Oxisol of Sete Lagoas, Minas Gerais, Brazil. These results indicated that the application of phosphogypsum as soil amendment in agriculture would not cause a significant impact on the environment. (author)

  6. Determination of (90)Sr in soil samples using inductively coupled plasma mass spectrometry equipped with dynamic reaction cell (ICP-DRC-MS).

    Science.gov (United States)

    Feuerstein, J; Boulyga, S F; Galler, P; Stingeder, G; Prohaska, T

    2008-11-01

    A rapid method is reported for the determination of (90)Sr in contaminated soil samples in the vicinity of the Chernobyl Nuclear Power Plant by ICP-DRC-MS. Sample preparation and measurement procedures focus on overcoming the isobaric interference of (90)Zr, which is present in soils at concentrations higher by more than six orders of magnitude than (90)Sr. Zirconium was separated from strontium in two steps to reduce the interference by (90)Zr(+) ions by a factor of more than 10(7): (i) by ion exchange using a Sr-specific resin and (ii) by reaction with oxygen as reaction gas in a dynamic reaction cell (DRC) of a quadrupole ICP-MS. The relative abundance sensitivity of the ICP-MS was studied systematically and the peak tailing originating from (88)Sr on mass 90 u was found to be about 3 x 10(-9). Detection limits of 4 fg g(-1) (0.02 Bq g(-1)) were achieved when measuring Sr solutions containing no Zr. In digested uncontaminated soil samples after matrix separation as well as in a solution of 5 microg g(-1) Sr and 50 ng g(-1) Zr a detection limit of 0.2 pg g(-1) soil (1 Bq g(-1) soil) was determined. (90)Sr concentrations in three soil samples collected in the vicinity of the Chernobyl Nuclear Power Plant were 4.66+/-0.27, 13.48+/-0.68 and 12.9+/-1.5 pg g(-1) corresponding to specific activities of 23.7+/-1.3, 68.6+/-3.5 and 65.6+/-7.8 Bq g(-1), respectively. The ICP-DRC-MS results were compared to the activities measured earlier by radiometry. Although the ICP-DRC-MS is inferior to commonly used radiometric methods with respect to the achievable minimum detectable activity it represents a time- and cost-effective alternative technique for fast monitoring of high-level (90)Sr contamination in environmental or nuclear industrial samples down to activities of about 1 Bq g(-1).

  7. Determination of 90Sr in soil samples using inductively coupled plasma mass spectrometry equipped with dynamic reaction cell (ICP-DRC-MS)

    International Nuclear Information System (INIS)

    Feuerstein, J.; Boulyga, S.F.; Galler, P.; Stingeder, G.; Prohaska, T.

    2008-01-01

    A rapid method is reported for the determination of 90 Sr in contaminated soil samples in the vicinity of the Chernobyl Nuclear Power Plant by ICP-DRC-MS. Sample preparation and measurement procedures focus on overcoming the isobaric interference of 90 Zr, which is present in soils at concentrations higher by more than six orders of magnitude than 90 Sr. Zirconium was separated from strontium in two steps to reduce the interference by 90 Zr + ions by a factor of more than 10 7 : (i) by ion exchange using a Sr-specific resin and (ii) by reaction with oxygen as reaction gas in a dynamic reaction cell (DRC) of a quadrupole ICP-MS. The relative abundance sensitivity of the ICP-MS was studied systematically and the peak tailing originating from 88 Sr on mass 90 u was found to be about 3 x 10 -9 . Detection limits of 4 fg g -1 (0.02 Bq g -1 ) were achieved when measuring Sr solutions containing no Zr. In digested uncontaminated soil samples after matrix separation as well as in a solution of 5 μg g -1 Sr and 50 ng g -1 Zr a detection limit of 0.2 pg g -1 soil (1 Bq g -1 soil) was determined. 90 Sr concentrations in three soil samples collected in the vicinity of the Chernobyl Nuclear Power Plant were 4.66 ± 0.27, 13.48 ± 0.68 and 12.9 ± 1.5 pg g -1 corresponding to specific activities of 23.7 ± 1.3, 68.6 ± 3.5 and 65.6 ± 7.8 Bq g -1 , respectively. The ICP-DRC-MS results were compared to the activities measured earlier by radiometry. Although the ICP-DRC-MS is inferior to commonly used radiometric methods with respect to the achievable minimum detectable activity it represents a time- and cost-effective alternative technique for fast monitoring of high-level 90 Sr contamination in environmental or nuclear industrial samples down to activities of about 1 Bq g -1

  8. Determination of 210Pb and 210Po in soil or rock samples containing refractory matrices

    International Nuclear Information System (INIS)

    Jia Guogang; Torri, Giancarlo

    2007-01-01

    A new method has been developed for determination of 21 Pb and 21 Po in soil or rock samples containing refractory matrices. The samples were first fused with Na 2 CO 3 and Na 2 O 2 at 600 o C for pre-treatment and then 210 Pb and 210 Po were sequentially leached out at 200-250 o C with HNO 3 +HF, HClO 4 and HCl. About 10% of the leaching solution was used for 21 Po determination, carried out by spontaneous deposition of polonium on a silver disc from a weakly acidic solution that contained hydroxylamine hydrochloride, sodium citrate and 209 Po tracer, measurement being made by α-spectrometry. The remains of the leaching solution were used for determination of 21 Pb, conducted by precipitation as sulphate, purification with Na 2 S as PbS in 6 M ammonium acetate, separation from α-emitters by an anion-exchange resin column, source preparation as PbSO 4 , and measurement with a β-counter. The procedure has been checked with two certified IAEA reference materials, showing good agreement with the recommended values. The lower limits of detection for 1 g of analysed soil or rock samples were found to be 0.75 Bq kg -1 for 210 Po and 2.2 Bq kg -1 for 210 Pb. A variety of solid sample species analysed through use of the procedure gave average yields of 90.0±9.8% for 210 Po and 88.4±7.1% for 210 Pb

  9. Colloid mobilization and heavy metal transport in the sampling of soil solution from Duckum soil in South Korea.

    Science.gov (United States)

    Lee, Seyong; Ko, Il-Won; Yoon, In-Ho; Kim, Dong-Wook; Kim, Kyoung-Woong

    2018-03-24

    Colloid mobilization is a significant process governing colloid-associated transport of heavy metals in subsurface environments. It has been studied for the last three decades to understand this process. However, colloid mobilization and heavy metal transport in soil solutions have rarely been studied using soils in South Korea. We investigated the colloid mobilization in a variety of flow rates during sampling soil solutions in sand columns. The colloid concentrations were increased at low flow rates and in saturated regimes. Colloid concentrations increased 1000-fold higher at pH 9.2 than at pH 7.3 in the absence of 10 mM NaCl solution. In addition, those were fourfold higher in the absence than in the presence of the NaCl solution at pH 9.2. It was suggested that the mobility of colloids should be enhanced in porous media under the basic conditions and the low ionic strength. In real field soils, the concentrations of As, Cr, and Pb in soil solutions increased with the increase in colloid concentrations at initial momentarily changed soil water pressure, whereas the concentrations of Cd, Cu, Fe, Ni, Al, and Co lagged behind the colloid release. Therefore, physicochemical changes and heavy metal characteristics have important implications for colloid-facilitated transport during sampling soil solutions.

  10. Radiation hazard indices of soil and water samples in Northern Malaysian Peninsula.

    Science.gov (United States)

    Almayahi, B A; Tajuddin, A A; Jaafar, M S

    2012-11-01

    The radioactivity quantity and quality were determined in soil and water samples in Northern Malaysian Peninsula (NMP) using HPGe spectroscopy and GR-135 spectrometer. The (226)Ra, (232)Th and (40)K concentrations in soil samples are 57±2, 68±4 and 427±17 Bq kg(-1), respectively, whereas in water samples were found to be 2.86±0.79, 3.78±1.73 and 152±12 Bq l(-1), respectively. These concentrations are within those reported from literature in other countries in the world. The radiological hazard indices of the samples were also calculated. The mean values obtained from soil samples are 186 Bq kg(-1), 88 nGy h(-1), 108 μSv y(-1), 0.50 and 0.65 for Radium Equivalent Activity (Ra(eq)), Absorbed Dose Rates (D(R)), Annual Effective Dose Rates (ED), External Hazard Index (H(ex)) and Internal Hazard Index (H(in)) respectively, whereas, for water samples were found to be 20, 10, 13, 0.05 and 0.06, respectively. All the health hazard indices are well below their recommended limits, except in two soil sampling sites which were found to be (*)025 (1.1 H(ex)) and (*)026 (1.1 H(ex), 1.6 H(in)). The calculated and the measured gamma dose rates had a good correlation coefficient, R=0.88. Moreover, the average value radon is 20 (in the range of 7-64) Bq m(-3), a positive correlation (R=0.81) was observed between the (222)Rn and (226)Ra concentrations in samples measured by the SNC continuous radon monitor (model 1029, Sun Nuclear Corporation) and HPGe detector, respectively. Some soils in this study with H(in) and H(ex)samples, therefore, water after processing and filtration is safe and suitable for use in household and industrial purposes. Copyright © 2012 Elsevier Ltd. All rights reserved.

  11. Challenges in TEM sample preparation of solvothermally grown CuInS2 films.

    Science.gov (United States)

    Frank, Anna; Changizi, Rasa; Scheu, Christina

    2018-06-01

    Transmission electron microscopy (TEM) is a widely used tool to characterize materials. The required samples need to be electron transparent which should be achieved without changing the microstructure. This work describes different TEM sample preparation techniques of nanostructured CuInS 2 thin films on fluorine-doped tin oxide substrates, synthesized solvothermally using l-cysteine as sulfur source. Focused ion beam lamellae, conventional cross section samples and scratch samples have been prepared and investigated. It was possible to prepare appropriate samples with each technique, however, each technique brings with it certain advantages and disadvantages. FIB preparation of solvothermally synthesized CuInS 2 suffers from two main drawbacks. First, the whole CuInS 2 layer displays a strongly increased Cu content caused by Cu migration and preferential removal of In. Further, electron diffraction shows the formation of an additional CuS phase after Ga + bombardment. Second, diffraction analysis is complicated by a strong contribution of crystalline Pt introduced during the FIB preparation and penetrating into the porous film surface. The conventional cross sectional CuInS 2 sample also shows a Cu signal enhancement which is caused by contribution of the brass tube material used for embedding. Additionally, Cu particles have been observed inside the CuInS 2 which have been sputtered on the film during preparation. Only the scratch samples allow an almost artefact-free and reliable elemental quantification using energy-dispersive X-ray spectroscopy. However, scratch samples suffer from the drawback that it is not possible to determine the layer thickness, which is possible for both cross sectional preparation techniques. Consequently, it is concluded that the type of sample preparation should be chosen dependent on the required information. A full characterization can only be achieved when the different techniques are combined. Copyright © 2018 Elsevier Ltd. All

  12. Classification of Surface and Deep Soil Samples Using Linear Discriminant Analysis

    International Nuclear Information System (INIS)

    Wasim, M.; Ali, M.; Daud, M.

    2015-01-01

    A statistical analysis was made of the activity concentrations measured in surface and deep soil samples for natural and anthropogenic gamma-emitting radionuclides. Soil samples were obtained from 48 different locations in Gilgit, Pakistan covering about 50 km/sup 2/ areas at an average altitude of 1550 m above sea level. From each location two samples were collected: one from the top soil (2-6 cm) and another from a depth of 6-10 cm. Four radionuclides including /sup 226/Ra, /sup 232/Th, /sup 40/K and /sup 137/Cs were quantified. The data was analyzed using t-test to find out activity concentration difference between the surface and depth samples. At the surface, the median activity concentrations were 23.7, 29.1, 4.6 and 115 Bq kg/sup -1/ for 226Ra, 232Th, 137Cs and 40K respectively. For the same radionuclides, the activity concentrations were respectively 25.5, 26.2, 2.9 and 191 Bq kg/sup -1/ for the depth samples. Principal component analysis (PCA) was applied to explore patterns within the data. A positive significant correlation was observed between the radionuclides /sup 226/Ra and /sup 232/Th. The data from PCA was further utilized in linear discriminant analysis (LDA) for the classification of surface and depth samples. LDA classified surface and depth samples with good predictability. (author)

  13. Automated SEM and TEM sample preparation applied to copper/low k materials

    Science.gov (United States)

    Reyes, R.; Shaapur, F.; Griffiths, D.; Diebold, A. C.; Foran, B.; Raz, E.

    2001-01-01

    We describe the use of automated microcleaving for preparation of both SEM and TEM samples as done by SELA's new MC500 and TEMstation tools. The MC500 is an automated microcleaving tool that is capable of producing cleaves with 0.25 μm accuracy resulting in SEM-ready samples. The TEMstation is capable of taking a sample output from the MC500 (or from SELA's earlier MC200 tool) and producing a FIB ready slice of 25±5 μm, mounted on a TEM-washer and ready for FIB thinning to electron transparency for TEM analysis. The materials selected for the tool set evaluation mainly included the Cu/TaN/HOSP low-k system. The paper is divided into three sections, experimental approach, SEM preparation and analysis of HOSP low-k, and TEM preparation and analysis of Cu/TaN/HOSP low-k samples. For the samples discussed, data is presented to show the quality of preparation provided by these new automated tools.

  14. Study on a pattern classification method of soil quality based on simplified learning sample dataset

    Science.gov (United States)

    Zhang, Jiahua; Liu, S.; Hu, Y.; Tian, Y.

    2011-01-01

    Based on the massive soil information in current soil quality grade evaluation, this paper constructed an intelligent classification approach of soil quality grade depending on classical sampling techniques and disordered multiclassification Logistic regression model. As a case study to determine the learning sample capacity under certain confidence level and estimation accuracy, and use c-means algorithm to automatically extract the simplified learning sample dataset from the cultivated soil quality grade evaluation database for the study area, Long chuan county in Guangdong province, a disordered Logistic classifier model was then built and the calculation analysis steps of soil quality grade intelligent classification were given. The result indicated that the soil quality grade can be effectively learned and predicted by the extracted simplified dataset through this method, which changed the traditional method for soil quality grade evaluation. ?? 2011 IEEE.

  15. Regional soil erosion assessment based on a sample survey and geostatistics

    Directory of Open Access Journals (Sweden)

    S. Yin

    2018-03-01

    Full Text Available Soil erosion is one of the most significant environmental problems in China. From 2010 to 2012, the fourth national census for soil erosion sampled 32 364 PSUs (Primary Sampling Units, small watersheds with the areas of 0.2–3 km2. Land use and soil erosion controlling factors including rainfall erosivity, soil erodibility, slope length, slope steepness, biological practice, engineering practice, and tillage practice for the PSUs were surveyed, and the soil loss rate for each land use in the PSUs was estimated using an empirical model, the Chinese Soil Loss Equation (CSLE. Though the information collected from the sample units can be aggregated to estimate soil erosion conditions on a large scale; the problem of estimating soil erosion condition on a regional scale has not been addressed well. The aim of this study is to introduce a new model-based regional soil erosion assessment method combining a sample survey and geostatistics. We compared seven spatial interpolation models based on the bivariate penalized spline over triangulation (BPST method to generate a regional soil erosion assessment from the PSUs. Shaanxi Province (3116 PSUs in China was selected for the comparison and assessment as it is one of the areas with the most serious erosion problem. Ten-fold cross-validation based on the PSU data showed the model assisted by the land use, rainfall erosivity factor (R, soil erodibility factor (K, slope steepness factor (S, and slope length factor (L derived from a 1 : 10 000 topography map is the best one, with the model efficiency coefficient (ME being 0.75 and the MSE being 55.8 % of that for the model assisted by the land use alone. Among four erosion factors as the covariates, the S factor contributed the most information, followed by K and L factors, and R factor made almost no contribution to the spatial estimation of soil loss. The LS factor derived from 30 or 90 m Shuttle Radar Topography Mission

  16. Experimental Study of Factors Affecting Soil Erodibility

    Science.gov (United States)

    Larionov, G. A.; Bushueva, O. G.; Gorobets, A. V.; Dobrovolskaya, N. G.; Kiryukhina, Z. P.; Krasnov, S. F.; Litvin, L. F.; Maksimova, I. A.; Sudnitsyn, I. I.

    2018-03-01

    The effect of different factors and preparation conditions of monofraction samples from the arable horizon of leached chernozem on soil erodibility and its relationship with soil tensile strength (STS) has been studied. The exposure of samples at 38°C reduces their erodibility by two orders of magnitude. The drying of samples, on the contrary, increases their erodibility. It has been shown that erodibility decreases during the experiment. It has been found that the inoculation of soil with yeast cultures ( Naganishia albida, Lipomyces tetrasporus) reliably increases the STS value in 1.5-1.9 times. The sterile soil is eroded more intensively than the unsterile soil: at 4.9 and 0.3 g/(m2 s), respectively. The drying of soil followed by wetting to the initial water content (30%) has no significant effect on the STS value in almost all experimental treatments.

  17. Polymeric ionic liquid-based portable tip microextraction device for on-site sample preparation of water samples.

    Science.gov (United States)

    Chen, Lei; Pei, Junxian; Huang, Xiaojia; Lu, Min

    2018-06-05

    On-site sample preparation is highly desired because it avoids the transportation of large-volume samples and ensures the accuracy of the analytical results. In this work, a portable prototype of tip microextraction device (TMD) was designed and developed for on-site sample pretreatment. The assembly procedure of TMD is quite simple. Firstly, polymeric ionic liquid (PIL)-based adsorbent was in-situ prepared in a pipette tip. After that, the tip was connected with a syringe which was driven by a bidirectional motor. The flow rates in adsorption and desorption steps were controlled accurately by the motor. To evaluate the practicability of the developed device, the TMD was used to on-site sample preparation of waters and combined with high-performance liquid chromatography with diode array detection to measure trace estrogens in water samples. Under the most favorable conditions, the limits of detection (LODs, S/N = 3) for the target analytes were in the range of 4.9-22 ng/L, with good coefficients of determination. Confirmatory study well evidences that the extraction performance of TMD is comparable to that of the traditional laboratory solid-phase extraction process, but the proposed TMD is more simple and convenient. At the same time, the TMD avoids complicated sampling and transferring steps of large-volume water samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  18. Procedure for plutonium analysis of large (100g) soil and sediment samples

    International Nuclear Information System (INIS)

    Meadows, J.W.T.; Schweiger, J.S.; Mendoza, B.; Stone, R.

    1975-01-01

    A method for the complete dissolution of large soil or sediment samples is described. This method is in routine usage at Lawrence Livermore Laboratory for the analysis of fall-out levels of Pu in soils and sediments. Intercomparison with partial dissolution (leach) techniques shows the complete dissolution method to be superior for the determination of plutonium in a wide variety of environmental samples. (author)

  19. Optimization of Sample Preparation processes of Bone Material for Raman Spectroscopy.

    Science.gov (United States)

    Chikhani, Madelen; Wuhrer, Richard; Green, Hayley

    2018-03-30

    Raman spectroscopy has recently been investigated for use in the calculation of postmortem interval from skeletal material. The fluorescence generated by samples, which affects the interpretation of Raman data, is a major limitation. This study compares the effectiveness of two sample preparation techniques, chemical bleaching and scraping, in the reduction of fluorescence from bone samples during testing with Raman spectroscopy. Visual assessment of Raman spectra obtained at 1064 nm excitation following the preparation protocols indicates an overall reduction in fluorescence. Results demonstrate that scraping is more effective at resolving fluorescence than chemical bleaching. The scraping of skeletonized remains prior to Raman analysis is a less destructive method and allows for the preservation of a bone sample in a state closest to its original form, which is beneficial in forensic investigations. It is recommended that bone scraping supersedes chemical bleaching as the preferred method for sample preparation prior to Raman spectroscopy. © 2018 American Academy of Forensic Sciences.

  20. Magnetic separation techniques in sample preparation for biological analysis: a review.

    Science.gov (United States)

    He, Jincan; Huang, Meiying; Wang, Dongmei; Zhang, Zhuomin; Li, Gongke

    2014-12-01

    Sample preparation is a fundamental and essential step in almost all the analytical procedures, especially for the analysis of complex samples like biological and environmental samples. In past decades, with advantages of superparamagnetic property, good biocompatibility and high binding capacity, functionalized magnetic materials have been widely applied in various processes of sample preparation for biological analysis. In this paper, the recent advancements of magnetic separation techniques based on magnetic materials in the field of sample preparation for biological analysis were reviewed. The strategy of magnetic separation techniques was summarized. The synthesis, stabilization and bio-functionalization of magnetic nanoparticles were reviewed in detail. Characterization of magnetic materials was also summarized. Moreover, the applications of magnetic separation techniques for the enrichment of protein, nucleic acid, cell, bioactive compound and immobilization of enzyme were described. Finally, the existed problems and possible trends of magnetic separation techniques for biological analysis in the future were proposed. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. State of the art in sample preparation for trace element analysis (M1)

    International Nuclear Information System (INIS)

    Barnes, R.M.

    2002-01-01

    Full text: The accelerated capabilities of modern trace element analysis techniques, especially inductively coupled plasma mass spectrometry (ICP-MS), have challenged the sample preparation competence of most laboratories. Exceptional analytical sensitivity, remarkable analysis speed, automated sample presentation, and intelligent sample sequencing of modern spectroscopic instrumentation have lead to demanding requirements for appropriate sample preparation steps needed for ultra trace concentration and speciation measurements. Contamination control, reliable digestion and extraction techniques, presentation of chemical forms, sample matrix management, and intelligent sample processing available today are often inadequate for the most demanding measurements. Some commercial instrumentation provides convenient implementation of well-established contamination control measures, and reagent and container purity are steadily being improved. Direct sample introduction approaches offer alternatives to conventional solution samples, but achieving calibration reliability is difficult. Developing new sample preparation chemistry is especially arduous and rare, yet progress exists in characterizing microwave-assisted reactions. This presentation will describe contemporary targets for modern sample preparation approaches for ultra trace elemental analysis and the likelihood that they can be reasonably achieved. (author)

  2. Quantification of bitumen particles in aerosol and soil samples using HP-GPC

    DEFF Research Database (Denmark)

    Fauser, Patrik; Tjell, Jens Christian; Mosbæk, Hans

    2000-01-01

    A method for identifying and quantifying bitumen particles, generated from the wear of roadway asphalts, in aerosol and soil samples has been developed. Bitumen is found to be the only contributor to airborne particles containing organic molecules with molecular weights larger than 2000 g pr. mol....... These are separated and identified using High Performance Gel Permeation Chromatography (HP-GPC) with fluorescence detection. As an additional detection method Infra Red spectrometry (IR) is employed for selected samples. The methods have been used on aerosol, soil and other samples....

  3. Spatial Variation of Soil Lead in an Urban Community Garden: Implications for Risk-Based Sampling.

    Science.gov (United States)

    Bugdalski, Lauren; Lemke, Lawrence D; McElmurry, Shawn P

    2014-01-01

    Soil lead pollution is a recalcitrant problem in urban areas resulting from a combination of historical residential, industrial, and transportation practices. The emergence of urban gardening movements in postindustrial cities necessitates accurate assessment of soil lead levels to ensure safe gardening. In this study, we examined small-scale spatial variability of soil lead within a 15 × 30 m urban garden plot established on two adjacent residential lots located in Detroit, Michigan, USA. Eighty samples collected using a variably spaced sampling grid were analyzed for total, fine fraction (less than 250 μm), and bioaccessible soil lead. Measured concentrations varied at sampling scales of 1-10 m and a hot spot exceeding 400 ppm total soil lead was identified in the northwest portion of the site. An interpolated map of total lead was treated as an exhaustive data set, and random sampling was simulated to generate Monte Carlo distributions and evaluate alternative sampling strategies intended to estimate the average soil lead concentration or detect hot spots. Increasing the number of individual samples decreases the probability of overlooking the hot spot (type II error). However, the practice of compositing and averaging samples decreased the probability of overestimating the mean concentration (type I error) at the expense of increasing the chance for type II error. The results reported here suggest a need to reconsider U.S. Environmental Protection Agency sampling objectives and consequent guidelines for reclaimed city lots where soil lead distributions are expected to be nonuniform. © 2013 Society for Risk Analysis.

  4. The effect of sample preparation methods on glass performance

    International Nuclear Information System (INIS)

    Oh, M.S.; Oversby, V.M.

    1990-01-01

    A series of experiments was conducted using SRL 165 synthetic waste glass to investigate the effects of surface preparation and leaching solution composition on the alteration of the glass. Samples of glass with as-cast surfaces produced smooth reaction layers and some evidence for precipitation of secondary phases from solution. Secondary phases were more abundant in samples reacted in deionized water than for those reacted in a silicate solution. Samples with saw-cut surfaces showed a large reduction in surface roughness after 7 days of reaction in either solution. Reaction in silicate solution for up to 91 days produced no further change in surface morphology, while reaction in DIW produced a spongy surface that formed the substrate for further surface layer development. The differences in the surface morphology of the samples may create microclimates that control the details of development of alteration layers on the glass; however, the concentrations of elements in leaching solutions show differences of 50% or less between samples prepared with different surface conditions for tests of a few months duration. 6 refs., 7 figs., 1 tab

  5. Preparation of Cytology Samples: Tricks of the Trade.

    Science.gov (United States)

    Moore, A Russell

    2017-01-01

    General principles and techniques for collection, preparation, and staining of cytologic samples in the general practice setting are reviewed. Tips for collection of digital images are also discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

  6. Sample preparation procedures utilized in microbial metabolomics: An overview.

    Science.gov (United States)

    Patejko, Małgorzata; Jacyna, Julia; Markuszewski, Michał J

    2017-02-01

    Bacteria are remarkably diverse in terms of their size, structure and biochemical properties. Due to this fact, it is hard to develop a universal method for handling bacteria cultures during metabolomic analysis. The choice of suitable processing methods constitutes a key element in any analysis, because only appropriate selection of procedures may provide accurate results, leading to reliable conclusions. Because of that, every analytical experiment concerning bacteria requires individually and very carefully planned research methodology. Although every study varies in terms of sample preparation, there are few general steps to follow while planning experiment, like sampling, separation of cells from growth medium, stopping their metabolism and extraction. As a result of extraction, all intracellular metabolites should be washed out from cell environment. What is more, extraction method utilized cannot cause any chemical decomposition or degradation of the metabolome. Furthermore, chosen extraction method should correlate with analytical technique, so it will not disturb or prolong following sample preparation steps. For those reasons, we observe a need to summarize sample preparation procedures currently utilized in microbial metabolomic studies. In the presented overview, papers concerning analysis of extra- and intracellular metabolites, published over the last decade, have been discussed. Presented work gives some basic guidelines that might be useful while planning experiments in microbial metabolomics. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Results of Soil Vapor Sampling at SA 6, McClellan Air Force Base, California

    National Research Council Canada - National Science Library

    1998-01-01

    ...) and total petroleum hydrocarbon (TPH) contamination in site soil. The soil vapor sampling event was performed in accordance with the Final Sampling and Analysis Plan to Support Recommendation for No Further Investigation at SA 6 (Parsons ES, 1998...

  8. Estimation of radon concentration in soil and groundwater samples of Northern Rajasthan, India

    International Nuclear Information System (INIS)

    Mittal, Sudhir; Asha Rani; Mehra, Rohit

    2015-01-01

    In the present investigation, analysis of radon concentration in 20 water and soil samples collected from different locations of Bikaner and Jhunjhunu districts of Rajasthan, India has been carried out by using RAD7 an electronic Radon detector. The water samples are taken from hand pumps and tube wells having depths ranging from 50 to 600 feet. All the soil gas measurements have been carried out at 100 cm depth. The measured radon concentration in water samples lies in the range from 0.50 to 22 Bq l -1 with the mean value of 4.42 Bq l -1 . Only in one water sample radon concentration is found to be higher than the safe limit of 11 Bq l -1 recommended US Environmental Protection Agency (USEPA, 1991). The measured value of radon concentration in all ground water samples is within the safe limit from 4 to 40 Bq l -1 recommended by United Nations Scientific Committee on the Effects of Atomic Radiation (UNSCEAR, 2008). The total annual effective dose estimated due to radon concentration in water ranges from 1.37 to 60 μSV y -1 with the mean value of 12.08 μSV y -1 . The total annual effective dose from all locations of our studied area is found to be well within the safe limit 0.1 mSv y -1 recommended by World Health Organization (WHO, 2004) and European Council (ED, 1998). Radon measurement in soil samples varies from 941 to 10050 Bq m -3 with the mean value of 4561 Bq m -3 , The radon concentration observed from the soil samples from our study area lies within the range reported by other investigators. Moreover a positive correlation of radon concentration in water with soil samples has been observed. It was observed that the soil and water of Bikaner and Jhunjhunu districts are suitable for drinking and construction purpose without posing any health hazard. (author)

  9. Random sampling or geostatistical modelling? Choosing between design-based and model-based sampling strategies for soil (with discussion)

    NARCIS (Netherlands)

    Brus, D.J.; Gruijter, de J.J.

    1997-01-01

    Classical sampling theory has been repeatedly identified with classical statistics which assumes that data are identically and independently distributed. This explains the switch of many soil scientists from design-based sampling strategies, based on classical sampling theory, to the model-based

  10. Sample preparation techniques for (p, X) spectrometry

    International Nuclear Information System (INIS)

    Whitehead, N.E.

    1985-01-01

    Samples are ashed at low temperature, using oxygen plasma; a rotary evaporator, and freeze drying speeded up the ashing. The new design of apparatus manufactured was only 10 watt but was as efficient as a 200 watt commercial machine; a circuit diagram is included. Samples of hair and biopsy samples of skin were analysed by the technique. A wool standard was prepared for interlaboratory comparison exercises. It was based on New Zealand merino sheep wool and was 2.9 kg in weight. A washing protocol was developed, which preserves most of the trace element content. The wool was ground in liquid nitrogen using a plastic pestle and beaker, driven by a rotary drill press. (author)

  11. Rapid separation method for {sup 237}Np and Pu isotopes in large soil samples

    Energy Technology Data Exchange (ETDEWEB)

    Maxwell, Sherrod L., E-mail: sherrod.maxwell@srs.go [Savannah River Nuclear Solutions, LLC, Building 735-B, Aiken, SC 29808 (United States); Culligan, Brian K.; Noyes, Gary W. [Savannah River Nuclear Solutions, LLC, Building 735-B, Aiken, SC 29808 (United States)

    2011-07-15

    A new rapid method for the determination of {sup 237}Np and Pu isotopes in soil and sediment samples has been developed at the Savannah River Site Environmental Lab (Aiken, SC, USA) that can be used for large soil samples. The new soil method utilizes an acid leaching method, iron/titanium hydroxide precipitation, a lanthanum fluoride soil matrix removal step, and a rapid column separation process with TEVA Resin. The large soil matrix is removed easily and rapidly using these two simple precipitations with high chemical recoveries and effective removal of interferences. Vacuum box technology and rapid flow rates are used to reduce analytical time.

  12. Radioactivity measurements of soil samples in the Region Vranje (Bratoselce Village) for the period 2001-2004

    International Nuclear Information System (INIS)

    Eremic-savkovic, M.; Pantelic, G.; Tanaskovic, I.; Vuletic, V.; Javorina, L.

    2006-01-01

    Systematic examination of radioactive contamination of soil samples was established at the Institute for Occupational and Radiological Health. With the bombing of our country (Spring 1999) the monitoring of radioactivity has changed. We also measured the activities of uranium and it descendants. This paper presents the results of radioactivity monitoring of the soil in small area 700 m near village Bratoselce in region Vranje during the period 2001 - 2004. From 2001 to 2004, we collected different samples from this fenced area as well as outside this area assuming not to be contaminated, before, during and after decontamination. Some soil samples were made as a mix of small samples from a large area of location. Other samples were taken at the points formerly designated as contaminated or from shell-craters seen on the fenced area surface. All samples were analyzed by gamma spectrometry and measurements of alpha and beta activity. On the basis of measurements of soil activities, analysis of 238 U and 235 U, as well as in comparison with natural activity ratio being 21.4, it may be concluded that depleted uranium contamination was present both in the fenced area and outside it, because this ratio in the samples of soil was found to be 34 to 73. Natural activity in soil samples was slightly higher in relation to mean soil activity in Serbia. (authors)

  13. Can The Pore Scale Geometry Explain Soil Sample Scale Hydrodynamic Properties?

    Directory of Open Access Journals (Sweden)

    Sarah Smet

    2018-04-01

    Full Text Available For decades, the development of new visualization techniques has brought incredible insights into our understanding of how soil structure affects soil function. X-ray microtomography is a technique often used by soil scientists but challenges remain with the implementation of the procedure, including how well the samples represent the uniqueness of the pore network and structure and the systemic compromise between sample size and resolution. We, therefore, chose to study soil samples from two perspectives: a macroscopic scale with hydrodynamic characterization and a microscopic scale with structural characterization through the use of X-ray microtomography (X-ray μCT at a voxel size of 21.53 μm3 (resampled at 433 μm3. The objective of this paper is to unravel the relationships between macroscopic soil properties and microscopic soil structure. The 24 samples came from an agricultural field (Cutanic Luvisol and the macroscopic hydrodynamic properties were determined using laboratory measurements of the saturated hydraulic conductivity (Ks, air permeability (ka, and retention curves (SWRC. The X-ray μCT images were segmented using a global method and multiple microscopic measurements were calculated. We used Bayesian statistics to report the credible correlation coefficients and linear regressions models between macro- and microscopic measurements. Due to the small voxel size, we observed unprecedented relationships, such as positive correlations between log(Ks and a μCT global connectivity indicator, the fractal dimension of the μCT images or the μCT degree of anisotropy. The air permeability measured at a water matric potential of −70 kPa was correlated to the average coordination number and the X-ray μCT porosity, but was best explained by the average pore volume of the smallest pores. Continuous SWRC were better predicted near saturation when the pore-size distributions calculated on the X-ray μCT images were used as model input. We

  14. Assessing NIR & MIR Spectral Analysis as a Method for Soil C Estimation Across a Network of Sampling Sites

    Science.gov (United States)

    Spencer, S.; Ogle, S.; Borch, T.; Rock, B.

    2008-12-01

    Monitoring soil C stocks is critical to assess the impact of future climate and land use change on carbon sinks and sources in agricultural lands. A benchmark network for soil carbon monitoring of stock changes is being designed for US agricultural lands with 3000-5000 sites anticipated and re-sampling on a 5- to10-year basis. Approximately 1000 sites would be sampled per year producing around 15,000 soil samples to be processed for total, organic, and inorganic carbon, as well as bulk density and nitrogen. Laboratory processing of soil samples is cost and time intensive, therefore we are testing the efficacy of using near-infrared (NIR) and mid-infrared (MIR) spectral methods for estimating soil carbon. As part of an initial implementation of national soil carbon monitoring, we collected over 1800 soil samples from 45 cropland sites in the mid-continental region of the U.S. Samples were processed using standard laboratory methods to determine the variables above. Carbon and nitrogen were determined by dry combustion and inorganic carbon was estimated with an acid-pressure test. 600 samples are being scanned using a bench- top NIR reflectance spectrometer (30 g of 2 mm oven-dried soil and 30 g of 8 mm air-dried soil) and 500 samples using a MIR Fourier-Transform Infrared Spectrometer (FTIR) with a DRIFT reflectance accessory (0.2 g oven-dried ground soil). Lab-measured carbon will be compared to spectrally-estimated carbon contents using Partial Least Squares (PLS) multivariate statistical approach. PLS attempts to develop a soil C predictive model that can then be used to estimate C in soil samples not lab-processed. The spectral analysis of soil samples either whole or partially processed can potentially save both funding resources and time to process samples. This is particularly relevant for the implementation of a national monitoring network for soil carbon. This poster will discuss our methods, initial results and potential for using NIR and MIR spectral

  15. Natural radioactivity in soils from Piracicaba, SP (Brazil)

    International Nuclear Information System (INIS)

    Oliveira, H. de.

    1988-01-01

    Using high resolution gamma spectrometry, the specific radioactivity of soils and rocks from Piracicaba, SP (Brazil) was determined. For this purpose, the Ra, Th and Ac natural series and some other nuclides such as sup(40)K and sup(137)Cs were considered. Soil samples representing the main Soil Groups were collected at 60-cm depth. Typical rock samples were also collected. After initial sample preparation, the sealed sample were allowed to rest until reaching the conditions approaching the secular equilibrium. Thereafter, counting was carried out, peak areas being the measurements basis. The mean ponderated values for soil specific activity were 24.1 and 34.8 Bq.kg sup(-1) for the sup(226)Ra and sup(232)Th, respectively. (author)

  16. Portable Automation of Static Chamber Sample Collection for Quantifying Soil Gas Flux

    Energy Technology Data Exchange (ETDEWEB)

    Davis, Morgan P.; Groh, Tyler A.; Parkin, Timothy B.; Williams, Ryan J.; Isenhart, Thomas M.; Hofmockel, Kirsten S.

    2018-01-01

    Quantification of soil gas flux using the static chamber method is labor intensive. The number of chambers that can be sampled is limited by the spacing between chambers and the availability of trained research technicians. An automated system for collecting gas samples from chambers in the field would eliminate the need for personnel to return to the chamber during a flux measurement period and would allow a single technician to sample multiple chambers simultaneously. This study describes Chamber Automated Sampling Equipment (FluxCASE) to collect and store chamber headspace gas samples at assigned time points for the measurement of soil gas flux. The FluxCASE design and operation is described, and the accuracy and precision of the FluxCASE system is evaluated. In laboratory measurements of nitrous oxide (N2O), carbon dioxide (CO2), and methane (CH4) concentrations of a standardized gas mixture, coefficients of variation associated with automated and manual sample collection were comparable, indicating no loss of precision. In the field, soil gas fluxes measured from FluxCASEs were in agreement with manual sampling for both N2O and CO2. Slopes of regression equations were 1.01 for CO2 and 0.97 for N2O. The 95% confidence limits of the slopes of the regression lines included the value of one, indicating no bias. Additionally, an expense analysis found a cost recovery ranging from 0.6 to 2.2 yr. Implementing the FluxCASE system is an alternative to improve the efficiency of the static chamber method for measuring soil gas flux while maintaining the accuracy and precision of manual sampling.

  17. Traceability and measurement uncertainty in sample preparation (W5)

    International Nuclear Information System (INIS)

    Wegscheider, W.; Walner, U.; Moser, J.

    2002-01-01

    Full text: Very few chemical measurements are being made directly on the object of interest and sample preparation is thus the rule rather than the exception in daily practice. Unfortunately the operations undertaken in the course of sample preparation are prone to rendering a sample useless for the purpose of interpreting a measurement performed on it, as it might not represent the original and relevant status any longer. Sample preparation along with sampling itself constitutes therefore a procedure that leads to a loss of representation of the original specimen or population. On the other hand it is also not sufficient to confine aspects of traceability and measurement uncertainty to the ultimate measurement, as the key purpose of measuring is to supply adequate data for some kind of decision, be it in production, in health, in the environment, or indeed in any other circumstance. These considerations have led to severe confusion in the community as to what traceability really means in chemistry. CITAC and EURACHEM have only recently issued a preliminary document that clarifies these issues and gives a firm handle on the future development of quality assurance in analytical chemistry. In this talk it will be attempted to outline the general ideas and procedures that lead to traceability of analytical chemical results accompanied by valid statements of their uncertainty. It will be argued that the central element in achieving these goals is a well-designed validation study that frequently goes beyond those requirements currently laid out in official documents. (author)

  18. Determination of naturally occurring radionuclides in soil samples of Ayranci, Turkey

    Science.gov (United States)

    Agar, Osman; Eke, Canel; Boztosun, Ismail; Emin Korkmaz, M.

    2015-04-01

    The specific activity, radiation hazard index and the annual effective dose of the naturally occurring radioactive elements (238U, 232Th and 40K) were determined in soil samples collected from 12 different locations in Ayranci region by using a NaI(Tl) gamma-ray spectrometer. The measured activity concentrations of the natural radionuclides in studied soil samples were compared with the corresponding results of different countries and the internationally reported values. From the analysis, it is found that these materials may be safely used as construction materials and do not pose significant radiation hazards.

  19. Mechanical Conversion for High-Throughput TEM Sample Preparation

    International Nuclear Information System (INIS)

    Kendrick, Anthony B; Moore, Thomas M; Zaykova-Feldman, Lyudmila

    2006-01-01

    This paper presents a novel method of direct mechanical conversion from lift-out sample to TEM sample holder. The lift-out sample is prepared in the FIB using the in-situ liftout Total Release TM method. The mechanical conversion is conducted using a mechanical press and one of a variety of TEM coupons, including coupons for both top-side and back-side thinning. The press joins a probe tip point with attached TEM sample to the sample coupon and separates the complete assembly as a 3mm diameter TEM grid, compatible with commercially available TEM sample holder rods. This mechanical conversion process lends itself well to the high through-put requirements of in-line process control and to materials characterization labs where instrument utilization and sample security are critically important

  20. Preparative yield and properties of humic acids obtained by sequential alkaline extractions

    Science.gov (United States)

    Kholodov, V. A.; Yaroslavtseva, N. V.; Konstantinov, A. I.; Perminova, I. V.

    2015-10-01

    The preparative yield, composition, and structure of humic acids obtained by sequential alkaline extractions from two soils (a soddy-podzolic soil under forest and a typical chernozem in treatment with permanent black fallow of a long-term experiment since 1964) have been studied. The preparative yield of humic acids from the first extraction is 0.40 and 0.94% for the soddy-podzolic soil (Retisols) and the chernozem, respectively. The preparative yield from the second extraction is lower by several times, and the yield from the third extraction is lower by an order of magnitude. The study of the obtained preparations by elemental analysis, gel-permeation chromatography, and 13C NMR spectroscopy has shown insignificant changes in the elemental, molecular-weight, and structural-group composition of humic acids among the extractions. It has been supposed that this is related to the soil features: typical climatic factors for the formation of soil subtype in the case of soddy-podzolic soil and the land use in the long-term experiment in the case of typical chernozem. It has been concluded that that a single extraction is sufficient for the separation of humic acids and the preparation of a representative sample.

  1. A study for natural radioactivity levels in some soil samples using gamma spectrometry

    International Nuclear Information System (INIS)

    Mohamed, Yousif Hassab El Rasoul

    1997-05-01

    The purpose of this study was to investigate a few selected soil samples and to study their natural radioactivity using gamma spectrometry. The first sample was a rock phosphate from Nuba mountains region which is being considered as a low cost fertilizer. Another sample came from Miri lake area (Nuba mountains) which is known to have elevated natural radioactivity level. The other four samples came from different other regions in Sudan for comparison. The idea was to identify the radioactive nuclides present in these soil samples, to trace their sources and to determine the activity present in them. (Author)

  2. 40 CFR 205.171-2 - Test exhaust system sample selection and preparation.

    Science.gov (United States)

    2010-07-01

    ... Systems § 205.171-2 Test exhaust system sample selection and preparation. (a)(1) Exhaust systems... 40 Protection of Environment 24 2010-07-01 2010-07-01 false Test exhaust system sample selection and preparation. 205.171-2 Section 205.171-2 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY...

  3. Droplet Size-Aware and Error-Correcting Sample Preparation Using Micro-Electrode-Dot-Array Digital Microfluidic Biochips.

    Science.gov (United States)

    Li, Zipeng; Lai, Kelvin Yi-Tse; Chakrabarty, Krishnendu; Ho, Tsung-Yi; Lee, Chen-Yi

    2017-12-01

    Sample preparation in digital microfluidics refers to the generation of droplets with target concentrations for on-chip biochemical applications. In recent years, digital microfluidic biochips (DMFBs) have been adopted as a platform for sample preparation. However, there remain two major problems associated with sample preparation on a conventional DMFB. First, only a (1:1) mixing/splitting model can be used, leading to an increase in the number of fluidic operations required for sample preparation. Second, only a limited number of sensors can be integrated on a conventional DMFB; as a result, the latency for error detection during sample preparation is significant. To overcome these drawbacks, we adopt a next generation DMFB platform, referred to as micro-electrode-dot-array (MEDA), for sample preparation. We propose the first sample-preparation method that exploits the MEDA-specific advantages of fine-grained control of droplet sizes and real-time droplet sensing. Experimental demonstration using a fabricated MEDA biochip and simulation results highlight the effectiveness of the proposed sample-preparation method.

  4. Guidance for Soil Sampling for Energetics and Metals

    Science.gov (United States)

    2011-10-01

    studies have measured the persistence of HE in the field. Radtke et al. (2002) sampled surface soils at an explosives testing area that had not been...in Eagle River Flats, Alaska: The Role of Munitions Residues. CRREL Report CR-92-5. Radtke C. W., D. Gianotto, and F. F. Roberto. 2002. Effects of

  5. Integration of electromagnetic induction sensor data in soil sampling scheme optimization using simulated annealing.

    Science.gov (United States)

    Barca, E; Castrignanò, A; Buttafuoco, G; De Benedetto, D; Passarella, G

    2015-07-01

    Soil survey is generally time-consuming, labor-intensive, and costly. Optimization of sampling scheme allows one to reduce the number of sampling points without decreasing or even increasing the accuracy of investigated attribute. Maps of bulk soil electrical conductivity (EC a ) recorded with electromagnetic induction (EMI) sensors could be effectively used to direct soil sampling design for assessing spatial variability of soil moisture. A protocol, using a field-scale bulk EC a survey, has been applied in an agricultural field in Apulia region (southeastern Italy). Spatial simulated annealing was used as a method to optimize spatial soil sampling scheme taking into account sampling constraints, field boundaries, and preliminary observations. Three optimization criteria were used. the first criterion (minimization of mean of the shortest distances, MMSD) optimizes the spreading of the point observations over the entire field by minimizing the expectation of the distance between an arbitrarily chosen point and its nearest observation; the second criterion (minimization of weighted mean of the shortest distances, MWMSD) is a weighted version of the MMSD, which uses the digital gradient of the grid EC a data as weighting function; and the third criterion (mean of average ordinary kriging variance, MAOKV) minimizes mean kriging estimation variance of the target variable. The last criterion utilizes the variogram model of soil water content estimated in a previous trial. The procedures, or a combination of them, were tested and compared in a real case. Simulated annealing was implemented by the software MSANOS able to define or redesign any sampling scheme by increasing or decreasing the original sampling locations. The output consists of the computed sampling scheme, the convergence time, and the cooling law, which can be an invaluable support to the process of sampling design. The proposed approach has found the optimal solution in a reasonable computation time. The

  6. Phosphatase activity in Antarctica soil samples as a biosignature of extant life

    Science.gov (United States)

    Sato, Shuji; Itoh, Yuki; Takano, Yoshinori; Fukui, Manabu; Kaneko, Takeo; Kobayashi, Kensei

    Microbial activities have been detected in such extreme terrestrial environments as deep lithosphere, a submarine hydrothermal systems, stratosphere, and Antarctica. Microorganisms have adapted to such harsh environments by evolving their biomolecules. Some of these biomolecules such as enzymes might have different characteristics from those of organisms in ordinary environments. Many biosignatures (or biomarkers) have been proposed to detect microbial activities in such extreme environments. A number of techniques are proposed to evaluate biological activities in extreme environments including cultivation methods, assay of metabolism, and analysis of bioorganic compounds like amino acids and DNA. Enzyme activities are useful signature of extant life in extreme environments. Among many enzymes, phosphatase could be a good indicator of biological activities, since phosphate esters are essential for all the living terrestrial organisms. In addition, alkaline phosphatase is known as a typical zinc-containing metalloenzyme and quite stable in environments. We analyzed phosphatase activities in Antarctica soil samples to see whether they can be used as biosignatures for extant life. In addition, we characterized phosphatases extracted from the Antarctica soil samples, and compared with those obtained from other types of environments. Antarctica surface environments are quite severe environments for life since it is extremely cold and dry and exposed to strong UV and cosmic rays. We tried to evaluate biological activities in Antarctica by measuring phosphatase activities. Surface soil samples are obtained at the Sites 1-8 near Showa Base in Antarctica during the 47th Japan Antarctic exploration mission in 2005-6. Activities of acid phosphatase (ACP) and alkaline phosphatase (ALP) are measured spectrophotometrically after mixing the powdered sample and p-nitrophenyl phosphate solution (pH 6.5 for ACP, pH 8.0 for ALP). ALP was characterized after extraction from soils with

  7. Automated Blood Sample Preparation Unit (ABSPU) for Portable Microfluidic Flow Cytometry.

    Science.gov (United States)

    Chaturvedi, Akhil; Gorthi, Sai Siva

    2017-02-01

    Portable microfluidic diagnostic devices, including flow cytometers, are being developed for point-of-care settings, especially in conjunction with inexpensive imaging devices such as mobile phone cameras. However, two pervasive drawbacks of these have been the lack of automated sample preparation processes and cells settling out of sample suspensions, leading to inaccurate results. We report an automated blood sample preparation unit (ABSPU) to prevent blood samples from settling in a reservoir during loading of samples in flow cytometers. This apparatus automates the preanalytical steps of dilution and staining of blood cells prior to microfluidic loading. It employs an assembly with a miniature vibration motor to drive turbulence in a sample reservoir. To validate performance of this system, we present experimental evidence demonstrating prevention of blood cell settling, cell integrity, and staining of cells prior to flow cytometric analysis. This setup is further integrated with a microfluidic imaging flow cytometer to investigate cell count variability. With no need for prior sample preparation, a drop of whole blood can be directly introduced to the setup without premixing with buffers manually. Our results show that integration of this assembly with microfluidic analysis provides a competent automation tool for low-cost point-of-care blood-based diagnostics.

  8. A soil washing pilot plant for removing petroleum hydrocarbons from contaminated soils

    International Nuclear Information System (INIS)

    Toor, I.A.; Roehrig, G.R.

    1992-01-01

    A soil washing pilot plant was built and tested for its ability to remove petroleum hydrocarbons from certain soils. The ITEX soil washing pilot plant is a trailer mountable mobile unit which has a washing capacity of two tons per hour of contaminated soils. A benchscale study was carried out prior to the fabrication of the pilot plant. The first sample was contaminated with diesel fuel while the second sample was contaminated with crude oil. Various nonionic, cationic and anionic cleaning agents were evaluated for their ability to remove petroleum hydrocarbons from these materials. The nonionic cleaning agents were more successful in cleaning the soils in general. The ultimate surfactant choice was based on several factors including cost, biodegradability, cleaning efficiency and other technical considerations. The soil samples were characterized in terms of their particle size distributions. Commercial diesel fuel was carefully mixed in this sand to prepare a representative sample for the pilot plant study. Two pilot runs were made using this material. A multistage washing study was also conducted in the laboratory which indicates that the contamination level can be reduced to 100 ppm using only four stages. Because the pilot plant washing efficiency is twice as high, it is believed that ultimate contamination levels can be reduced to lower levels using the same number of stages. However, this hypothesis has not been demonstrated to date

  9. Soil analysis. Modern instrumental technique

    International Nuclear Information System (INIS)

    Smith, K.A.

    1993-01-01

    This book covers traditional methods of analysis and specialist monographs on individual instrumental techniques, which are usually not written with soil or plant analysis specifically in mind. The principles of the techniques are combined with discussions of sample preparation and matrix problems, and critical reviews of applications in soil science and related disciplines. Individual chapters are processed separately for inclusion in the appropriate data bases

  10. Error Analysis of Ceramographic Sample Preparation for Coating Thickness Measurement of Coated Fuel Particles

    International Nuclear Information System (INIS)

    Liu Xiaoxue; Li Ziqiang; Zhao Hongsheng; Zhang Kaihong; Tang Chunhe

    2014-01-01

    The thicknesses of four coatings of HTR coated fuel particle are very important parameters. It is indispensable to control the thickness of four coatings of coated fuel particles for the safety of HTR. A measurement method, ceramographic sample-microanalysis method, to analyze the thickness of coatings was developed. During the process of ceramographic sample-microanalysis, there are two main errors, including ceramographic sample preparation error and thickness measurement error. With the development of microscopic techniques, thickness measurement error can be easily controlled to meet the design requirements. While, due to the coated particles are spherical particles of different diameters ranged from 850 to 1000μm, the sample preparation process will introduce an error. And this error is different from one sample to another. It’s also different from one particle to another in the same sample. In this article, the error of the ceramographic sample preparation was calculated and analyzed. Results show that the error introduced by sample preparation is minor. The minor error of sample preparation guarantees the high accuracy of the mentioned method, which indicates this method is a proper method to measure the thickness of four coatings of coated particles. (author)

  11. Soil Characterization by Large Scale Sampling of Soil Mixed with Buried Construction Debris at a Former Uranium Fuel Fabrication Facility

    International Nuclear Information System (INIS)

    Nardi, A.J.; Lamantia, L.

    2009-01-01

    Recent soil excavation activities on a site identified the presence of buried uranium contaminated building construction debris. The site previously was the location of a low enriched uranium fuel fabrication facility. This resulted in the collection of excavated materials from the two locations where contaminated subsurface debris was identified. The excavated material was temporarily stored in two piles on the site until a determination could be made as to the appropriate disposition of the material. Characterization of the excavated material was undertaken in a manner that involved the collection of large scale samples of the excavated material in 1 cubic meter Super Sacks. Twenty bags were filled with excavated material that consisted of the mixture of both the construction debris and the associated soil. In order to obtain information on the level of activity associated with the construction debris, ten additional bags were filled with construction debris that had been separated, to the extent possible, from the associated soil. Radiological surveys were conducted of the resulting bags of collected materials and the soil associated with the waste mixture. The 30 large samples, collected as bags, were counted using an In-Situ Object Counting System (ISOCS) unit to determine the average concentration of U-235 present in each bag. The soil fraction was sampled by the collection of 40 samples of soil for analysis in an on-site laboratory. A fraction of these samples were also sent to an off-site laboratory for additional analysis. This project provided the necessary soil characterization information to allow consideration of alternate options for disposition of the material. The identified contaminant was verified to be low enriched uranium. Concentrations of uranium in the waste were found to be lower than the calculated site specific derived concentration guideline levels (DCGLs) but higher than the NRC's screening values. The methods and results are presented

  12. Solid Phase Microextraction (SPME in Determination of Pesticide Residues in Soil Samples

    Directory of Open Access Journals (Sweden)

    Rada Đurović

    2011-01-01

    Full Text Available The basic principles and application possibilities of the methods based on solid phase microextraction (SPME in the analysis of pesticide residues in soil samples are presented in the paper. The most important experimental parameters which affect SPME efficacy inpesticide determination (type and thickness of microextraction fiber, duration of microextraction,temperature at which it is conducted, effect of addition of salts (the effect of efflorescence,temperature and time of desorption, the choice of optimal solvent for pesticide exctraction from the soil and the optimal number of extraction steps, as well as general guidelines for their optimization are also shown. In the end, current applications of SPMEmethods in the analysis of pesticide residues in soil samples are presented.

  13. Miniaturizing EM Sample Preparation: Opportunities, Challenges, and "Visual Proteomics".

    Science.gov (United States)

    Arnold, Stefan A; Müller, Shirley A; Schmidli, Claudio; Syntychaki, Anastasia; Rima, Luca; Chami, Mohamed; Stahlberg, Henning; Goldie, Kenneth N; Braun, Thomas

    2018-03-01

    This review compares and discusses conventional versus miniaturized specimen preparation methods for transmission electron microscopy (TEM). The progress brought by direct electron detector cameras, software developments and automation have transformed transmission cryo-electron microscopy (cryo-EM) and made it an invaluable high-resolution structural analysis tool. In contrast, EM specimen preparation has seen very little progress in the last decades and is now one of the main bottlenecks in cryo-EM. Here, we discuss the challenges faced by specimen preparation for single particle EM, highlight current developments, and show the opportunities resulting from the advanced miniaturized and microfluidic sample grid preparation methods described, such as visual proteomics and time-resolved cryo-EM studies. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Optimized preparation of urine samples for two-dimensional electrophoresis and initial application to patient samples

    DEFF Research Database (Denmark)

    Lafitte, Daniel; Dussol, Bertrand; Andersen, Søren

    2002-01-01

    OBJECTIVE: We optimized of the preparation of urinary samples to obtain a comprehensive map of urinary proteins of healthy subjects and then compared this map with the ones obtained with patient samples to show that the pattern was specific of their kidney disease. DESIGN AND METHODS: The urinary...

  15. Development and Application of Immunoaffinity Chromatography for Coplanar PCBs in Soil and Sediment

    Science.gov (United States)

    An immunoaffinity chromatography (IAC) column was developed as a simple cleanup procedure for preparing environmental samples for analysis of polychlorinated biphenyls (PCBs). Soil and sediment samples were prepared using pressurized liquid extraction (PLE), followed by the IAC c...

  16. 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.

  17. Environmental monitoring of fluoride emissions using precipitation, dust, plant and soil samples

    International Nuclear Information System (INIS)

    Franzaring, J.; Hrenn, H.; Schumm, C.; Klumpp, A.; Fangmeier, A.

    2006-01-01

    A pollution gradient was observed in precipitation, plants and soils sampled at different locations around a fluoride producing chemical plant in Germany. In all samples the influence of emissions was discernible up to a distance of 500 m from the plant. However, fluoride concentrations in plant bioindicators (leaves of birch and black berry) and in bulk precipitation showed a more pronounced relationship with the distance from the source than fluoride concentrations in soil. Vegetables sampled in the vicinity of the plant also had elevated concentrations of fluoride, but only the consumption of larger quantities of this material would lead to exceedances of recommended daily F-intake. The present study did not indicate the existence of low phytotoxicity thresholds for fluoride in the plant species used in the study. Even at very high fluoride concentrations in leaf tissue (963 ppm) plants did not show injury due to HF. Dust sampling downwind of the chemical plant confirmed that particulate fluoride was of minor importance in the study area. - A pronounced pollution gradient was observed in precipitation, plants and soils sampled at different locations around a fluoride emitting chemical plant in Germany

  18. Analysis of soils by glow discharge mass spectrometry

    International Nuclear Information System (INIS)

    Duckworth, D.C.; Barshick, C.M.; Smith, D.H.

    1993-01-01

    The analysis of soils by conventional solution-based techniques, such as inductively coupled plasma and thermal ionization mass spectrometry, is complicated by the need for sample dissolution or the combination of a solids atomizer with an auxiliary ionization source. Since time is an important consideration in waste remediation, there exists a need for a method of rapidly analysing many soil samples with little sample preparation; glow discharge mass spectrometry (GDMS) has the potential to meet this need. Because GDMS is a bulk solids technique, sample preparation is simplified in comparison to other methods. Even with the most difficult samples (geological materials, such as soils and volcanic rock), all that is required is grinding, drying and mixing with a conducting host material prior to electrode formation. As a first test of GDMS for soil analysis, a National Institute of Standards and Technology (NIST) Standard Reference Material (SRM) was analysed by direct current GDMS. Fifty-one elements were quantified from a single cathode using ion beam ratios and ''standard'' relative elemental sensitivity factors (RSF). Average errors for the suite of elements were less than a factor of 4 and 1.4 for uncorrected and corrected values, respectively. User-generated RSF values were applied to the analysis of several elements in NIST SRM 2704 Buffalo River Sediment. In the absence of isobaric interferences, accuracies ranging from 0.6 to 73% were observed, demonstrating the potential of the technique for the determination of many elements. The presence of entrained water and inhomogeneity resulting from cathode preparation is thought to affect matrix-to-matrix reproducibility. While further success depends on developing means of circumventing mass spectral interferences and addressing factors affecting plasma chemistry, the immediate goal of developing a screening method for priority metals in soils was met. (Author)

  19. 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

  20. Determination of thorium and uranium contents in soil samples ...

    Indian Academy of Sciences (India)

    using CR-39 and LR-115-II solid-state nuclear track detectors (SSNTDs). ... standard soil samples have been determined and compared with its known values. ... measure α-tracks activity [1], where SSNTDs have been used in geology [2–6] ...

  1. Gamma spectroscopy analysis of archived Marshall Island soil samples

    International Nuclear Information System (INIS)

    Herman, S.; Hoffman, K.; Lavelle, K.; Trauth, A.; Glover, S.E.; Connick, W.; Spitz, H.; LaMont, S.P.; Hamilton, T.

    2016-01-01

    Four samples of archival Marshall Islands soil were subjected to non-destructive, broad energy (17 keV-2.61 MeV) gamma-ray spectrometry analysis using a series of different high-resolution germanium detectors. These archival samples were collected in 1967 from different locations on Bikini Atoll and were contaminated with a range of fission and activation products, and other nuclear material from multiple weapons tests. Unlike samples collected recently, these samples have been stored in sealed containers and have been unaffected by approximately 50 years of weathering. Initial results show that the samples contained measurable but proportionally different concentrations of plutonium, 241 Am, and 137 Cs, and 60 Co. (author)

  2. Novel sample preparation for operando TEM of catalysts

    International Nuclear Information System (INIS)

    Miller, Benjamin K.; Barker, Trevor M.; Crozier, Peter A.

    2015-01-01

    A new TEM sample preparation method is developed to facilitate operando TEM of gas phase catalysis. A porous Pyrex-fiber pellet TEM sample was produced, allowing a comparatively large amount of catalyst to be loaded into a standard Gatan furnace-type tantalum heating holder. The increased amount of catalyst present inside the environmental TEM allows quantitative determination of the gas phase products of a catalytic reaction performed in-situ at elevated temperatures. The product gas concentration was monitored using both electron energy loss spectroscopy (EELS) and residual gas analysis (RGA). Imaging of catalyst particles dispersed over the pellet at atomic resolution is challenging, due to charging of the insulating glass fibers. To overcome this limitation, a metal grid is placed into the holder in addition to the pellet, allowing catalyst particles dispersed over the grid to be imaged, while particles in the pellet, which are assumed to experience identical conditions, contribute to the overall catalytic conversion inside the environmental TEM cell. The gas within the cell is determined to be well-mixed, making this assumption reasonable. - Highlights: • High in-situ conversion of CO to CO 2 achieved by a novel TEM sample preparation method. • A 3 mm fiber pellet increases the TEM sample surface area by 50×. • Operando atomic resolution is maintained by also including a 3 mm grid in the sample. • Evidence for a well-mixed gas composition inside the ETEM cell is given

  3. Naturally Occurring Radionuclides and Rare Earth Elements Pattern in Weathered Japanese Soil Samples

    International Nuclear Information System (INIS)

    Sahoo, S.K.; Hosoda, M.; Takahashi, H.; Sorimachi, A.; Ishikawa, T.; Tokonami, S.; Uchida, S.

    2011-01-01

    From the viewpoint of radiation protection, determination of natural radionuclides e.g. thorium and uranium in soil samples are important. Accurate methods for determination of Th and U is gaining importance. The geochemical behavior of Th, U and rare earth elements (REEs) are relatively close to one another while compared to other elements in geological environment. Radioactive elements like 232 Th and 238 U along with their decay products (e.g. 226 Ra) are present in most of the environmental matrices and can be transferred to living bodies by different pathways that can lead to sources of exposure of man. Therefore, it is necessary to monitor these natural radionuclides in weathered soil samples to assess the possible hazards. The activity concentrations of 226 Ra, 228 Th, and 40 K in soils have been measured using a g γ-ray spectroscopy system with high purity germanium detector. The thorium, uranium and REEs were determined from the same sample using inductively coupled plasma mass spectrometry (ICP-MS). Granitic rocks contain higher amounts of Th, U and light REEs compared to other igneous rocks such as basalt and andesites. Therefore, it is necessary to understand the interaction between REEs and nature of soils, as soils are complex heterogeneous mixture of organic and inorganic solids, water and gases. In this paper, we have discussed about distribution pattern of 226 Ra, 232 Th and 238 U along with REEs in soil samples of weathered acid rock (granite and ryolite) collected from two prefectures in Japan: 1. Gifu and 2. Okinawa. (author)

  4. Determination method for 129I in soil samples by MIP-MS

    International Nuclear Information System (INIS)

    Uezu, Yasuhiro; Nakano, Masanao; Fujita, Hiroki; Watanabe, Hitoshi; Maruo, Yoshihiro

    2001-01-01

    The radioactive iodine-129 ( 129 I) is an important radionuclide for environmental assessment because it has a long half-life and is accumulated in the thyroid gland in humans. A new analytical technique by Microwave Induced Plasma Mass Spectrometer (MIP-MS) was applied to the determination of 129 I in soil samples. In environmental samples, a large amount of matrix elements are present. Therefore, the matrix elements were eliminated by ashing at 1000degC, and iodine isotopes were trapped by an activated charcoal and finally extracted by 10% tetramethylammonium hydroxide (TMAH). The concentration of 129 I in a soil samples were compared between results of neutron activation analysis and MIP-MS method. The results showed an excellent agreement. (author)

  5. Soil sample moisture content as a function of time during oven drying for gamma-ray spectroscopic measurements

    International Nuclear Information System (INIS)

    Benke, R.R.; Kearfott, K.J.

    1999-01-01

    In routine gamma-ray spectroscopic analysis of collected soil samples, procedure often calls to remove soil moisture by oven drying overnight at a temperature of 100 deg. C . Oven drying not only minimizes the gamma-ray self-attenuation of soil samples due to the absence of water during the gamma-ray spectroscopic analysis, but also allows for a straightforward calculation of the specific activity of radionuclides in soil, historically based on the sample dry weight. Because radon exhalation is strongly dependent on moisture , knowledge of the oven-drying time dependence of the soil moisture content, combined with radon exhalation measurements during oven drying and at room temperature for varying soil moisture contents, would allow conclusions to be made on how the oven-drying radon exhalation rate depends on soil moisture content. Determinations of the oven-drying radon exhalation from soil samples allow corrections to be made for the immediate laboratory gamma-ray spectroscopy of radionuclides in the natural uranium decay chain. This paper presents the results of soil moisture content measurements during oven drying and suggests useful empirical fits to the moisture data

  6. Measuring environmental change in forest ecosystems by repeated soil sampling: a North American perspective

    Science.gov (United States)

    Lawrence, Gregory B.; Fernandez, Ivan J.; Richter, Daniel D.; Ross, Donald S.; Hazlett, Paul W.; Bailey, Scott W.; Oiumet, Rock; Warby, Richard A.F.; Johnson, Arthur H.; Lin, Henry; Kaste, James M.; Lapenis, Andrew G.; Sullivan, Timothy J.

    2013-01-01

    Environmental change is monitored in North America through repeated measurements of weather, stream and river flow, air and water quality, and most recently, soil properties. Some skepticism remains, however, about whether repeated soil sampling can effectively distinguish between temporal and spatial variability, and efforts to document soil change in forest ecosystems through repeated measurements are largely nascent and uncoordinated. In eastern North America, repeated soil sampling has begun to provide valuable information on environmental problems such as air pollution. This review synthesizes the current state of the science to further the development and use of soil resampling as an integral method for recording and understanding environmental change in forested settings. The origins of soil resampling reach back to the 19th century in England and Russia. The concepts and methodologies involved in forest soil resampling are reviewed and evaluated through a discussion of how temporal and spatial variability can be addressed with a variety of sampling approaches. Key resampling studies demonstrate the type of results that can be obtained through differing approaches. Ongoing, large-scale issues such as recovery from acidification, long-term N deposition, C sequestration, effects of climate change, impacts from invasive species, and the increasing intensification of soil management all warrant the use of soil resampling as an essential tool for environmental monitoring and assessment. Furthermore, with better awareness of the value of soil resampling, studies can be designed with a long-term perspective so that information can be efficiently obtained well into the future to address problems that have not yet surfaced.

  7. Environmental radiation in coal and soil samples from Savannah area (Chatham County, GA)

    International Nuclear Information System (INIS)

    Hongo, D.; Ghuman, G.S.; Chandra, K.

    1997-01-01

    Radiation measurements were made in coal and fly ash samples from Savannah Electric ampersand Power Company (SEPCO) plant on the Savannah River and the soil core samples from three sites along the flow gradient of Savannah State University Campus Creek. The objective of this study was to determine the magnitude of natural radiation due to radon and potassium in the Savannah area and possible effect of external factors such as the operations at Savannah River Site (SRS). The instrument used for this purpose was Geiger Counter Model 500 (Tennelec/Nucleus, Inc.) which was standardized with known samples of Sr-90 (0.1 μCi t 1/2 = 28.6 yrs., beta radiation) and Co-60 (1.0 μCi t 1/2 = 5.27 yrs., gamma radiation). Beta and gamma radiations in the samples were differentiated with the help of polyethylene and lead absorbers. Results showed quite low radioactivity in bituminous coal from SEPCO plant and it reduced by a factor of 0.5 and 0.25 in fly ash and weathered fly ash, respectively. Radioactivity of soil samples was slightly greater in the top soil (0-3 cm) of two sites and it decreased markedly with depth (20 cm). Site III soil samples containing lime shells had a negligible radioactivity because carbonate rocks developed from calcareous skeletal matter have low radioactivity from their beginning. Radioactivity appeared to be mainly associated with the fine textured top soil of two sites (high clay content) and it exhibited very little leaching downward into lower layers. Clay particles with greater radioactivity, are formed from the decomposition of feldspars and micas which contain a large fraction of earth's potassium fraction. Measurements with the use of absorbers indicated that the observed radiation in all the samples was mainly due to the gamma rays. A comparison with the radioactivity in coal dust and fly ash samples from SRS revealed that the Savannah samples contained extremely low radiation, which may be due only to the natural sources

  8. Fluoride concentrations in soils, vegetation samples and soil fauna in the direct vicinity of a pollution source

    International Nuclear Information System (INIS)

    Vogel, J.; Ottow, J.C.G.; Breimer, R.F.

    1989-01-01

    Fluoride analyses CF t = total F; F w = water soluble F and F HCI HCI-extractable F) of different soils, vegetation samples and soil fauna (Helix pomatia, Lumbricus spp., arthropodes) in a locally polluted area (for nearly 65 years) clearly revealed an F-accumulation in top soil, vegetation and animals. Based on 1N HCI-extractable fluoride, two contamination zones around the emitting industry could be identified. In the calcareous soils, leaching of fluoride seems to be insignificant because of a strong immobilization as CaF 2 . A highly significant correlation between the F HCI content of soils and Lumbricus spp. (with and without gut content) or Helix pomatia shells was found. Fluoride concentrations in washed leaves of Hedera helix and in decaying grass reached levels of 306 and 997 μgF/g respectively. Saprophagous soil arthropods contained high fluoride levels, up to 732 μgF/g in Armadillidium vulgare. (orig.)

  9. Pilot studies for the North American Soil Geochemical Landscapes Project - Site selection, sampling protocols, analytical methods, and quality control protocols

    Science.gov (United States)

    Smith, D.B.; Woodruff, L.G.; O'Leary, R. M.; Cannon, W.F.; Garrett, R.G.; Kilburn, J.E.; Goldhaber, M.B.

    2009-01-01

    In 2004, the US Geological Survey (USGS) and the Geological Survey of Canada sampled and chemically analyzed soils along two transects across Canada and the USA in preparation for a planned soil geochemical survey of North America. This effort was a pilot study to test and refine sampling protocols, analytical methods, quality control protocols, and field logistics for the continental survey. A total of 220 sample sites were selected at approximately 40-km intervals along the two transects. The ideal sampling protocol at each site called for a sample from a depth of 0-5 cm and a composite of each of the O, A, and C horizons. The Ca, Fe, K, Mg, Na, S, Ti, Ag, As, Ba, Be, Bi, Cd, Ce, Co, Cr, Cs, Cu, Ga, In, La, Li, Mn, Mo, Nb, Ni, P, Pb, Rb, Sb, Sc, Sn, Sr, Te, Th, Tl, U, V, W, Y, and Zn by inductively coupled plasma-mass spectrometry and inductively coupled plasma-atomic emission spectrometry following a near-total digestion in a mixture of HCl, HNO3, HClO4, and HF. Separate methods were used for Hg, Se, total C, and carbonate-C on this same size fraction. Only Ag, In, and Te had a large percentage of concentrations below the detection limit. Quality control (QC) of the analyses was monitored at three levels: the laboratory performing the analysis, the USGS QC officer, and the principal investigator for the study. This level of review resulted in an average of one QC sample for every 20 field samples, which proved to be minimally adequate for such a large-scale survey. Additional QC samples should be added to monitor within-batch quality to the extent that no more than 10 samples are analyzed between a QC sample. Only Cr (77%), Y (82%), and Sb (80%) fell outside the acceptable limits of accuracy (% recovery between 85 and 115%) because of likely residence in mineral phases resistant to the acid digestion. A separate sample of 0-5-cm material was collected at each site for determination of organic compounds. A subset of 73 of these samples was analyzed for a suite of

  10. Laboratory Electrical Resistivity Studies on Cement Stabilized Soil

    Science.gov (United States)

    Lokesh, K. N.; Jacob, Jinu Mary

    2017-01-01

    Electrical resistivity measurement of freshly prepared uncured and cured soil-cement materials is done and the correlations between the factors controlling the performance of soil-cement and electrical resistivity are discussed in this paper. Conventional quality control of soil-cement quite often involves wastage of a lot of material, if it does not meet the strength criteria. In this study, it is observed that, in soil-cement, resistivity follows a similar trend as unconfined compressive strength, with increase in cement content and time of curing. Quantitative relations developed for predicting 7-day strength of soil-cement mix, using resistivity of the soil-cement samples at freshly prepared state, after 1-hour curing help to decide whether the soil-cement mix meets the desired strength and performance criteria. This offers the option of the soil-cement mix to be upgraded (possibly with additional cement) in its fresh state itself, if it does not fulfil the performance criteria, rather than wasting the material after hardening. PMID:28540364

  11. Modern methods of sample preparation for GC analysis

    NARCIS (Netherlands)

    de Koning, S.; Janssen, H.-G.; Brinkman, U.A.Th.

    2009-01-01

    Today, a wide variety of techniques is available for the preparation of (semi-) solid, liquid and gaseous samples, prior to their instrumental analysis by means of capillary gas chromatography (GC) or, increasingly, comprehensive two-dimensional GC (GC × GC). In the past two decades, a large number

  12. Collection and preparation of wet and dry stream-sediment samples

    International Nuclear Information System (INIS)

    Puchlik, K.

    1977-03-01

    Lawrence Livermore Laboratory is responsible for the Hydrogeochemistry and Stream Sediment Reconnaissance (HSSR) program for uranium in the seven far western states. The work thus far has concentrated on the arid to semi-arid regions of the West and this paper discusses the collection and preparation of sediment samples in the Basin and Range province. The sample collection and preparation procedures described here may not be applicable to other parts of the far western states or other areas. These procedures also differ somewhat from those used by the other three laboratories involved in the HSSR program

  13. Operable Unit 3-13, Group 3, Other Surface Soils (Phase II) Field Sampling Plan

    Energy Technology Data Exchange (ETDEWEB)

    G. L. Schwendiman

    2006-07-27

    This Field Sampling Plan describes the Operable Unit 3-13, Group 3, Other Surface Soils, Phase II remediation field sampling activities to be performed at the Idaho Nuclear Technology and Engineering Center located within the Idaho National Laboratory Site. Sampling activities described in this plan support characterization sampling of new sites, real-time soil spectroscopy during excavation, and confirmation sampling that verifies that the remedial action objectives and remediation goals presented in the Final Record of Decision for Idaho Nuclear Technology and Engineering Center, Operable Unit 3-13 have been met.

  14. Assessment and distribution of antimony in soils around three coal mines, Anhui, China

    Science.gov (United States)

    Qi, C.; Liu, Gaisheng; Kang, Y.; Lam, P.K.S.; Chou, C.

    2011-01-01

    Thirty-three soil samples were collected from the Luling, Liuer, and Zhangji coal mines in the Huaibei and Huainan areas of Anhui Province, China. The samples were analyzed for antimony (Sb) by inductively coupled plasmaoptical emission spectrometry (ICP-OES) method. The average Sb content in the 33 samples was 4 mg kg-1, which is lower than in coals from this region (6.2 mg kg-1). More than 75% of the soils sampled showed a significant degree of Sb pollution (enrichment factors [EFs] 5-20). The soils collected near the gob pile and coal preparation plant were higher in Sb content than those collected from residential areas near the mines. The gob pile and tailings from the preparation plant were high in mineral matter content and high in Sb. They are the sources of Sb pollution in surface soils in the vicinity of coal mines. The spatial dispersion of Sb in surface soil in the mine region shows that Sb pollution could reach out as far as 350 m into the local environment conditions. Crops in rice paddies may adsorb some Sb and reduce the Sb content in soils from paddyfields. Vertical distribution of Sb in two soil profiles indicates that Sb is normally relatively immobile in soils. ?? 2011 Air & Waste Management Association.

  15. Two media method for linear attenuation coefficient determination of irregular soil samples

    International Nuclear Information System (INIS)

    Vici, Carlos Henrique Georges

    2004-01-01

    In several situations of nuclear applications, the knowledge of gamma-ray linear attenuation coefficient for irregular samples is necessary, such as in soil physics and geology. This work presents the validation of a methodology for the determination of the linear attenuation coefficient (μ) of irregular shape samples, in such a way that it is not necessary to know the thickness of the considered sample. With this methodology irregular soil samples (undeformed field samples) from Londrina region, north of Parana were studied. It was employed the two media method for the μ determination. It consists of the μ determination through the measurement of a gamma-ray beam attenuation by the sample sequentially immersed in two different media, with known and appropriately chosen attenuation coefficients. For comparison, the theoretical value of μ was calculated by the product of the mass attenuation coefficient, obtained by the WinXcom code, and the measured value of the density sample. This software employs the chemical composition of the samples and supplies a table of the mass attenuation coefficients versus the photon energy. To verify the validity of the two media method, compared with the simple gamma ray transmission method, regular pome stone samples were used. With these results for the attenuation coefficients and their respective deviations, it was possible to compare the two methods. In this way we concluded that the two media method is a good tool for the determination of the linear attenuation coefficient of irregular materials, particularly in the study of soils samples. (author)

  16. Sampling and sample preparation methods for the analysis of trace elements in biological material

    International Nuclear Information System (INIS)

    Sansoni, B.; Iyengar, V.

    1978-05-01

    The authors attempt to give a most systamtic possible treatment of the sample taking and sample preparation of biological material (particularly in human medicine) for trace analysis (e.g. neutron activation analysis, atomic absorption spectrometry). Contamination and loss problems are discussed as well as the manifold problems of the different consistency of solid and liquid biological materials, as well as the stabilization of the sample material. The process of dry and wet ashing is particularly dealt with, where new methods are also described. (RB) [de

  17. Sample preparation with solid phase microextraction and exhaustive extraction approaches: Comparison for challenging cases.

    Science.gov (United States)

    Boyacı, Ezel; Rodríguez-Lafuente, Ángel; Gorynski, Krzysztof; Mirnaghi, Fatemeh; Souza-Silva, Érica A; Hein, Dietmar; Pawliszyn, Janusz

    2015-05-11

    In chemical analysis, sample preparation is frequently considered the bottleneck of the entire analytical method. The success of the final method strongly depends on understanding the entire process of analysis of a particular type of analyte in a sample, namely: the physicochemical properties of the analytes (solubility, volatility, polarity etc.), the environmental conditions, and the matrix components of the sample. Various sample preparation strategies have been developed based on exhaustive or non-exhaustive extraction of analytes from matrices. Undoubtedly, amongst all sample preparation approaches, liquid extraction, including liquid-liquid (LLE) and solid phase extraction (SPE), are the most well-known, widely used, and commonly accepted methods by many international organizations and accredited laboratories. Both methods are well documented and there are many well defined procedures, which make them, at first sight, the methods of choice. However, many challenging tasks, such as complex matrix applications, on-site and in vivo applications, and determination of matrix-bound and free concentrations of analytes, are not easily attainable with these classical approaches for sample preparation. In the last two decades, the introduction of solid phase microextraction (SPME) has brought significant progress in the sample preparation area by facilitating on-site and in vivo applications, time weighted average (TWA) and instantaneous concentration determinations. Recently introduced matrix compatible coatings for SPME facilitate direct extraction from complex matrices and fill the gap in direct sampling from challenging matrices. Following introduction of SPME, numerous other microextraction approaches evolved to address limitations of the above mentioned techniques. There is not a single method that can be considered as a universal solution for sample preparation. This review aims to show the main advantages and limitations of the above mentioned sample

  18. Automated dried blood spots standard and QC sample preparation using a robotic liquid handler.

    Science.gov (United States)

    Yuan, Long; Zhang, Duxi; Aubry, Anne-Francoise; Arnold, Mark E

    2012-12-01

    A dried blood spot (DBS) bioanalysis assay involves many steps, such as the preparation of standard (STD) and QC samples in blood, the spotting onto DBS cards, and the cutting-out of the spots. These steps are labor intensive and time consuming if done manually, which, therefore, makes automation very desirable in DBS bioanalysis. A robotic liquid handler was successfully applied to the preparation of STD and QC samples in blood and to spot the blood samples onto DBS cards using buspirone as the model compound. This automated preparation was demonstrated to be accurate and consistent. However the accuracy and precision of automated preparation were similar to those from manual preparation. The effect of spotting volume on accuracy was evaluated and a trend of increasing concentrations of buspirone with increasing spotting volumes was observed. The automated STD and QC sample preparation process significantly improved the efficiency, robustness and safety of DBS bioanalysis.

  19. 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.

  20. Norm in soil and sludge samples in Dukhan oil Field, Qatar state

    Energy Technology Data Exchange (ETDEWEB)

    Al-Kinani, A.T.; Hushari, M.; Al-Sulaiti, Huda; Alsadig, I.A., E-mail: mmhushari@moe.gov.qa [Radiation and Chemical Protection Department, Ministry of Environment, Doha (Qatar)

    2015-07-01

    The main objective of this work is to measure the activity concentrations of Naturally Occurring radioactive Materials (NORM) produced as a buy products in oil production. The analyses of NORM give available information for guidelines concerning radiation protection. Recently NORM subjected to restricted regulation issued by high legal authority at Qatar state. Twenty five samples of soil from Dukhan onshore oil field and 10 sludge samples collected from 2 offshore fields at Qatar state. High resolution low-level gamma-ray spectrometry used to measure gamma emitters of NORM. The activity concentrations of natural radionuclide in 22 samples from Dukhan oil field, were with average worldwide values . Only three soil samples have high activity concentration of Ra-226 which is more than 185 Bq/kg the exempted level for NORM in the Quatrain regulation. The natural radionuclide activity concentrations of 10 sludge samples from offshore oil fields was greater than 1100Bq/kg the exempted values of NORM set by Quatrain regulation so the sludge need special treatments. The average hazards indices (H{sub ex} , D , and Ra{sub eq}), for the 22 samples were below the word permissible values .This means that the human exposure to such material not impose any radiation risk. The average hazards indices (H{sub ex} , D , and Ra{sub eq}), for 3 soil samples and sludge samples are higher than the published maximal permissible. Thus human exposure to such material impose radiation risk. (author)

  1. Norm in soil and sludge samples in Dukhan oil Field, Qatar state

    International Nuclear Information System (INIS)

    Al-Kinani, A.T.; Hushari, M.; Al-Sulaiti, Huda; Alsadig, I.A.

    2015-01-01

    The main objective of this work is to measure the activity concentrations of Naturally Occurring radioactive Materials (NORM) produced as a buy products in oil production. The analyses of NORM give available information for guidelines concerning radiation protection. Recently NORM subjected to restricted regulation issued by high legal authority at Qatar state. Twenty five samples of soil from Dukhan onshore oil field and 10 sludge samples collected from 2 offshore fields at Qatar state. High resolution low-level gamma-ray spectrometry used to measure gamma emitters of NORM. The activity concentrations of natural radionuclide in 22 samples from Dukhan oil field, were with average worldwide values . Only three soil samples have high activity concentration of Ra-226 which is more than 185 Bq/kg the exempted level for NORM in the Quatrain regulation. The natural radionuclide activity concentrations of 10 sludge samples from offshore oil fields was greater than 1100Bq/kg the exempted values of NORM set by Quatrain regulation so the sludge need special treatments. The average hazards indices (H ex , D , and Ra eq ), for the 22 samples were below the word permissible values .This means that the human exposure to such material not impose any radiation risk. The average hazards indices (H ex , D , and Ra eq ), for 3 soil samples and sludge samples are higher than the published maximal permissible. Thus human exposure to such material impose radiation risk. (author)

  2. Contamination of apple orchard soils and fruit trees with copper-based fungicides: sampling aspects.

    Science.gov (United States)

    Wang, Quanying; Liu, Jingshuang; Liu, Qiang

    2015-01-01

    Accumulations of copper in orchard soils and fruit trees due to the application of Cu-based fungicides have become research hotspots. However, information about the sampling strategies, which can affect the accuracy of the following research results, is lacking. This study aimed to determine some sampling considerations when Cu accumulations in the soils and fruit trees of apple orchards are studied. The study was conducted in three apple orchards from different sites. Each orchard included two different histories of Cu-based fungicides usage, varying from 3 to 28 years. Soil samples were collected from different locations varying with the distances from tree trunk to the canopy drip line. Fruits and leaves from the middle heights of tree canopy at two locations (outer canopy and inner canopy) were collected. The variation in total soil Cu concentrations between orchards was much greater than the variation within orchards. Total soil Cu concentrations had a tendency to increase with the increasing history of Cu-based fungicides usage. Moreover, total soil Cu concentrations had the lowest values at the canopy drip line, while the highest values were found at the half distances between the trunk and the canopy drip line. Additionally, Cu concentrations of leaves and fruits from the outer parts of the canopy were significantly higher than from the inner parts. Depending on the findings of this study, not only the between-orchard variation but also the within-orchard variation should be taken into consideration when conducting future soil and tree samplings in apple orchards.

  3. Mobility of arsenic, cadmium and zinc in a multi-element contaminated soil profile assessed by in-situ soil pore water sampling, column leaching and sequential extraction

    International Nuclear Information System (INIS)

    Beesley, Luke; Moreno-Jimenez, Eduardo; Clemente, Rafael; Lepp, Nicholas; Dickinson, Nicholas

    2010-01-01

    Three methods for predicting element mobility in soils have been applied to an iron-rich soil, contaminated with arsenic, cadmium and zinc. Soils were collected from 0 to 30 cm, 30 to 70 cm and 70 to 100 cm depths in the field and soil pore water was collected at different depths from an adjacent 100 cm deep trench. Sequential extraction and a column leaching test in the laboratory were compared to element concentrations in pore water sampled directly from the field. Arsenic showed low extractability, low leachability and occurred at low concentrations in pore water samples. Cadmium and zinc were more labile and present in higher concentrations in pore water, increasing with soil depth. Pore water sampling gave the best indication of short term element mobility when field conditions were taken into account, but further extraction and leaching procedures produced a fuller picture of element dynamics, revealing highly labile Cd deep in the soil profile. - Mobility of arsenic, cadmium and zinc in a polluted soil can be realistically interpreted by in-situ soil pore water sampling.

  4. Sampling season affects conclusions on soil arthropod community structure responses to metal pollution in Mediterranean urban soils

    NARCIS (Netherlands)

    Santorufo, L.; van Gestel, C.A.M.; Maisto, G.

    2014-01-01

    This study aimed to assess if the period of sampling affected conclusions on the responses of arthropod community structure to metal pollution in urban soils in the Mediterranean area. Higher temperature and lower precipitation were detected in autumn than in spring. In both samplings, the most

  5. Determination of total organic phosphorus in samples of mineral soils

    Directory of Open Access Journals (Sweden)

    Armi Kaila

    1962-01-01

    Full Text Available In this paper some observations on the estimation of organic phosphorus in mineral soils are reported. The fact is emphasized that the accuracy of all the methods available is relatively poor. Usually, there are no reasons to pay attention to differences less than about 20 ppm. of organic P. Analyses performed on 345 samples of Finnish mineral soils by the extraction method of MEHTA et. al. (10 and by a simple procedure adopted by the author (successive extractions with 4 N H2SO4 and 0.5 N NaOH at room temperature in the ratio of 1 to 100 gave, on the average, equal results. It seemed to be likely that the MEHTA method removed the organic phosphorus more completely than did the less vigorous method, but in the former the partial hydrolysis of organic phosphorus compounds tends to be higher than in the latter. An attempt was made to find out whether the differences between the respective values for organic phosphorus obtained by an ignition method and the simple extraction method could be connected with any characteristics of the soil. No correlation or only a low correlation coefficient could be calculated between the difference in the results of these two methods and e. g. the pH-value, the content of clay, organic carbon, aluminium and iron soluble in Tamm’s acid oxalate, the indicator of the phosphate sorption capacity, or the »Fe-bound» inorganic phosphorus, respectively. The absolute difference tended to increase with an increase in the content of organic phosphorus. For the 250 samples of surface soils analyzed, the ignition method gave values which were, on the average, about 50 ppm. higher than the results obtained by the extraction procedure. The corresponding difference for the 120 samples from deeper layers was about 20 ppm of organic P. The author recommends, for the present, the determination of the total soil organic phosphorus as an average of the results obtained by the ignition method and the extraction method.

  6. Independent assessment of matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) sample preparation quality : Effect of sample preparation on MALDI-MS of synthetic polymers

    NARCIS (Netherlands)

    Kooijman, Pieter C.; Kok, Sander; Honing, Maarten

    2017-01-01

    Rationale: Matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) provides detailed and in-depth information about the molecular characteristics of synthetic polymers. To obtain the most accurate results the sample preparation parameters should be chosen to suit the sample and the

  7. Application of autoradiographic methods for contaminant distribution studies in soils

    International Nuclear Information System (INIS)

    Povetko, O.G.; Higley, K.A.

    2000-01-01

    In order to determine physical location of contaminants in soil, solidified soil 'thin' sections, which preserve the undisturbed structural characteristics of the original soil, were prepared. This paper describes an application of different autoradiographic methods to identify the distribution of selected nuclides along key structural features of sample soils and sizes of 'hot particles' of contaminant. These autoradiographic methods included contact autoradiography using CR-39 (Homalite Plastics) plastic alpha track detectors and neutron-induced autoradiography that produced fission fragment tracks in Lexan (Thrust Industries, Inc.) plastic detectors. Intact soil samples containing weapons-grade plutonium from Rocky Flats Environmental Test Site and control samples from outside the site location were used in thin soil section preparation. Distribution of particles of actinides was observed and analyzed through the soil section depth profile from the surface to the 15-cm depth. The combination of two autoradiographic methods allowed to distinguish alpha- emitting particles of natural U, 239+240 Pu and non-fissile alpha-emitters. Locations of 990 alpha 'stars' caused by 239+240 Pu and 241 Am 'hot particles' were recorded, particles were sized, their size-frequency, depth and activity distributions were analyzed. Several large colloidal conglomerates of 239+240 Pu and 241 Am 'hot particles' were found in soil profile. Their alpha and fission fragment 'star' images were micro photographed. (author)

  8. CTEPP STANDARD OPERATING PROCEDURE FOR COLLECTION OF SOIL SAMPLES FOR PERSISTENT ORGANIC POLLUTANTS (SOP-2.20)

    Science.gov (United States)

    This SOP describes the method for collecting soil samples from the child's outdoor play area to measure for persistent organic pollutants. Soil samples are collected by scraping up the top 0.5 cm of soil in a 0.095 m2 (1 ft2) area in the middle of the child's play area.

  9. Sampling and analysis plan for Mount Plant D ampersand D soils packages, Revision 1

    International Nuclear Information System (INIS)

    1991-02-01

    There are currently 682 containers of soils in storage at Mound Plant, generated between April 1 and October 31, 1990 as a result of excavation of soils containing plutonium-238 at two ongoing Decontamination and Decommissioning (D ampersand D) Program sites. These areas are known as Area 14, the waste transfer system (WTS) hillside, and Area 17, the Special Metallurgical (SM) Building area. The soils from these areas are part of Mound Plant waste stream number AMDM-000000010, Contaminated Soil, and are proposed for shipment to the Nevada Test Site (NTS) for disposal as low-level radioactive waste. The sealed waste packages, constructed of either wood or metal, are currently being stored in Building 31 and at other locations throughout the Mound facility. At a meeting in Las Vegas, Nevada on October, 26, 1990, DOE Nevada Operations Office (DOE-NV) and NTS representatives requested that the Mound Plant D ampersand D soils proposed for shipment to NTS be sampled for Toxicity Characteristic Leaching Procedure (TCLP) constituents. On December 14, 1990, DOE-NV also requested that additional analyses be performed on the soils from one of the soils boxes for polychlorinated biphenyls (PCBs), particle size distribution, and free liquids. The purpose of this plan is to document the proposed sampling and analyses of the packages of D ampersand D soils produced prior to October 31, 1990. In order to provide a thorough description of the soils excavated from the WTS and SM areas, sections 1.1 and 1.2 provide historical Information concerning the D ampersand D soils, including waste stream evaluations and past sampling data

  10. 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.

  11. 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.

  12. Universal Sample Preparation Module for Molecular Analysis in Space, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Lynntech proposes to develop and demonstrate the ability of a compact, light-weight, and automated universal sample preparation module (USPM) to process samples from...

  13. 14CO2 analysis of soil gas: Evaluation of sample size limits and sampling devices

    Science.gov (United States)

    Wotte, Anja; Wischhöfer, Philipp; Wacker, Lukas; Rethemeyer, Janet

    2017-12-01

    Radiocarbon (14C) analysis of CO2 respired from soils or sediments is a valuable tool to identify different carbon sources. The collection and processing of the CO2, however, is challenging and prone to contamination. We thus continuously improve our handling procedures and present a refined method for the collection of even small amounts of CO2 in molecular sieve cartridges (MSCs) for accelerator mass spectrometry 14C analysis. Using a modified vacuum rig and an improved desorption procedure, we were able to increase the CO2 recovery from the MSC (95%) as well as the sample throughput compared to our previous study. By processing series of different sample size, we show that our MSCs can be used for CO2 samples of as small as 50 μg C. The contamination by exogenous carbon determined in these laboratory tests, was less than 2.0 μg C from fossil and less than 3.0 μg C from modern sources. Additionally, we tested two sampling devices for the collection of CO2 samples released from soils or sediments, including a respiration chamber and a depth sampler, which are connected to the MSC. We obtained a very promising, low process blank for the entire CO2 sampling and purification procedure of ∼0.004 F14C (equal to 44,000 yrs BP) and ∼0.003 F14C (equal to 47,000 yrs BP). In contrast to previous studies, we observed no isotopic fractionation towards lighter δ13C values during the passive sampling with the depth samplers.

  14. Mapping of depleted uranium with in situ spectrometry and soil samples

    International Nuclear Information System (INIS)

    Shebell, P.; Reginatto, M.; Monetti, M.; Faller, S.; Davis, L.

    1999-01-01

    Depleted uranium (DU) has been developed in the past two decades as a highly effective material for armor penetrating rounds and vehicle shielding. There is now a growing interest in the defense community to determine the presence and extent of DU contamination quickly and with a minimum amount of intrusive sampling. We report on a new approach using deconvolution techniques to quantitatively map DU contamination in surface soil. This approach combines data from soil samples with data from in situ gamma-ray spectrometry measurements to produce an accurate and detailed map of DU contamination. Results of a field survey at the Aberdeen Proving Ground are presented. (author)

  15. Elemental analysis of soil and plant samples at El-Manzala lake neutron activation analysis technique. Vol. 4

    Energy Technology Data Exchange (ETDEWEB)

    Eissa, E A; Rofail, N B; Hassan, A M [Reactor and Neutron Physics Department, Nuclear Research Center, Atomic Energy Authority, Cairo (Egypt); Abd El-Haleem, A S [Radiactive Environment Pollution Department, Hot Laboratories Center, Nuclear Research Center, Atomic Energy Authority, Cairo (Egypt); El-Abbady, W H [Phsics Department, Faculty of Science , Al-Azhar University, (Egypt)

    1996-03-01

    Soil and plant samples were collected from from two locations, Bahr El-Baker, and Bahr kados at the manzala lake, where, where high pollution is expected. The samples were especially treated and prepared for investigation by thermal neutron activation analysis (NAA). The irradiation facilities of the first egyptian research reactor (ET-R R-1), and the hyper pure germanium (HPGe) detection system were used for analysis. Among the 34 identified Fe, Co, As, Cd, Te, La, Sm, Rb, Hg, Th, and U are of a special significance because of the their toxic deleterious impact on living organisms. This work is part of a research project concerning pollution studies on the river Nile and some lakes of egypt. The data obtained in the present work stands as a reference basic record for any future follow up of contamination level. 1 tab.

  16. Elemental analysis of soil and plant samples at El-Manzala lake neutron activation analysis technique. Vol. 4

    International Nuclear Information System (INIS)

    Eissa, E.A.; Rofail, N.B.; Hassan, A.M.; Abd El-Haleem, A.S.; El-Abbady, W.H.

    1996-01-01

    Soil and plant samples were collected from from two locations, Bahr El-Baker, and Bahr kados at the manzala lake, where, where high pollution is expected. The samples were especially treated and prepared for investigation by thermal neutron activation analysis (NAA). The irradiation facilities of the first egyptian research reactor (ET-R R-1), and the hyper pure germanium (HPGe) detection system were used for analysis. Among the 34 identified Fe, Co, As, Cd, Te, La, Sm, Rb, Hg, Th, and U are of a special significance because of the their toxic deleterious impact on living organisms. This work is part of a research project concerning pollution studies on the river Nile and some lakes of egypt. The data obtained in the present work stands as a reference basic record for any future follow up of contamination level. 1 tab

  17. Field sampling of soil pore water to evaluate trace element mobility and associated environmental risk

    Energy Technology Data Exchange (ETDEWEB)

    Moreno-Jimenez, Eduardo, E-mail: eduardo.moreno@uam.es [Departamento de Quimica Agricola, Universidad Autonoma de Madrid, 28049 Madrid (Spain); Beesley, Luke [James Hutton Institute, Craigiebuckler, Aberdeen AB15 8QH (United Kingdom); Lepp, Nicholas W. [35, Victoria Road, Formby, Liverpool L37 7DH (United Kingdom); Dickinson, Nicholas M. [Department of Ecology, Lincoln University, Lincoln 7647, PO Box 84 (New Zealand); Hartley, William [School of Computing, Science and Engineering, University of Salford, Cockcroft Building, Salford, M5 4WT (United Kingdom); Clemente, Rafael [Dep. of Soil and Water Conservation and Organic Waste Management, CEBAS-CSIC, Campus Universitario de Espinardo, PO Box 164, 30100 Espinardo, Murcia (Spain)

    2011-10-15

    Monitoring soil pollution is a key aspect in sustainable management of contaminated land but there is often debate over what should be monitored to assess ecological risk. Soil pore water, containing the most labile pollutant fraction in soils, can be easily collected in situ offering a routine way to monitor this risk. We present a compilation of data on concentration of trace elements (As, Cd, Cu, Pb, and Zn) in soil pore water collected in field conditions from a range of polluted and non-polluted soils in Spain and the UK during single and repeated monitoring, and propose a simple eco-toxicity test using this media. Sufficient pore water could be extracted for analysis both under semi-arid and temperate conditions, and eco-toxicity comparisons could be effectively made between polluted and non-polluted soils. We propose that in-situ pore water extraction could enhance the realism of risk assessment at some contaminated sites. - Highlights: > In situ pore water sampling successfully evaluates trace elements mobility in soils. > Field sampling proved robust for different soils, sites and climatic regimes. > Measurements may be directly related to ecotoxicological assays. > Both short and long-term monitoring of polluted lands may be achieved. > This method complements other widely used assays for environmental risk assessment. - In situ pore water sampling from a wide variety of soils proves to be a beneficial application to monitor the stability of pollutants in soils and subsequent risk through mobility.

  18. Microbial diversity in firework chemical exposed soil and water samples collected in Virudhunagar district, Tamil Nadu, India.

    Science.gov (United States)

    Dhasarathan, P; Theriappan, P; Ashokraja, C

    2010-03-01

    Microbial diversity of soil and water samples collected from pyrochemicals exposed areas of Virdhunagar district (Tamil Nadu, India) was studied. Soil and water samples from cultivable area, waste land and city area of the same region were also studied for a comparative acount. There is a remarkable reduction in total heterotrophic bacterial population (THB) in pyrochemicals exposed soil and water samples (42 × 10(4) CFU/g and 5.6 × 10(4) CFU/ml respectively), compared to the THB of cultivable area soil and water samples (98 × 10(7) CFU/g and 38.6 × 10(7) CFU/ml). The generic composition the THB of the pyrochemicals exposed samples too exhibited considerable change compared to other samples. Pseudomonas sp. was the predominant one (41.6%) followed by Achromobacter sp. (25%) in pyrochemical exposed soil and Pseudomonas sp. was the predominant one (25%) in pyrochemical exposed water samples followed by Bacillus sp. (25%) and Micrococcus sp. (16.6%). It was observed that Cornybacterium sp. and Micrococcus sp. were absent completely in pyrochemical exposed soil and Achromobacter sp. was missing in the pyrochemical exposed water samples, which were present in the other samples. The outcome of this study clearly demonstrates that pollutants such as chemicals used in pyrotechniques affect the microbial biodiversity and suitable measures have to be taken to control the pollution level and to save biodiversity.

  19. Critical evaluation of distillation procedure for the determination of methylmercury in soil samples.

    Science.gov (United States)

    Perez, Pablo A; Hintelman, Holger; Quiroz, Waldo; Bravo, Manuel A

    2017-11-01

    In the present work, the efficiency of distillation process for extracting monomethylmercury (MMHg) from soil samples was studied and optimized using an experimental design methodology. The influence of soil composition on MMHg extraction was evaluated by testing of four soil samples with different geochemical characteristics. Optimization suggested that the acid concentration and the duration of the distillation process were most significant and the most favorable conditions, established as a compromise for the studied soils, were determined to be a 70 min distillation using an 0.2 M acid. Corresponding limits of detection (LOD) and quantification (LOQ) were 0.21 and 0.7 pg absolute, respectively. The optimized methodology was applied with satisfactory results to soil samples and was compared to a reference methodology based on isotopic dilution analysis followed by gas chromatography-inductively coupled plasma mass spectrometry (IDA-GC-ICP-MS). Using the optimized conditions, recoveries ranged from 82 to 98%, which is an increase of 9-34% relative to the previously used standard operating procedure. Finally, the validated methodology was applied to quantify MMHg in soils collected from different sites impacted by coal fired power plants in the north-central zone of Chile, measuring MMHg concentrations ranging from 0.091 to 2.8 ng g -1 . These data are to the best of our knowledge the first MMHg measurements reported for Chile. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Recent developments in sample preparation and data pre-treatment in metabonomics research.

    Science.gov (United States)

    Li, Ning; Song, Yi peng; Tang, Huiru; Wang, Yulan

    2016-01-01

    Metabonomics is a powerful approach for biomarker discovery and an effective tool for pinpointing endpoint metabolic effects of external stimuli, such as pathogens and disease development. Due to its wide applications, metabonomics is required to deal with various biological samples of different properties. Hence sample preparation and corresponding data pre-treatment become important factors in ensuring validity of an investigation. In this review, we summarize some recent developments in metabonomics sample preparation and data-pretreatment procedures. Copyright © 2015 Elsevier Inc. All rights reserved.

  1. Current advances and strategies towards fully automated sample preparation for regulated LC-MS/MS bioanalysis.

    Science.gov (United States)

    Zheng, Naiyu; Jiang, Hao; Zeng, Jianing

    2014-09-01

    Robotic liquid handlers (RLHs) have been widely used in automated sample preparation for liquid chromatography-tandem mass spectrometry (LC-MS/MS) bioanalysis. Automated sample preparation for regulated bioanalysis offers significantly higher assay efficiency, better data quality and potential bioanalytical cost-savings. For RLHs that are used for regulated bioanalysis, there are additional requirements, including 21 CFR Part 11 compliance, software validation, system qualification, calibration verification and proper maintenance. This article reviews recent advances in automated sample preparation for regulated bioanalysis in the last 5 years. Specifically, it covers the following aspects: regulated bioanalysis requirements, recent advances in automation hardware and software development, sample extraction workflow simplification, strategies towards fully automated sample extraction, and best practices in automated sample preparation for regulated bioanalysis.

  2. Determination of {sup 90}Sr in soil samples using inductively coupled plasma mass spectrometry equipped with dynamic reaction cell (ICP-DRC-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Feuerstein, J.; Boulyga, S.F.; Galler, P.; Stingeder, G. [Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, University of Natural Resources and Applied Life Sciences, Muthgasse 18, A-1190 Vienna (Austria); Prohaska, T. [Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, University of Natural Resources and Applied Life Sciences, Muthgasse 18, A-1190 Vienna (Austria)], E-mail: thomas.prohaska@boku.ac.at

    2008-11-15

    A rapid method is reported for the determination of {sup 90}Sr in contaminated soil samples in the vicinity of the Chernobyl Nuclear Power Plant by ICP-DRC-MS. Sample preparation and measurement procedures focus on overcoming the isobaric interference of {sup 90}Zr, which is present in soils at concentrations higher by more than six orders of magnitude than {sup 90}Sr. Zirconium was separated from strontium in two steps to reduce the interference by {sup 90}Zr{sup +} ions by a factor of more than 10{sup 7}: (i) by ion exchange using a Sr-specific resin and (ii) by reaction with oxygen as reaction gas in a dynamic reaction cell (DRC) of a quadrupole ICP-MS. The relative abundance sensitivity of the ICP-MS was studied systematically and the peak tailing originating from {sup 88}Sr on mass 90 u was found to be about 3 x 10{sup -9}. Detection limits of 4 fg g{sup -1} (0.02 Bq g{sup -1}) were achieved when measuring Sr solutions containing no Zr. In digested uncontaminated soil samples after matrix separation as well as in a solution of 5 {mu}g g{sup -1} Sr and 50 ng g{sup -1} Zr a detection limit of 0.2 pg g{sup -1} soil (1 Bq g{sup -1} soil) was determined. {sup 90}Sr concentrations in three soil samples collected in the vicinity of the Chernobyl Nuclear Power Plant were 4.66 {+-} 0.27, 13.48 {+-} 0.68 and 12.9 {+-} 1.5 pg g{sup -1} corresponding to specific activities of 23.7 {+-} 1.3, 68.6 {+-} 3.5 and 65.6 {+-} 7.8 Bq g{sup -1}, respectively. The ICP-DRC-MS results were compared to the activities measured earlier by radiometry. Although the ICP-DRC-MS is inferior to commonly used radiometric methods with respect to the achievable minimum detectable activity it represents a time- and cost-effective alternative technique for fast monitoring of high-level {sup 90}Sr contamination in environmental or nuclear industrial samples down to activities of about 1 Bq g{sup -1}.

  3. Synthesis and application of magnetic molecularly imprinted polymers in sample preparation.

    Science.gov (United States)

    Huang, Shuyao; Xu, Jianqiao; Zheng, Jiating; Zhu, Fang; Xie, Lijun; Ouyang, Gangfeng

    2018-04-12

    Magnetic molecularly imprinted polymers (MMIPs) have superior advantages in sample pretreatment because of their high selectivity for target analytes and the fast and easy isolation from samples. To meet the demand of both good magnetic property and good extraction performance, MMIPs with various structures, from traditional core-shell structures to novel composite structures with a larger specific surface area and more accessible binding sites, are fabricated by different preparation technologies. Moreover, as the molecularly imprinted polymer (MIP) layers determine the affinity, selectivity, and saturated adsorption amount of MMIPs, the development and innovation of the MIP layer are attracting attention and are reviewed here. Many studies that used MMIPs as sorbents in dispersive solid-phase extraction of complex samples, including environmental, food, and biofluid samples, are summarized. Graphical abstract The application of magnetic molecularly imprinted polymers (MIPs) in the sample preparation procedure improves the analytical performances for complex samples. MITs molecular imprinting technologies.

  4. Strength and Compressibility Characteristics of Reconstituted Organic Soil at Khulna Region of Bangladesh

    OpenAIRE

    Tahia Rabbee; Islam M. Rafizul

    2012-01-01

    This study depicts the experimental investigations into the effect of organic content on the shear strength and compressibility parameters of reconstituted soil. To these attempts, disturbed soil samples were collected from two selected locations of Khulna region. The reconstituted soil having organic content of 5-35 % were prepared in the laboratory to mix at various proportions of inorganic and organic soil at the water content equal to 1.25 times of liquid limits of collected samples .The ...

  5. Estimation of radioactivity in some sand and soil samples

    International Nuclear Information System (INIS)

    Gupta, Monika; Chauhan, R.P.; Garg, Ajay; Kumar, Sushil; Sonkawade, R.G.

    2010-01-01

    Natural radioactivity is composed of the cosmogenic and primordial radionuclides. It is common in the rocks and soil that make up our planet, water and oceans, and in our building materials and homes. Natural radioactivity in sand and soils comes from 238 U and 232 Th series and natural 40 K. Radon is formed from the decay of radium which in turn is formed from uranium. The gaseous radioactive isotope of radon from natural sources has a significant share in the total quantum of natural sources exposure to the human bwings. Gamma radiation from 238 U, 232 Th and 40 K represents the main external source of irradiation of the human body. In the present study, the activity for 238 U, 232 Th and 40 K is found to vary from 45 ± 1.2 to 97 ± 4.9 Bq/kg, 63 ± 2.0 to 132 ± 3.2 Bq/kg and 492 ± 5.9 to 1110 ± 10.5 Bq/kg, respectively in the soil samples while the variations have been observed from 63 ± 3.8 to 65 ± 3.7 Bq/kg, 86 ±2.5 to 96 ± 2.6 Bq/kg and 751 ± 7.7 to 824 ± 8.2 Bq/kg, respectively in the sand samples. (author)

  6. Sample preparation and detection device for infectious agents

    Science.gov (United States)

    Miles, Robin R.; Wang, Amy W.; Fuller, Christopher K.; Lemoff, Asuncion V.; Bettencourt, Kerry A.; Yu, June

    2003-06-10

    A sample preparation and analysis device which incorporates both immunoassays and PCR assays in one compact, field-portable microchip. The device provides new capabilities in fluid and particle control which allows the building of a fluidic chip with no moving parts, thus decreasing fabrication cost and increasing the robustness of the device. The device can operate in a true continuous (not batch) mode. The device incorporates magnetohydrodynamic (MHD) pumps to move the fluid through the system, acoustic mixing and fractionation, dielectropheretic (DEP) sample concentration and purification, and on-chip optical detection capabilities.

  7. Evaluation of the effects of enzyme-based liquid chemical stabilizers on subgrade soils

    CSIR Research Space (South Africa)

    Mgangira, Martin B

    2009-07-01

    Full Text Available The purpose of this study was to asses the strength of enzyme treated soil material. Thus the aim of the paper is to present laboratory results on the effects of two enzyme-based liquid chemicals as soil stabilizers. Soil samples were prepared...

  8. Quantitative Field Testing Rotylenchulus reniformis DNA from Metagenomic Samples Isolated Directly from Soil

    Science.gov (United States)

    Showmaker, Kurt; Lawrence, Gary W.; Lu, Shien; Balbalian, Clarissa; Klink, Vincent P.

    2011-01-01

    A quantitative PCR procedure targeting the β-tubulin gene determined the number of Rotylenchulus reniformis Linford & Oliveira 1940 in metagenomic DNA samples isolated from soil. Of note, this outcome was in the presence of other soil-dwelling plant parasitic nematodes including its sister genus Helicotylenchus Steiner, 1945. The methodology provides a framework for molecular diagnostics of nematodes from metagenomic DNA isolated directly from soil. PMID:22194958

  9. Preliminary characterizations study on three soil samples from the Idaho National Engineering Laboratory warm waste pond

    International Nuclear Information System (INIS)

    Burchett, R.T.; Richardson, W.S.; Hay, S.

    1994-01-01

    Three soil samples (Soil 1,2,and 3) from the Warm Waste Pond (WWP) system at the Test Reactor Area (TRA) of the Idaho National Engineering Laboratory (INEL) were sent to the National Air and Radiation Environmental Laboratory (NAREL) in Montgomery, Alabama, for soil characterization and analysis. Each sample was vigorously washed and separated by particle size using wet sieving and vertical-column hydroclassification. The resulting fractions were analyzed for radioactivity by gamma spectroscopy. The following conclusions are based on the results of these analyses: (1) The three samples examined are dissimilar in many characteristics examined in the study. (2) The optimal parameters for vigorously washing the soil samples are a washing time of 30 min 350 rpm using a liquid-to-solid ratio of 4/1 (volume of water/volume of soil). (3) The only size fraction from Soil 1 that is below the 690 picocuries per gram (pCi/g) cesium-137 Record of Division (ROD) criterion is the +25.4-mm(+1-in) fraction, which represents 17 percent of the total soil. (4) There is no size fraction from Soil 2 that is below the 690 pCi/g cesium-137 criterion. (5) At optimal conditions, at least 66 percent of Soil 3 can be recovered with a cesium-137 activity level below the 690 pCi/g criterion. (6) For Soil 3, lowering the liquid-to-solid ratio from 4/1 to 2/1 during vigorous washing produces a higher weight-percent recovery of soil below the 690 pCi/g criterion. At a liquid-to-solid ratio of 2/1, 76 percent of the soil can be recovered with a concentration below the removal criterion, indicating that attrition followed by particle-size separation represents a potential method for remediation

  10. Measuring environmental change in forest ecosystems by repeated soil sampling: A North American perspective

    Science.gov (United States)

    Gregory B. Lawrence; Ivan J. Fernandez; Daniel D. Richter; Donald S. Ross; Paul W. Hazlett; Scott W. Bailey; Rock Ouimet; Richard A. F. Warby; Arthur H. Johnson; Henry Lin; James M. Kaste; Andrew G. Lapenis; Timothy J. Sullivan

    2013-01-01

    Environmental change is monitored in North America through repeated measurements of weather, stream and river flow, air and water quality, and most recently, soil properties. Some skepticism remains, however, about whether repeated soil sampling can effectively distinguish between temporal and spatial variability, and efforts to document soil change in forest...

  11. 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.

  12. 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

  13. Planning spatial sampling of the soil from an uncertain reconnaissance variogram

    Science.gov (United States)

    Lark, R. Murray; Hamilton, Elliott M.; Kaninga, Belinda; Maseka, Kakoma K.; Mutondo, Moola; Sakala, Godfrey M.; Watts, Michael J.

    2017-12-01

    An estimated variogram of a soil property can be used to support a rational choice of sampling intensity for geostatistical mapping. However, it is known that estimated variograms are subject to uncertainty. In this paper we address two practical questions. First, how can we make a robust decision on sampling intensity, given the uncertainty in the variogram? Second, what are the costs incurred in terms of oversampling because of uncertainty in the variogram model used to plan sampling? To achieve this we show how samples of the posterior distribution of variogram parameters, from a computational Bayesian analysis, can be used to characterize the effects of variogram parameter uncertainty on sampling decisions. We show how one can select a sample intensity so that a target value of the kriging variance is not exceeded with some specified probability. This will lead to oversampling, relative to the sampling intensity that would be specified if there were no uncertainty in the variogram parameters. One can estimate the magnitude of this oversampling by treating the tolerable grid spacing for the final sample as a random variable, given the target kriging variance and the posterior sample values. We illustrate these concepts with some data on total uranium content in a relatively sparse sample of soil from agricultural land near mine tailings in the Copperbelt Province of Zambia.

  14. Optimization of deconvolution software used in the study of spectra of soil samples from Madagascar

    International Nuclear Information System (INIS)

    ANDRIAMADY NARIMANANA, S.F.

    2005-01-01

    The aim of this work is to perform the deconvolution of gamma spectra by using the deconvolution peak program. Synthetic spectra, reference materials and ten soil samples with various U-238 activities from three regions of Madagascar were used. This work concerns : soil sample spectra with low activities of about (47±2) Bq.kg -1 from Ankatso, soil sample spectra with average activities of about (125±2)Bq.kg -1 from Antsirabe and soil sample spectra with high activities of about (21100± 120) Bq.kg -1 from Vinaninkarena. Singlet and multiplet peaks with various intensities were found in each soil spectrum. Interactive Peak Fit (IPF) program in Genie-PC from Canberra Industries allows to deconvoluate many multiplet regions : quartet within 235 keV-242 keV, Pb-214 and Pb-212 within 294 keV -301 keV; Th-232 daughters within 582 keV - 584 keV; Ac-228 within 904 keV -911 keV and within 964 keV-970 keV and Bi-214 within 1401 keV - 1408 keV. Those peaks were used to quantify considered radionuclides. However, IPF cannot resolve Ra-226 peak at 186,1 keV. [fr

  15. Measurement of radon exhalation rate in various building materials and soil samples

    Science.gov (United States)

    Bala, Pankaj; Kumar, Vinod; Mehra, Rohit

    2017-03-01

    Indoor radon is considered as one of the potential dangerous radioactive elements. Common building materials and soil are the major source of this radon gas in the indoor environment. In the present study, the measurement of radon exhalation rate in the soil and building material samples of Una and Hamirpur districts of Himachal Pradesh has been done with solid state alpha track detectors, LR-115 type-II plastic track detectors. The radon exhalation rate for the soil samples varies from 39.1 to 91.2 mBq kg-1 h-1 with a mean value 59.7 mBq kg-1 h-1. Also the radium concentration of the studied area is found and it varies from 30.6 to 51.9 Bq kg-1 with a mean value 41.6 Bq kg-1. The exhalation rate for the building material samples varies from 40.72 (sandstone) to 81.40 mBq kg-1 h-1 (granite) with a mean value of 59.94 mBq kg-1 h-1.

  16. Thorium, uranium and rare earth elements concentration in weathered Japanese soil samples

    International Nuclear Information System (INIS)

    Sahoo, Sarata Kumar; Hosoda, Masahiro; Kamagata, Sadatoshi; Sorimachi, Atsuyuki; Ishikawa, Tetsuo; Tokonami, Shinji; Uchida, Shigeo

    2011-01-01

    The geochemical behavior of thorium, uranium and rare earth elements (REEs) are relatively close to one another while compared to other elements in a geological environment. Radioactive elements like 232 Th and 238 U along with their decay products (e.g. 226 Ra) are present in most environmental matrices and can be transferred to living bodies by different pathways which can lead to the sources of exposure to man. For these reasons, it has been necessary to monitor those natural radionuclides in weathered soil samples to assess the possible hazards. It has been observed that granitic rocks contain higher amounts of U, Th and light REEs compared to other igneous rocks such as basalt and andesites. To better understand the interaction between REEs and soils, the nature of soils must be considered. In this paper, we discussed the distribution pattern of 232 Th and 238 U along with REEs in soil samples of weathered acid rock (granite and ryolite) collected from two prefectures of Japan: (1) Kobe city in Hyogo prefecture and (2) Mutsu city and Higashidori village in Aomori prefecture. (author)

  17. Radioactivity Levels And Gamma Dose Rate In Soil Samples From Federation Of Bosnia And Herzegovina

    International Nuclear Information System (INIS)

    Deljkic, D.; Kadic, I.; Ilic, Z.; Vidic, A.

    2015-01-01

    Activity concentrations of 226Ra, 232Th, 40K and 137Cs in soil samples collected from different regions of Federation of Bosnia and Herzegovina have been measured by gamma-ray spectrometry. The measured activity concentrations for these radionuclides are compared with the reported data from different other countries and it is found that measured activity concentrations are comparable with the worldwide measured average values reported by the UNSCEAR. Experimental results were obtained by using a high-purity germanium (HPGe) detector and gamma - ray spectrometry analysis system at Institute for Public Health FBiH (Radiation Protection Center). The measuring time of all soil samples was 86000 seconds. It was found that the soil specific activity ranges from 24.59 to 161.20 Bq/kg for 226Ra, from 17.60 to 66.45 Bq/kg for 232Th, from 179.50 to 598.04 Bq kg-1 for 40K and from 11.13 to 108.69 Bq/kg for 137Cs with the mean values of 62.34; 46.97; 392.76 and 51.49 Bq/kg, respectively. The radium equivalent activity in all the soil samples is lower than the safe limit (370 Bq/kg), ranges from 63.58 to 287.03 Bq/kg with the mean value of 159.71 Bq/kg. Man-made radionuclide 137Cs is also present in detectable amount in all soil samples. Presence of 137Cs indicates that the samples in this area also receive some fallout from nuclear accident in Chernobyl power plant in 1986. The value of external radiation hazard indices is found to be less than unity (mean value of 0.43). Absorbed dose rates and effective dose equivalents are also determined for the samples. The concentration of radionuclides found in the soil samples during the present study does not pose any potential health hazard to the general public. (author).

  18. Quality evaluation of processed clay soil samples.

    Science.gov (United States)

    Steiner-Asiedu, Matilda; Harrison, Obed Akwaa; Vuvor, Frederick; Tano-Debrah, Kwaku

    2016-01-01

    This study assessed the microbial quality of clay samples sold on two of the major Ghanaian markets. The study was a cross-sectional assessing the evaluation of processed clay and effects it has on the nutrition of the consumers in the political capital town of Ghana. The items for the examination was processed clay soil samples. Staphylococcus spp and fecal coliforms including Klebsiella, Escherichia, and Shigella and Enterobacterspp were isolated from the clay samples. Samples from the Kaneshie market in Accra recorded the highest total viable counts 6.5 Log cfu/g and Staphylococcal count 5.8 Log cfu/g. For fecal coliforms, Madina market samples had the highest count 6.5 Log cfu/g and also recorded the highest levels of yeast and mould. For Koforidua, total viable count was highest in the samples from the Zongo market 6.3 Log cfu/g. Central market samples had the highest count of fecal coliforms 4.6 Log cfu/g and yeasts and moulds 6.5 Log cfu/g. "Small" market recorded the highest staphylococcal count 6.2 Log cfu/g. The water activity of the clay samples were low, and ranged between 0.65±0.01 and 0.66±0.00 for samples collected from Koforidua and Accra respectively. The clay samples were found to contain Klebsiella spp. Escherichia, Enterobacter, Shigella spp. staphylococcus spp., yeast and mould. These have health implications when consumed.

  19. Paraquat-loaded alginate/chitosan nanoparticles: Preparation, characterization and soil sorption studies

    Energy Technology Data Exchange (ETDEWEB)

    Santos Silva, Mariana dos; Sgarbi Cocenza, Daniela [Department of Environmental Engineering, Sao Paulo State University - UNESP, Avenida Tres de Marco, No. 511, CEP 18087-180, Sorocaba, SP (Brazil); Grillo, Renato; Silva de Melo, Nathalie Ferreira [Department of Environmental Engineering, Sao Paulo State University - UNESP, Avenida Tres de Marco, No. 511, CEP 18087-180, Sorocaba, SP (Brazil); Department of Biochemistry, Institute of Biology, State University of Campinas - UNICAMP, Campinas, SP (Brazil); Tonello, Paulo Sergio [Department of Environmental Engineering, Sao Paulo State University - UNESP, Avenida Tres de Marco, No. 511, CEP 18087-180, Sorocaba, SP (Brazil); Camargo de Oliveira, Luciana [Department of Chemistry, UFSCAr, Campus Sorocaba, SP (Brazil); Lopes Cassimiro, Douglas [Institute of Chemistry, Sao Paulo State University - UNESP, Araraquara, SP (Brazil); Rosa, Andre Henrique [Department of Environmental Engineering, Sao Paulo State University - UNESP, Avenida Tres de Marco, No. 511, CEP 18087-180, Sorocaba, SP (Brazil); Fernandes Fraceto, Leonardo, E-mail: leonardo@sorocaba.unesp.br [Department of Environmental Engineering, Sao Paulo State University - UNESP, Avenida Tres de Marco, No. 511, CEP 18087-180, Sorocaba, SP (Brazil); Department of Biochemistry, Institute of Biology, State University of Campinas - UNICAMP, Campinas, SP (Brazil)

    2011-06-15

    Agrochemicals are amongst the contaminants most widely encountered in surface and subterranean hydrological systems. They comprise a variety of molecules, with properties that confer differing degrees of persistence and mobility in the environment, as well as different toxic, carcinogenic, mutagenic and teratogenic potentials, which can affect non-target organisms including man. In this work, alginate/chitosan nanoparticles were prepared as a carrier system for the herbicide paraquat. The preparation and physico-chemical characterization of the nanoparticles was followed by evaluation of zeta potential, pH, size and polydispersion. The techniques employed included transmission electron microscopy, differential scanning calorimetry and Fourier transform infrared spectroscopy. The formulation presented a size distribution of 635 {+-} 12 nm, polydispersion of 0.518, zeta potential of -22.8 {+-} 2.3 mV and association efficiency of 74.2%. There were significant differences between the release profiles of free paraquat and the herbicide associated with the alginate/chitosan nanoparticles. Tests showed that soil sorption of paraquat, either free or associated with the nanoparticles, was dependent on the quantity of organic matter present. The results presented in this work show that association of paraquat with alginate/chitosan nanoparticles alters the release profile of the herbicide, as well as its interaction with the soil, indicating that this system could be an effective means of reducing negative impacts caused by paraquat.

  20. Soil-Transmitted Helminth Eggs Are Present in Soil at Multiple Locations within Households in Rural Kenya.

    Directory of Open Access Journals (Sweden)

    Lauren Steinbaum

    Full Text Available Almost one-quarter of the world's population is infected with soil-transmitted helminths (STH. We conducted a study to determine the prevalence and location of STH-Ascaris, Trichuris, and hookworm spp.-egg contamination in soil within rural household plots in Kenya. Field staff collected soil samples from July to September 2014 from the house entrance and the latrine entrance of households in Kakamega County; additional spatial sampling was conducted at a subset of households (N = 22 samples from 3 households. We analyzed soil samples using a modified version of the US Environmental Protection Agency (EPA method for enumerating Ascaris in biosolids. We found 26.8% of households had one or more species of STH eggs present in the soil in at least one household location (n = 18 out of 67 households, and Ascaris was the most commonly detected STH (19.4%, n = 13 out of 67 households. Prevalence of STH eggs in soil was equally likely at the house entrance (19.4%, N = 67 as at the latrine entrance (11.3%, N = 62 (p = 0.41. We also detected STH eggs at bathing and food preparation areas in the three houses revisited for additional spatial sampling, indicating STH exposure can occur at multiple sites within a household plot, not just near the latrine. The highest concentration of eggs in one house occurred in the child's play area. Our findings suggest interventions to limit child exposure to household soil could complement other STH control strategies.

  1. High-resolution X-ray diffraction with no sample preparation.

    Science.gov (United States)

    Hansford, G M; Turner, S M R; Degryse, P; Shortland, A J

    2017-07-01

    It is shown that energy-dispersive X-ray diffraction (EDXRD) implemented in a back-reflection geometry is extremely insensitive to sample morphology and positioning even in a high-resolution configuration. This technique allows high-quality X-ray diffraction analysis of samples that have not been prepared and is therefore completely non-destructive. The experimental technique was implemented on beamline B18 at the Diamond Light Source synchrotron in Oxfordshire, UK. The majority of the experiments in this study were performed with pre-characterized geological materials in order to elucidate the characteristics of this novel technique and to develop the analysis methods. Results are presented that demonstrate phase identification, the derivation of precise unit-cell parameters and extraction of microstructural information on unprepared rock samples and other sample types. A particular highlight was the identification of a specific polytype of a muscovite in an unprepared mica schist sample, avoiding the time-consuming and difficult preparation steps normally required to make this type of identification. The technique was also demonstrated in application to a small number of fossil and archaeological samples. Back-reflection EDXRD implemented in a high-resolution configuration shows great potential in the crystallographic analysis of cultural heritage artefacts for the purposes of scientific research such as provenancing, as well as contributing to the formulation of conservation strategies. Possibilities for moving the technique from the synchrotron into museums are discussed. The avoidance of the need to extract samples from high-value and rare objects is a highly significant advantage, applicable also in other potential research areas such as palaeontology, and the study of meteorites and planetary materials brought to Earth by sample-return missions.

  2. Determination of elemental in soil samples from Gebeng area using NAA technique

    International Nuclear Information System (INIS)

    Md Suhaimi Elias; Wo, Y.M.; Mohd Suhaimi Hamzah

    2016-01-01

    Rapid development and urbanization will increase number of residence and industrial area. Without proper management and control of pollution, these will give an adverse effect to environment and human life. The objective of this study to identify and quantify key contaminants into the environment of the Gebeng area as a result of industrial and human activities. Gebeng area was gazetted as one of the industrial estate in Pahang state. Assessment of elemental pollution in soil of Gebeng area base on level of concentration, enrichment factor and geo-accumulation index. The enrichment factors (EFs) were determined by the elemental rationing method, whilst the geo-accumulation index (I_g_e_o) by comparing of current to continental crustal average concentration of element. Twenty-seven of soil samples were collected from Gebeng area. Soil samples were analysed by using Neutron Activation Analyses (NAA) technique. The obtained data showed higher concentration of iron (Fe) due to abundance in soil compared to other elements. The results of enrichment factor showed that Gebeng area have enrich with elements of As, Br, Hf, Sb, Th and U. Base on the geo-accumulation index (I_g_e_o) classification, the soil quality of Gebeng area can be classified as class 0, (uncontaminated) to Class 3, (moderately to heavily contaminated). (author)

  3. Application of immunoaffinity columns for different food item samples preparation in micotoxins determination

    Directory of Open Access Journals (Sweden)

    Ćurčić Marijana

    2016-01-01

    Full Text Available In analytical methods used for monitoring of what special attention is paid to sample preparation. Therefore, the objective of this study was testing the efficiency of immunoaffinity columns (IAC that are based on solid phase extraction principles used for samples preparation in determining aflatoxins and ochratoxins. Aflatoxins and ochratoxins concentrations were determined in totally 56 samples of food items: wheat, corn, rice, barley and other grains (19 samples, flour and flour products from grain and additives for the bakery industry (7 samples, fruits and vegetables (3 samples, hazelnut, walnut, almond, coconut flour (4 samples, roasted cocoa beans, peanuts, tea, coffee (16 samples, spices (4 samples and meat and meat products (4 samples. Obtained results indicate advantage of IAC use for sample preparation based on enhanced specificity due to binding of extracted molecules to incorporated specific antibodies and rinsing the rest molecules from sample which could interfere with further analysis. Additional advantage is the usage of small amount of organic solvents and consequently decreased exposure of staff who conduct micotoxins determination. Of special interest is increase in method sensitivity since limit of quantification for aflatoxins and ochratoxins determination method is lower than maximal allowed concentration of these toxines prescribed by national rule book.

  4. HASE - The Helsinki adaptive sample preparation line

    Energy Technology Data Exchange (ETDEWEB)

    Palonen, V., E-mail: vesa.palonen@helsinki.fi [Department of Physics, University of Helsinki, P.O. Box 43, FI-00014 (Finland); Pesonen, A. [Laboratory of Chronology, Finnish Museum of Natural History, P.O. Box 64, FI-00014 (Finland); Herranen, T.; Tikkanen, P. [Department of Physics, University of Helsinki, P.O. Box 43, FI-00014 (Finland); Oinonen, M. [Laboratory of Chronology, Finnish Museum of Natural History, P.O. Box 64, FI-00014 (Finland)

    2013-01-15

    We have designed and built an adaptive sample preparation line with separate modules for combustion, molecular sieve handling, CO{sub 2} gas cleaning, CO{sub 2} storage, and graphitization. The line is also connected to an elemental analyzer. Operation of the vacuum equipment, a flow controller, pressure sensors, ovens, and graphitization reactors are automated with a reliable NI-cRIO real-time system. Stepped combustion can be performed in two ovens at temperatures up to 900 Degree-Sign C. Depending on the application, CuO or O{sub 2}-flow combustion can be used. A flow controller is used to adjust the O{sub 2} flow and pressure during combustion. For environmental samples, a module for molecular sieve regeneration and sample desorption is attached to the line replacing the combustion module. In the storage module, CO{sub 2} samples can be stored behind a gas-tight diaphragm valve and either stored for later graphitization or taken for measurements with separate equipment (AMS gas ion source or a separate mass spectrometer). The graphitization module consists of four automated reactors, capable of graphitizing samples with masses from 3 mg down to 50 {mu}g.

  5. HTI CONE PENETROMETER PROBES PREPARATION DEVELOPMENTAL TESTING REPORT

    Energy Technology Data Exchange (ETDEWEB)

    IWATATE, D.F.

    1998-10-26

    The HTI subsurface characterization task will use the Hanford Cone Penetrometer platform (CPP) to deploy soil sensor and sampling probes into the vadose zone/soils around AX-104 during FY-99. This report provides the data and information compiled during vendor field development tests and laboratory/bench checkout. This document is a vendor deliverable item identified in the ARA Statement of Work HNF-2881, Revision 1. This version of the DTR includes to-be-determined items and some incomplete sections. The Rev. 0 is being released to support the concurrent task of procedure preparation and Qualification Test Plan preparation. Revision 1 is planned to contain all data and information.

  6. Gel-aided sample preparation (GASP)--a simplified method for gel-assisted proteomic sample generation from protein extracts and intact cells.

    Science.gov (United States)

    Fischer, Roman; Kessler, Benedikt M

    2015-04-01

    We describe a "gel-assisted" proteomic sample preparation method for MS analysis. Solubilized protein extracts or intact cells are copolymerized with acrylamide, facilitating denaturation, reduction, quantitative cysteine alkylation, and matrix formation. Gel-aided sample preparation has been optimized to be highly flexible, scalable, and to allow reproducible sample generation from 50 cells to milligrams of protein extracts. This methodology is fast, sensitive, easy-to-use on a wide range of sample types, and accessible to nonspecialists. © 2014 The Authors. PROTEOMICS published by Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Multiresidual determination of pesticides in agricultural soil sample using Quechers extraction methodology

    International Nuclear Information System (INIS)

    Castro Garcia, Consuelo del Pilar

    2011-01-01

    To achieve a sustainable agricultural production there are used different organic and inorganic products, among them we found the fertilizers and pesticides. When they are applied most of the product falls to the ground, generating significant sources of pollution in the areas near the application and depending on the mobility of the pesticide, it can reach more remote areas. That is why it is important to determine the pesticide residues in soil after their application, being the selection of the extraction method crucial for the subsequent traces detection. In the present work there was evaluated the QUECHERS extraction technique, a method used in food but modified for a different and complex matrix like soil in order to achieve acceptable efficiencies multi-residue extraction of 20 pesticides and their subsequent determination by gas chromatography with electron capture and mass detection. The method was applied for the determination of pesticides in three soil samples from an agricultural site with different slopes between them. The Results indicated that 75% of the pesticides tested had acceptable efficiencies, thus meeting the objective of achieving multiresidue determination of pesticides in agricultural soil samples by extraction methodology QUECHERS. Besides, the presence of the fungicide penconazole was only detected in the three samples, being the highest concentration of pesticide found in the area with less slope (V_A_B_A_J_O) (author)

  8. Characterization and forensic analysis of soil samples using laser-induced breakdown spectroscopy (LIBS).

    Science.gov (United States)

    Jantzi, Sarah C; Almirall, José R

    2011-07-01

    A method for the quantitative elemental analysis of surface soil samples using laser-induced breakdown spectroscopy (LIBS) was developed and applied to the analysis of bulk soil samples for discrimination between specimens. The use of a 266 nm laser for LIBS analysis is reported for the first time in forensic soil analysis. Optimization of the LIBS method is discussed, and the results compared favorably to a laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) method previously developed. Precision for both methods was LIBS limits of detection were LIBS method successfully discriminated samples from two different sites in Dade County, FL. Analysis of variance, Tukey's post hoc test and Student's t test resulted in 100% discrimination with no type I or type II errors. Principal components analysis (PCA) resulted in clear groupings of the two sites. A correct classification rate of 99.4% was obtained with linear discriminant analysis using leave-one-out validation. Similar results were obtained when the same samples were analyzed by LA-ICP-MS, showing that LIBS can provide similar information to LA-ICP-MS. In a forensic sampling/spatial heterogeneity study, the variation between sites, between sub-plots, between samples and within samples was examined on three similar Dade sites. The closer the sampling locations, the closer the grouping on a PCA plot and the higher the misclassification rate. These results underscore the importance of careful sampling for geographic site characterization.

  9. Taxonomic and functional profiles of soil samples from Atlantic forest and Caatinga biomes in northeastern Brazil.

    Science.gov (United States)

    Pacchioni, Ralfo G; Carvalho, Fabíola M; Thompson, Claudia E; Faustino, André L F; Nicolini, Fernanda; Pereira, Tatiana S; Silva, Rita C B; Cantão, Mauricio E; Gerber, Alexandra; Vasconcelos, Ana T R; Agnez-Lima, Lucymara F

    2014-06-01

    Although microorganisms play crucial roles in ecosystems, metagenomic analyses of soil samples are quite scarce, especially in the Southern Hemisphere. In this work, the microbial diversity of soil samples from an Atlantic Forest and Caatinga was analyzed using a metagenomic approach. Proteobacteria and Actinobacteria were the dominant phyla in both samples. Among which, a significant proportion of stress-resistant bacteria associated to organic matter degradation was found. Sequences related to metabolism of amino acids, nitrogen, and DNA and stress resistance were more frequent in Caatinga soil, while the forest sample showed the highest occurrence of hits annotated in phosphorous metabolism, defense mechanisms, and aromatic compound degradation subsystems. The principal component analysis (PCA) showed that our samples are close to the desert metagenomes in relation to taxonomy, but are more similar to rhizosphere microbiota in relation to the functional profiles. The data indicate that soil characteristics affect the taxonomic and functional distribution; these characteristics include low nutrient content, high drainage (both are sandy soils), vegetation, and exposure to stress. In both samples, a rapid turnover of organic matter with low greenhouse gas emission was suggested by the functional profiles obtained, reinforcing the importance of preserving natural areas. © 2014 The Authors. MicrobiologyOpen published by John Wiley & Sons Ltd.

  10. Neutron activation and radiometric investigation of Kazakhstan soils

    International Nuclear Information System (INIS)

    Gwozdz, R.; Popov, J.V.; Shishkov, I.A.; Poznyak, V.; Solodukhin, V.P.

    2001-01-01

    Full text: Great diversity of radio-ecological problems requires measurement of materials with vastly differing chemical composition and density, and varying volume. In case of gamma spectrometry such variation in composition, density and volume changes the response of a measuring system quite drastically. A necessary correction is usually achieved by applying one of the four correction methods. The first one is applying a standard with composition as close to the measured sample as possible. The second method needs some previous knowledge about the chemical composition of the sample and a subsequent calculation of the mass absorption coefficient. The third method, an intensity ratio of two gamma lines, can only be applied when an isotope in the investigated sample has two measurable gamma lines. The fourth method consists in an additional gamma transmission measurement, using an isotopic source. Application of the first two methods to samples collected in Kazakhstan is evaluated and the results achieved are described. Instrumental neutron activation analysis by either long, or short irradiation was applied to three groups of samples. The first 15 samples were from the Semipalatinsk area, the next 15 from the area north for the Kara-Tau range. The third group of 5 samples was from the Syr-Darya valley. The Kara-Tau and Syr-Darya samples originate from the area adjacent to an uranium mining site. Only two samples are collected at cultivated soil, all the other are collected at the steppe or semi-desert areas, In the additional group measured there were ten sub-samples of the environmental soil standard, prepared at the Institute of Nuclear Physics. Activation analysis was applied as well to Soil-6 and Soil IAEA-375, two reference materials distributed by IAEA. Determination of concentration of about 40 elements in very sample enabled computation of mass absorption coefficients for all the investigated samples. Results of calculation and experimental testing prove

  11. Nonlinear binding of phenanthrene to the extracted fulvic acid fraction in soil in comparison with other organic matter fractions and to the whole soil sample

    International Nuclear Information System (INIS)

    Liu Wenxin; Xu, Shanshan; Xing, Baoshan; Pan, Bo; Tao, Shu

    2010-01-01

    Fractions of soil organic matter in a natural soil were extracted and sorption (or binding) characteristics of phenanthrene on each fraction and to the whole sample were investigated. The organic carbon normalized single point sorption (or binding) coefficient followed lipid > humin (HM) > humic acid (HA) > fulvic acid (FA) > whole soil sample, while the nonlinear exponent exhibited lipid > FA > HA > whole soil sample > HM. FA showed nonlinear binding of phenanthrene as it often does with other fractions. HM and HA contributed the majority of organic carbon in the soil. The calculated sorption coefficients of the whole soil were about two times greater than the measured values at different equilibrium phenanthrene concentrations. As for phenanthrene, the sorption capacity and nonlinearity of the physically mixed HA-HM mixtures were stronger as compared to the chemically reconstituted HA-HM composite. This was attributed to (besides the conditioning effect of the organic solvents) interactions between HA and HM and acid-base additions during fractionation. - Nonlinear binding of phenanthrene to fulvic acid extracted from soil organic matter was found.

  12. Misrepresentation of hydro-erosional processes in rainfall simulations using disturbed soil samples

    Science.gov (United States)

    Thomaz, Edivaldo L.; Pereira, Adalberto A.

    2017-06-01

    Interrill erosion is a primary soil erosion process which consists of soil detachment by raindrop impact and particle transport by shallow flow. Interill erosion affects other soil erosion sub-processes, e.g., water infiltration, sealing, crusting, and rill initiation. Interrill erosion has been widely studied in laboratories, and the use of a sieved soil, i.e., disturbed soil, has become a standard method in laboratory experiments. The aims of our study are to evaluate the hydro-erosional response of undisturbed and disturbed soils in a laboratory experiment, and to quantify the extent to which hydraulic variables change during a rainstorm. We used a splash pan of 0.3 m width, 0.45 m length, and 0.1 m depth. A rainfall simulation of 58 mm h- 1 lasting for 30 min was conducted on seven replicates of undisturbed and disturbed soils. During the experiment, several hydro-physical parameters were measured, including splashed sediment, mean particle size, runoff, water infiltration, and soil moisture. We conclude that use of disturbed soil samples results in overestimation of interrill processes. Of the nine assessed parameters, four displayed greater responses in the undisturbed soil: infiltration, topsoil shear strength, mean particle size of eroded particles, and soil moisture. In the disturbed soil, five assessed parameters displayed greater responses: wash sediment, final runoff coefficient, runoff, splash, and sediment yield. Therefore, contextual soil properties are most suitable for understanding soil erosion, as well as for defining soil erodibility.

  13. Si(Li)-NaI(Tl) sandwich detector array for measurements of trace radionuclides in soil samples

    International Nuclear Information System (INIS)

    Strauss, M.G.; Sherman, I.S.; Roche, C.T.; Pehl, R.H.

    1986-01-01

    An ultra-sensitive X/γ-ray detector system for assaying trace radioactivity in actinide contaminated soil and ash samples has been developed. The new system consists of an array of 6 large Si(Li) X-ray detectors sensitive on both faces and mounted on edge in a paddle-shaped cryostat with a 14 cm diameter Be window on each side. The paddle, with a sample of the soil placed at each window, is sandwiched between 2 large NaI(Tl) scintillators which suppress the γ background. With X-rays being measured simultaneously from soil in 2 sample holders and background reduced by 50% using anticoincidence, the sensitivity of this detector is 4 times higher than that of conventionally mounted Si(Li) detectors. A soil sample containing 50 pCi/g 239 Pu was measured in 5 min with an uncertainty of 1 and NpLsub(β1) X-ray peaks are resolved thus permitting measurement of trace Pu in the presence of 241 Am. This is the most sensitive and selective detector known for nondestructive assay of radioactivity in soil and other samples. (orig.)

  14. Mechanical impedance of soil crusts and water content in loamy soils

    Science.gov (United States)

    Josa March, Ramon; Verdú, Antoni M. C.; Mas, Maria Teresa

    2013-04-01

    Soil crust development affects soil water dynamics and soil aeration. Soil crusts act as mechanical barriers to fluid flow and, as their mechanical impedance increases with drying, they also become obstacles to seedling emergence. As a consequence, the emergence of seedling cohorts (sensitive seeds) might be reduced. However, this may be of interest to be used as an effective system of weed control. Soil crusting is determined by several factors: soil texture, rain intensity, sedimentation processes, etc. There are different ways to characterize the crusts. One of them is to measure their mechanical impedance (MI), which is linked to their moisture level. In this study, we measured the evolution of the mechanical impedance of crusts formed by three loamy soil types (clay loam, loam and sandy clay loam, USDA) with different soil water contents. The aim of this communication was to establish a mathematical relationship between the crust water content and its MI. A saturated soil paste was prepared and placed in PVC cylinders (50 mm diameter and 10 mm height) arranged on a plastic tray. Previously the plastic tray was sprayed with a hydrophobic liquid to prevent the adherence of samples. The samples on the plastic tray were left to air-dry under laboratory conditions until their IM was measured. To measure IM, a food texture analyzer was used. The equipment incorporates a mobile arm, a load cell to apply force and a probe. The arm moves down vertically at a constant rate and the cylindrical steel probe (4 mm diameter) penetrates the soil sample vertically at a constant rate. The equipment is provided with software to store data (time, vertical distance and force values) at a rate of up to 500 points per second. Water content in crust soil samples was determined as the loss of weight after oven-drying (105°C). From the results, an exponential regression between MI and the water content was obtained (determination coefficient very close to 1). This methodology allows

  15. A Proteomics Sample Preparation Method for Mature, Recalcitrant Leaves of Perennial Plants

    Science.gov (United States)

    Na, Zhang; Chengying, Lao; Bo, Wang; Dingxiang, Peng; Lijun, Liu

    2014-01-01

    Sample preparation is key to the success of proteomics studies. In the present study, two sample preparation methods were tested for their suitability on the mature, recalcitrant leaves of six representative perennial plants (grape, plum, pear, peach, orange, and ramie). An improved sample preparation method was obtained: Tris and Triton X-100 were added together instead of CHAPS to the lysis buffer, and a 20% TCA-water solution and 100% precooled acetone were added after the protein extraction for the further purification of protein. This method effectively eliminates nonprotein impurities and obtains a clear two-dimensional gel electrophoresis array. The method facilitates the separation of high-molecular-weight proteins and increases the resolution of low-abundance proteins. This method provides a widely applicable and economically feasible technology for the proteomic study of the mature, recalcitrant leaves of perennial plants. PMID:25028960

  16. A proteomics sample preparation method for mature, recalcitrant leaves of perennial plants.

    Directory of Open Access Journals (Sweden)

    Deng Gang

    Full Text Available Sample preparation is key to the success of proteomics studies. In the present study, two sample preparation methods were tested for their suitability on the mature, recalcitrant leaves of six representative perennial plants (grape, plum, pear, peach, orange, and ramie. An improved sample preparation method was obtained: Tris and Triton X-100 were added together instead of CHAPS to the lysis buffer, and a 20% TCA-water solution and 100% precooled acetone were added after the protein extraction for the further purification of protein. This method effectively eliminates nonprotein impurities and obtains a clear two-dimensional gel electrophoresis array. The method facilitates the separation of high-molecular-weight proteins and increases the resolution of low-abundance proteins. This method provides a widely applicable and economically feasible technology for the proteomic study of the mature, recalcitrant leaves of perennial plants.

  17. Advances in modern sample preparation techniques using microwaves assisted chemistry for metal species determination (W1)

    International Nuclear Information System (INIS)

    Ponard, O.F.X.

    2002-01-01

    Full text: Sample preparation has long been the bottleneck of environmental analysis for both total and species specific analysis. Digestion, extraction and preparation of the analytes are relying on a series of chemical reactions. The introduction of microwave assisted sample preparation has first been viewed as a mean to accelerate the kinetics of digestion of the matrix for total elements and fast samples preparation procedures. However, the extensive development and success of microwave digestion procedures in total elemental analysis has now allowed to have a larger insight of the perspectives offered by this technique. Microwave technologies now offer to have a precise control of the temperature and indirectly control the reaction kinetics taking place during the sample preparation procedures. Microwave assisted chemistry permits to perform simultaneously the fundamental steps required for metal species extraction and derivatization. The number of sample preparation steps used for organotin or organomercury species have been reduced to one and the total time of sample preparation brought down for a few hours to some minutes. Further, the developments of GC/ICP/MS techniques allow to routinely use speciated isotopic dilution methods has internal probe of the chemical reactions. These new approaches allow us to use the addition of the labeled species for isotopic dilution as a mean to evaluate and follow the chemical processes taking place during the extraction procedure. These procedures will help us to understand and check for the stability of the analytes during the chemistry of the sample preparation procedure and bring some insights of the chemistry taking place during the extraction. Understanding the different mechanisms involved in the sample preparation steps will allow us in return to further improve all theses procedures and bring us to the horizon of 'on-line sample preparation and detection'. (author)

  18. On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR.

    Science.gov (United States)

    Mandal, Abhishek; Boatz, Jennifer C; Wheeler, Travis B; van der Wel, Patrick C A

    2017-03-01

    A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation.

  19. On the use of ultracentrifugal devices for routine sample preparation in biomolecular magic-angle-spinning NMR

    Energy Technology Data Exchange (ETDEWEB)

    Mandal, Abhishek; Boatz, Jennifer C. [University of Pittsburgh School of Medicine, Department of Structural Biology (United States); Wheeler, Travis B. [University of Pittsburgh School of Medicine, Department of Cell Biology (United States); Wel, Patrick C. A. van der, E-mail: vanderwel@pitt.edu [University of Pittsburgh School of Medicine, Department of Structural Biology (United States)

    2017-03-15

    A number of recent advances in the field of magic-angle-spinning (MAS) solid-state NMR have enabled its application to a range of biological systems of ever increasing complexity. To retain biological relevance, these samples are increasingly studied in a hydrated state. At the same time, experimental feasibility requires the sample preparation process to attain a high sample concentration within the final MAS rotor. We discuss these considerations, and how they have led to a number of different approaches to MAS NMR sample preparation. We describe our experience of how custom-made (or commercially available) ultracentrifugal devices can facilitate a simple, fast and reliable sample preparation process. A number of groups have since adopted such tools, in some cases to prepare samples for sedimentation-style MAS NMR experiments. Here we argue for a more widespread adoption of their use for routine MAS NMR sample preparation.

  20. On-chip sample preparation for complete blood count from raw blood.

    Science.gov (United States)

    Nguyen, John; Wei, Yuan; Zheng, Yi; Wang, Chen; Sun, Yu

    2015-03-21

    This paper describes a monolithic microfluidic device capable of on-chip sample preparation for both RBC and WBC measurements from whole blood. For the first time, on-chip sample processing (e.g. dilution, lysis, and filtration) and downstream single cell measurement were fully integrated to enable sample preparation and single cell analysis from whole blood on a single device. The device consists of two parallel sub-systems that perform sample processing and electrical measurements for measuring RBC and WBC parameters. The system provides a modular environment capable of handling solutions of various viscosities by adjusting the length of channels and precisely controlling mixing ratios, and features a new 'offset' filter configuration for increased duration of device operation. RBC concentration, mean corpuscular volume (MCV), cell distribution width, WBC concentration and differential are determined by electrical impedance measurement. Experimental characterization of over 100,000 cells from 10 patient blood samples validated the system's capability for performing on-chip raw blood processing and measurement.

  1. Heavy metal accumulation in soils, plants, and hair samples: an assessment of heavy metal exposure risks from the consumption of vegetables grown on soils previously irrigated with wastewater.

    Science.gov (United States)

    Massaquoi, Lamin Daddy; Ma, Hui; Liu, Xue Hui; Han, Peng Yu; Zuo, Shu-Mei; Hua, Zhong-Xian; Liu, Dian-Wu

    2015-12-01

    It is common knowledge that soils irrigated with wastewater accumulate heavy metals more than those irrigated with cleaner water sources. However, little is known on metal concentrations in soils and cultivars after the cessation of wastewater use. This study assessed the accumulation and health risk of heavy metals 3 years post-wastewater irrigation in soils, vegetables, and farmers' hair. Soils, vegetables, and hair samples were collected from villages previously irrigating with wastewater (experimental villages) and villages with no history of wastewater irrigation (control villages). Soil samples were digested in a mixture of HCL/HNO3/HCLO4/HF. Plants and hair samples were digested in HNO3/HCLO4 mixture. Inductive coupled plasma-optical emission spectrometer (ICP-OES) was used to determine metal concentrations of digested extracts. Study results indicate a persistence of heavy metal concentration in soils and plants from farms previously irrigated with wastewater. In addition, soils previously irrigated with wastewater were severely contaminated with cadmium. Hair metal concentrations of farmers previously irrigating with wastewater were significantly higher (P metal concentrations in hair samples of farmers previously irrigating with wastewater were not associated with current soil metal concentrations. The study concludes that there is a persistence of heavy metals in soils and plants previously irrigated with wastewater, but high metal concentrations in hair samples of farmers cannot be associated with current soil metal concentrations.

  2. Radon mass exhalation rate in soil samples at South Bengaluru city, Karnataka, India

    International Nuclear Information System (INIS)

    Poojitha, C.G.; Pranesha, T.S.; Ganesh, K.E.; Sahoo, B.K.; Sapra, B.K.

    2017-01-01

    Radon mass exhalation rate in soil samples collected from different locations of South Bengaluru city were measured using scintillation based Smart radon thoron monitor (RnDuo). It has been observed that the mass exhalation rate estimated due to presence of radon concentration in soil samples ranges from 39.18 - 265.58 mBq/kg/h with an average value of 115.64 mBq/kg/h. Finally we compare our results with similar investigation from different parts of India. (author)

  3. A comparative study of 232Th and 238U activity estimation in soil samples by gamma spectrometry and neutron activation analysis technique

    International Nuclear Information System (INIS)

    Anilkumar, Rekha; Anilkumar, S.; Narayani, K.; Babu, D.A.R.; Sharma, D.N.

    2012-01-01

    Neutron activation analysis (NAA) is a well-established analytical technique. It has many advantages as compared to the other commonly used techniques. NAA can be performed in a variety of ways depending on the element, its activity level in the sample, interference from the sample matrix and other elements, etc. This technique is used to get high analytical sensitivity and low detection limits (ppm to ppb). The high sensitivity is due to the irradiation at high neutron flux available from the research reactors and the activity measurement is done using high resolution HPGe detectors. In this paper, the activity estimation of soil samples using neutron activation and direct gamma spectrometry methods are compared. Even though the weights of samples considered and samples preparation methods are different for these two methods, the estimated activity values are comparable. (author)

  4. Sr-90 determination in aqueous and soils samples

    International Nuclear Information System (INIS)

    Gonzalez Sintas, Maria F.; Cerchietti, Maria L.; Arguelles, Maria G.

    2009-01-01

    The main objective of this paper is to evaluate the method for Sr-90 determination in aqueous sample and soils. Area and Personal Dosimetry laboratory (DPA) determines the presence of Sr-90 by Liquid Scintillation (LSC) by applying method of the double window and corresponding adjustments. Calibration is performed by standard solutions of 90 Sr/ 90 Y, where spectral 90 Sr and 90 Y zones are optimized. The initial treatment of the liquid samples includes the concentration for evaporation, while the solid ones dissolve for microwave and acidic digestion. The separation of the analyte involves a selective chromatographic extraction. An average efficiency for 90 Sr of 77 ± 1 % was obtained; the factor a/b was 0,85 ± 0,01 and recovery of 82 ± 8 %. The resultant MAD was 0,10 Bq/L in aqueous samples and 0,10 Bq/g in solid samples. (author)

  5. Preparing and measuring ultra-small radiocarbon samples with the ARTEMIS AMS facility in Saclay, France

    Energy Technology Data Exchange (ETDEWEB)

    Delque-Kolic, E., E-mail: emmanuelle.delque-kolic@cea.fr [LMC14, CEA Saclay, Batiment 450 Porte 4E, 91191 Gif sur Yvette (France); Comby-Zerbino, C.; Ferkane, S.; Moreau, C.; Dumoulin, J.P.; Caffy, I.; Souprayen, C.; Quiles, A.; Bavay, D.; Hain, S.; Setti, V. [LMC14, CEA Saclay, Batiment 450 Porte 4E, 91191 Gif sur Yvette (France)

    2013-01-15

    The ARTEMIS facility in Saclay France measures, on average, 4500 samples a year for French organizations working in an array of fields, including environmental sciences, archeology and hydrology. In response to an increasing demand for the isolation of specific soil compounds and organic water fractions, we were motivated to evaluate our ability to reduce microgram samples using our standard graphitization lines and to measure the graphite thus obtained with our 3MV NEC Pelletron AMS. Our reduction facility consists of two fully automated graphitization lines. Each line has 12 reduction reactors with a reduction volume of 18 ml for the first line and 12 ml for the second. Under routine conditions, we determined that we could reduce the samples down to 10 {mu}g of carbon, even if the graphitization yield is consequently affected by the lower sample mass. Our results when testing different Fe/C ratios suggest that an amount of 1.5 mg of Fe powder was ideal (instead of lower amounts of catalyst) to prevent the sample from deteriorating too quickly under the Cs+ beam, and to facilitate pressing procedures. Several sets of microsamples produced from HOxI standard, international references and backgrounds were measured. When measuring {sup 14}C-free wood charcoal and HOxI samples we determined that our modern and dead blanks, due to the various preparation steps, were of 1.1 {+-} 0.8 and 0.2 {+-} 0.1 {mu}g, respectively. The results presented here were obtained for IAEA-C1, {sup 14}C-free wood, IAEA-C6, IAEA-C2 and FIRI C.

  6. Preparing and measuring ultra-small radiocarbon samples with the ARTEMIS AMS facility in Saclay, France

    International Nuclear Information System (INIS)

    Delqué-Količ, E.; Comby-Zerbino, C.; Ferkane, S.; Moreau, C.; Dumoulin, J.P.; Caffy, I.; Souprayen, C.; Quilès, A.; Bavay, D.; Hain, S.; Setti, V.

    2013-01-01

    The ARTEMIS facility in Saclay France measures, on average, 4500 samples a year for French organizations working in an array of fields, including environmental sciences, archeology and hydrology. In response to an increasing demand for the isolation of specific soil compounds and organic water fractions, we were motivated to evaluate our ability to reduce microgram samples using our standard graphitization lines and to measure the graphite thus obtained with our 3MV NEC Pelletron AMS. Our reduction facility consists of two fully automated graphitization lines. Each line has 12 reduction reactors with a reduction volume of 18 ml for the first line and 12 ml for the second. Under routine conditions, we determined that we could reduce the samples down to 10 μg of carbon, even if the graphitization yield is consequently affected by the lower sample mass. Our results when testing different Fe/C ratios suggest that an amount of 1.5 mg of Fe powder was ideal (instead of lower amounts of catalyst) to prevent the sample from deteriorating too quickly under the Cs+ beam, and to facilitate pressing procedures. Several sets of microsamples produced from HOxI standard, international references and backgrounds were measured. When measuring 14 C-free wood charcoal and HOxI samples we determined that our modern and dead blanks, due to the various preparation steps, were of 1.1 ± 0.8 and 0.2 ± 0.1 μg, respectively. The results presented here were obtained for IAEA-C1, 14 C-free wood, IAEA-C6, IAEA-C2 and FIRI C.

  7. Difficulties in preparing a standard sample of uranium metal having traces of nitrogen

    International Nuclear Information System (INIS)

    Toteja, R.S.D.; Jangida, B.L.; Sundaresan, M.

    1991-01-01

    Normally in the analysis of uranium for nitrogen, the nitrides are hydrolysed to give NH 3 and that for standardisation purposes to approximate the closest conditions of analysis of ammonia, NH 4 Cl is added to the sample and the recovery is tested. An appropriate method will be to have a standard sample of uranium with known amounts of nitrogen to be used as reference sample. The present work describes the efforts made in the preparation of such a reference sample and a general assessment of such methods available. In present work, known microamounts of nitrogen in an enclosed volume were allowed to react at a temperature of 773 K with a fixed amount of uranium metal of nitrogen content determined chemically. As the reaction of nitrogen with uranium is essentially a surface reaction, a sample had to be homogenised by allowing the nitrided sample to melt at about 1500 K and allow the nitrogen to diffuse through so that the concentration gradient along the profile will disappear. Attempts were made to prepare such samples in the range to 40 to 100 ppm of nitrogen. The density differences of uranium nitride and uranium metal made this diffusion and homogenisation process difficult. The prepared samples were analysed by the micro-kjeldahl's method and the recoveries tested. The equipment used for the preparation of the nitrided samples, for homogenisation and analysis of the results obtained are detailed in the paper together with the assessment of the general methods. (author). 2 refs., 1 fig., 1 tab

  8. A quantitative method to detect explosives and selected semivolatiles in soil samples by Fourier transform infrared spectroscopy

    International Nuclear Information System (INIS)

    Clapper-Gowdy, M.; Dermirgian, J.; Robitaille, G.

    1995-01-01

    This paper describes a novel Fourier transform infrared (FTIR) spectroscopic method that can be used to rapidly screen soil samples from potentially hazardous waste sites. Samples are heated in a thermal desorption unit and the resultant vapors are collected and analyzed in a long-path gas cell mounted in a FTIR. Laboratory analysis of a soil sample by FTIR takes approximately 10 minutes. This method has been developed to identify and quantify microgram concentrations of explosives in soil samples and is directly applicable to the detection of selected volatile organics, semivolatile organics, and pesticides

  9. The use of atomic absorption spectroscopy to measure arsenic, selenium, molybdenum, and vanadium in water and soil samples from uranium mill tailings sites

    International Nuclear Information System (INIS)

    Hollenbach, M.H.

    1988-01-01

    The Technical Measurements Center (TMC) was established to support the environmental measurement needs of the various DOE remedial action programs. A laboratory intercomparison study conducted by the TMC, using soil and water samples from sites contaminated by uranium mill tailings, indicated large discrepancies in analytical results reported by participating laboratories for arsenic, selenium, molybdenum, and vanadium. The present study was undertaken to investigate the most commonly used analytical techniques for measuring these four elements, ascertain routine and reliable quantification, and assess problems and successes of analysts. Based on a survey of the technical literature, the analytical technique of atomic absorption spectroscopy was selected for detailed study. The application of flame atomic absorption, graphite furnace atomic absorption, and hydride generation atomic absorption to the analysis of tailings-contaminated samples is discussed. Additionally, laboratory sample preparation methods for atomic absorption spectroscopy are presented. The conclusion of this report is that atomic absorption can be used effectively for the determination of arsenic, selenium, molybdenum, and vanadium in water and soil samples if the analyst understands the measurement process and is aware of potential problems. The problem of accurate quantification of arsenic, selenium, molybdenum, and vanadium in water and soil contaminated by waste products from uranium milling operations affects all DOE remedial action programs [Surplus Facilities Management Program (SFMP), Formerly Utilized Site Remedial Action Program (FUSRAP), and Uranium Mill Tailings Remedial Action Program (UMTRAP)], since all include sites where uranium was processed. 96 refs., 9 figs

  10. Solving mercury (Hg) speciation in soil samples by synchrotron X-ray microspectroscopic techniques.

    Science.gov (United States)

    Terzano, Roberto; Santoro, Anna; Spagnuolo, Matteo; Vekemans, Bart; Medici, Luca; Janssens, Koen; Göttlicher, Jörg; Denecke, Melissa A; Mangold, Stefan; Ruggiero, Pacifico

    2010-08-01

    Direct mercury (Hg) speciation was assessed for soil samples with a Hg concentration ranging from 7 up to 240 mg kg(-1). Hg chemical forms were identified and quantified by sequential extractions and bulk- and micro-analytical techniques exploiting synchrotron generated X-rays. In particular, microspectroscopic techniques such as mu-XRF, mu-XRD and mu-XANES were necessary to solve bulk Hg speciation, in both soil fractions soil samples were metacinnabar (beta-HgS), cinnabar (alpha-HgS), corderoite (Hg(3)S(2)Cl(2)), and an amorphous phase containing Hg bound to chlorine and sulfur. The amount of metacinnabar and amorphous phases increased in the fraction soil components was observed. All the observed Hg-species originated from the slow weathering of an inert Hg-containing waste material (K106, U.S. EPA) dumped in the area several years ago, which is changing into a relatively more dangerous source of pollution. Copyright 2010 Elsevier Ltd. All rights reserved.

  11. Skin sample preparation by collagenase digestion for diclofenac quantification using LC-MS/MS after topical application.

    Science.gov (United States)

    Nirogi, Ramakrishna; Padala, Naga Surya Prakash; Boggavarapu, Rajesh Kumar; Kalaikadhiban, Ilayaraja; Ajjala, Devender Reddy; Bhyrapuneni, Gopinadh; Muddana, Nageswara Rao

    2016-06-01

    Skin is the target site to evaluate the pharmacokinetic parameters of topical applications. Sample preparation is one of the influential steps in the bioanalysis of drugs in the skin. Evaluation of dermatopharmacokinetics at preclinical stage is challenging due to lack of proper sample preparation method. There is a need for an efficient sample preparation procedure for quantification of drugs in the skin using LC-MS/MS. The skin samples treated with collagenase followed by homogenization using a bead beater represents a best-fit method resulting in uniform homogenate for reproducible results. A new approach involving enzymatic treatment and mechanical homogenization techniques were evaluated for efficient sample preparation of skin samples in the bioanalysis.

  12. imFASP: An integrated approach combining in-situ filter-aided sample pretreatment with microwave-assisted protein digestion for fast and efficient proteome sample preparation.

    Science.gov (United States)

    Zhao, Qun; Fang, Fei; Wu, Ci; Wu, Qi; Liang, Yu; Liang, Zhen; Zhang, Lihua; Zhang, Yukui

    2016-03-17

    An integrated sample preparation method, termed "imFASP", which combined in-situ filter-aided sample pretreatment and microwave-assisted trypsin digestion, was developed for preparation of microgram and even nanogram amounts of complex protein samples with high efficiency in 1 h. For imFASP method, proteins dissolved in 8 M urea were loaded onto a filter device with molecular weight cut off (MWCO) as 10 kDa, followed by in-situ protein preconcentration, denaturation, reduction, alkylation, and microwave-assisted tryptic digestion. Compared with traditional in-solution sample preparation method, imFASP method generated more protein and peptide identifications (IDs) from preparation of 45 μg Escherichia coli protein sample due to the higher efficiency, and the sample preparation throughput was significantly improved by 14 times (1 h vs. 15 h). More importantly, when the starting amounts of E. coli cell lysate decreased to nanogram level (50-500 ng), the protein and peptide identified by imFASP method were improved at least 30% and 44%, compared with traditional in-solution preparation method, suggesting dramatically higher peptide recovery of imFASP method for trace amounts of complex proteome samples. All these results demonstrate that the imFASP method developed here is of high potential for high efficient and high throughput preparation of trace amounts of complex proteome samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. EG ampersand G Mount Plant, December 1990 and January 1991, D ampersand D soil box sampling

    International Nuclear Information System (INIS)

    1991-04-01

    Six hundred eighty-two (682) containers of soil were generated at Mound Plant between April 1 and October 31, 1990 as a result of the excavation of soils containing plutonium-238 at two ongoing Decontamination and Decommissioning (D ampersand D) Program sites; these areas are known as Area 14, the waste transfer system (WTS) hillside, and Area 17, the Special Metallurgical (SM) Building Area. The soils from these areas are part of the Mound Plant waste stream number AMDM-000000010, Contaminated Soil, and are proposed for shipment to the Nevada Test Site (NTS) for disposal as low-level radioactive waste. These containers of soil are currently in storage at Mound Plant. The purpose of this sampling and analysis was to demonstrate that the D ampersand D soils comply with the waste acceptance requirements of the NTS, as presented In Nevada Test Site Defense Waste Acceptance Criteria, Certification, and Transfer Requirements (DOE 1988). The sealed waste packages, constructed of wood or metal, are currently being stored In Building 31 and at other locations throughout the Mound Plant. For additional historical information concerning the D ampersand D soils, Including waste stream evaluations and past sampling data see the Sampling and Analysis Plan for Mound Plant D ampersand D Soils Packages (EG ampersand G 1991)

  14. Natural radioactivity measurements in soil samples from Hamirpur district, Himachal Pradesh, India

    International Nuclear Information System (INIS)

    Singh, Surinder; Singh, Baldev; Kumar, Ajay

    2003-01-01

    Radium, thorium and potassium analysis have been made in soil samples collected from some villages of Hamirpur district, Himachal Pradesh, India using gamma ray spectrometry. The work has been undertaken keeping in view the health hazard effects of these radioelements in the environment. The results for radium activity are also compared using track etch technique employing radon alpha method developed by Somogyi (Technical reports series no. 310, vol. 1, IAEA, Vienna, 1990, p. 229). The measurements have been taken using 5''x4'' NaI(Tl) detector. The gamma ray lines of 1.46, 1.76 and 2.62 MeV were employed for potassium, radium and thorium analysis. The results for radium content in soil obtained by gamma ray spectrometry agrees with that determined by the track etch technique. The radium activity in soil samples of Hamirpur district is found to be within the safe limits

  15. A review of sample preparation and its influence on pH determination in concrete samples

    International Nuclear Information System (INIS)

    Manso, S.; Aguado, A.

    2017-01-01

    If we are to monitor the chemical processes in cementitious materials, then pH assays in the pore solutions of cement pastes, mortars, and concretes are of key importance. However, there is no standard method that regulates the sample-preparation method for pH determination. The state-of-the-art of different methods for pH determination in cementitious materials is presented in this paper and the influence of sample preparation in each case. Moreover, an experimental campaign compares three different techniques for pH determination. Its results contribute to establishing a basic criterion to help researchers select the most suitable method, depending on the purpose of the research. A simple tool is described for selecting the easiest and the most economic pH determination method, depending on the objective; especially for researchers and those with limited experience in this field.

  16. A user-friendly robotic sample preparation program for fully automated biological sample pipetting and dilution to benefit the regulated bioanalysis.

    Science.gov (United States)

    Jiang, Hao; Ouyang, Zheng; Zeng, Jianing; Yuan, Long; Zheng, Naiyu; Jemal, Mohammed; Arnold, Mark E

    2012-06-01

    Biological sample dilution is a rate-limiting step in bioanalytical sample preparation when the concentrations of samples are beyond standard curve ranges, especially when multiple dilution factors are needed in an analytical run. We have developed and validated a Microsoft Excel-based robotic sample preparation program (RSPP) that automatically transforms Watson worklist sample information (identification, sequence and dilution factor) to comma-separated value (CSV) files. The Freedom EVO liquid handler software imports and transforms the CSV files to executable worklists (.gwl files), allowing the robot to perform sample dilutions at variable dilution factors. The dynamic dilution range is 1- to 1000-fold and divided into three dilution steps: 1- to 10-, 11- to 100-, and 101- to 1000-fold. The whole process, including pipetting samples, diluting samples, and adding internal standard(s), is accomplished within 1 h for two racks of samples (96 samples/rack). This platform also supports online sample extraction (liquid-liquid extraction, solid-phase extraction, protein precipitation, etc.) using 96 multichannel arms. This fully automated and validated sample dilution and preparation process has been applied to several drug development programs. The results demonstrate that application of the RSPP for fully automated sample processing is efficient and rugged. The RSPP not only saved more than 50% of the time in sample pipetting and dilution but also reduced human errors. The generated bioanalytical data are accurate and precise; therefore, this application can be used in regulated bioanalysis.

  17. Geochemical soil sampling for deeply-buried mineralized breccia pipes, northwestern Arizona

    Science.gov (United States)

    Wenrich, K.J.; Aumente-Modreski, R. M.

    1994-01-01

    Thousands of solution-collapse breccia pipes crop out in the canyons and on the plateaus of northwestern Arizona; some host high-grade uranium deposits. The mineralized pipes are enriched in Ag, As, Ba, Co, Cu, Mo, Ni, Pb, Sb, Se, V and Zn. These breccia pipes formed as sedimentary strata collapsed into solution caverns within the underlying Mississippian Redwall Limestone. A typical pipe is approximately 100 m (300 ft) in diameter and extends upward from the Redwall Limestone as much as 1000 m (3000 ft). Unmineralized gypsum and limestone collapses rooted in the Lower Permian Kaibab Limestone or Toroweap Formation also occur throughout this area. Hence, development of geochemical tools that can distinguish these unmineralized collapse structures, as well as unmineralized breccia pipes, from mineralized breccia pipes could significantly reduce drilling costs for these orebodies commonly buried 300-360 m (1000-1200 ft) below the plateau surface. Design and interpretation of soil sampling surveys over breccia pipes are plagued with several complications. (1) The plateau-capping Kaibab Limestone and Moenkopi Formation are made up of diverse lithologies. Thus, because different breccia pipes are capped by different lithologies, each pipe needs to be treated as a separate geochemical survey with its own background samples. (2) Ascertaining true background is difficult because of uncertainties in locations of poorly-exposed collapse cones and ring fracture zones that surround the pipes. Soil geochemical surveys were completed on 50 collapse structures, three of which are known mineralized breccia pipes. Each collapse structure was treated as an independent geochemical survey. Geochemical data from each collapse feature were plotted on single-element geochemical maps and processed by multivariate factor analysis. To contrast the results between geochemical surveys (collapse structures), a means of quantifying the anomalousness of elements at each site was developed. This

  18. Soil pollution and soil protection

    NARCIS (Netherlands)

    Haan, de F.A.M.; Visser-Reijneveld, M.I.

    1996-01-01

    This book was compiled from lecture handouts prepared for the international postgraduate course on soil quality, entitled 'Soil Pollution and Soil Protection' given jointly by the universities of Wageningen (The Netherlands), Gent and Leuven (Belgium), under the auspices of the international

  19. Compact low temperature scanning tunneling microscope with in-situ sample preparation capability

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jungdae [Department of Physics, The University of Texas, Austin, Texas 78712 (United States); Department of Physics and EHSRC, University of Ulsan, Ulsan 680-749 (Korea, Republic of); Nam, Hyoungdo; Schroeder, Allan; Shih, Chih-Kang, E-mail: shih@physics.utexas.edu [Department of Physics, The University of Texas, Austin, Texas 78712 (United States); Qin, Shengyong [Department of Physics, The University of Texas, Austin, Texas 78712 (United States); Department of Physics, University of Science and Technology of China, Hefei, Anhui 230026 (China); ICQD, Hefei National Laboratory for Physical Sciences at the Microscale, University of Science and Technology of China, Hefei, Anhui 230026 (China); Kim, Sang-ui [Department of Physics and EHSRC, University of Ulsan, Ulsan 680-749 (Korea, Republic of); Eom, Daejin [Korea Research Institute of Standards and Science, Daejeon 305-340 (Korea, Republic of)

    2015-09-15

    We report on the design of a compact low temperature scanning tunneling microscope (STM) having in-situ sample preparation capability. The in-situ sample preparation chamber was designed to be compact allowing quick transfer of samples to the STM stage, which is ideal for preparing temperature sensitive samples such as ultra-thin metal films on semiconductor substrates. Conventional spring suspensions on the STM head often cause mechanical issues. To address this problem, we developed a simple vibration damper consisting of welded metal bellows and rubber pads. In addition, we developed a novel technique to ensure an ultra-high-vacuum (UHV) seal between the copper and stainless steel, which provides excellent reliability for cryostats operating in UHV. The performance of the STM was tested from 2 K to 77 K by using epitaxial thin Pb films on Si. Very high mechanical stability was achieved with clear atomic resolution even when using cryostats operating at 77 K. At 2 K, a clean superconducting gap was observed, and the spectrum was easily fit using the BCS density of states with negligible broadening.

  20. Compact low temperature scanning tunneling microscope with in-situ sample preparation capability.

    Science.gov (United States)

    Kim, Jungdae; Nam, Hyoungdo; Qin, Shengyong; Kim, Sang-ui; Schroeder, Allan; Eom, Daejin; Shih, Chih-Kang

    2015-09-01

    We report on the design of a compact low temperature scanning tunneling microscope (STM) having in-situ sample preparation capability. The in-situ sample preparation chamber was designed to be compact allowing quick transfer of samples to the STM stage, which is ideal for preparing temperature sensitive samples such as ultra-thin metal films on semiconductor substrates. Conventional spring suspensions on the STM head often cause mechanical issues. To address this problem, we developed a simple vibration damper consisting of welded metal bellows and rubber pads. In addition, we developed a novel technique to ensure an ultra-high-vacuum (UHV) seal between the copper and stainless steel, which provides excellent reliability for cryostats operating in UHV. The performance of the STM was tested from 2 K to 77 K by using epitaxial thin Pb films on Si. Very high mechanical stability was achieved with clear atomic resolution even when using cryostats operating at 77 K. At 2 K, a clean superconducting gap was observed, and the spectrum was easily fit using the BCS density of states with negligible broadening.

  1. The effect of short-range spatial variability on soil sampling uncertainty

    Energy Technology Data Exchange (ETDEWEB)

    Perk, Marcel van der [Department of Physical Geography, Utrecht University, P.O. Box 80115, 3508 TC Utrecht (Netherlands)], E-mail: m.vanderperk@geo.uu.nl; De Zorzi, Paolo; Barbizzi, Sabrina; Belli, Maria [Agenzia per la Protezione dell' Ambiente e per i Servizi Tecnici (APAT), Servizio Laboratori, Misure ed Attivita di Campo, Via di Castel Romano, 100-00128 Roma (Italy); Fajgelj, Ales; Sansone, Umberto [International Atomic Energy Agency (IAEA), Agency' s Laboratories Seibersdorf, A-1400 Vienna (Austria); Jeran, Zvonka; Jacimovic, Radojko [Jozef Stefan Institute, Jamova 39, 1000 Ljubljana (Slovenia)

    2008-11-15

    This paper aims to quantify the soil sampling uncertainty arising from the short-range spatial variability of elemental concentrations in the topsoils of agricultural, semi-natural, and contaminated environments. For the agricultural site, the relative standard sampling uncertainty ranges between 1% and 5.5%. For the semi-natural area, the sampling uncertainties are 2-4 times larger than in the agricultural area. The contaminated site exhibited significant short-range spatial variability in elemental composition, which resulted in sampling uncertainties of 20-30%.

  2. The effect of short-range spatial variability on soil sampling uncertainty.

    Science.gov (United States)

    Van der Perk, Marcel; de Zorzi, Paolo; Barbizzi, Sabrina; Belli, Maria; Fajgelj, Ales; Sansone, Umberto; Jeran, Zvonka; Jaćimović, Radojko

    2008-11-01

    This paper aims to quantify the soil sampling uncertainty arising from the short-range spatial variability of elemental concentrations in the topsoils of agricultural, semi-natural, and contaminated environments. For the agricultural site, the relative standard sampling uncertainty ranges between 1% and 5.5%. For the semi-natural area, the sampling uncertainties are 2-4 times larger than in the agricultural area. The contaminated site exhibited significant short-range spatial variability in elemental composition, which resulted in sampling uncertainties of 20-30%.

  3. Application of instrument neutron-activation analysis in a comparative investigation of soil samples

    Energy Technology Data Exchange (ETDEWEB)

    Dimitrov, D. (Institute po Kriminalistika i Kriminologiya, Sofia (Bulgaria))

    1983-01-01

    A quantitative measurement of the contents of 17 chemical elements in soil samples, collected using the existing network from the surface of five cultivated areas in Bulgaria has been carried out. The values obtained have been used to calculate the evaluations psub(i) of the dispersions and for the ordering of the chemical elements according to their importance in criminology. The possibility for criminological comparison of single soil samples using the contents of the five most important elements - Th, Fe, Sc, Ce and Mn has been shown.

  4. Automated cellular sample preparation using a Centrifuge-on-a-Chip.

    Science.gov (United States)

    Mach, Albert J; Kim, Jae Hyun; Arshi, Armin; Hur, Soojung Claire; Di Carlo, Dino

    2011-09-07

    The standard centrifuge is a laboratory instrument widely used by biologists and medical technicians for preparing cell samples. Efforts to automate the operations of concentration, cell separation, and solution exchange that a centrifuge performs in a simpler and smaller platform have had limited success. Here, we present a microfluidic chip that replicates the functions of a centrifuge without moving parts or external forces. The device operates using a purely fluid dynamic phenomenon in which cells selectively enter and are maintained in microscale vortices. Continuous and sequential operation allows enrichment of cancer cells from spiked blood samples at the mL min(-1) scale, followed by fluorescent labeling of intra- and extra-cellular antigens on the cells without the need for manual pipetting and washing steps. A versatile centrifuge-analogue may open opportunities in automated, low-cost and high-throughput sample preparation as an alternative to the standard benchtop centrifuge in standardized clinical diagnostics or resource poor settings.

  5. Ultra-High-Throughput Sample Preparation System for Lymphocyte Immunophenotyping Point-of-Care Diagnostics.

    Science.gov (United States)

    Walsh, David I; Murthy, Shashi K; Russom, Aman

    2016-10-01

    Point-of-care (POC) microfluidic devices often lack the integration of common sample preparation steps, such as preconcentration, which can limit their utility in the field. In this technology brief, we describe a system that combines the necessary sample preparation methods to perform sample-to-result analysis of large-volume (20 mL) biopsy model samples with staining of captured cells. Our platform combines centrifugal-paper microfluidic filtration and an analysis system to process large, dilute biological samples. Utilizing commercialization-friendly manufacturing methods and materials, yielding a sample throughput of 20 mL/min, and allowing for on-chip staining and imaging bring together a practical, yet powerful approach to microfluidic diagnostics of large, dilute samples. © 2016 Society for Laboratory Automation and Screening.

  6. Area G perimeter surface-soil and single-stage water sampling. Environmental surveillance for fiscal year 95. Progress report

    International Nuclear Information System (INIS)

    Childs, M.; Conrad, R.

    1997-09-01

    ESH-19 personnel collected soil and single-stage water samples around the perimeter of Area G at Los Alamos National Laboratory (LANL) during FY 95 to characterize possible radionuclide movement out of Area G through surface water and entrained sediment runoff. Soil samples were analyzed for tritium, total uranium, isotopic plutonium, americium-241, and cesium-137. The single-stage water samples were analyzed for tritium and plutonium isotopes. All radiochemical data was compared with analogous samples collected during FY 93 and 94 and reported in LA-12986 and LA-13165-PR. Six surface soils were also submitted for metal analyses. These data were included with similar data generated for soil samples collected during FY 94 and compared with metals in background samples collected at the Area G expansion area

  7. Highly Reproducible Automated Proteomics Sample Preparation Workflow for Quantitative Mass Spectrometry.

    Science.gov (United States)

    Fu, Qin; Kowalski, Michael P; Mastali, Mitra; Parker, Sarah J; Sobhani, Kimia; van den Broek, Irene; Hunter, Christie L; Van Eyk, Jennifer E

    2018-01-05

    Sample preparation for protein quantification by mass spectrometry requires multiple processing steps including denaturation, reduction, alkylation, protease digestion, and peptide cleanup. Scaling these procedures for the analysis of numerous complex biological samples can be tedious and time-consuming, as there are many liquid transfer steps and timed reactions where technical variations can be introduced and propagated. We established an automated sample preparation workflow with a total processing time for 96 samples of 5 h, including a 2 h incubation with trypsin. Peptide cleanup is accomplished by online diversion during the LC/MS/MS analysis. In a selected reaction monitoring (SRM) assay targeting 6 plasma biomarkers and spiked β-galactosidase, mean intraday and interday cyclic voltammograms (CVs) for 5 serum and 5 plasma samples over 5 days were samples repeated on 3 separate days had total CVs below 20%. Similar results were obtained when the workflow was transferred to a second site: 93% of peptides had CVs below 20%. An automated trypsin digestion workflow yields uniformly processed samples in less than 5 h. Reproducible quantification of peptides was observed across replicates, days, instruments, and laboratory sites, demonstrating the broad applicability of this approach.

  8. Soil deflation analyses from wind erosion events

    Directory of Open Access Journals (Sweden)

    Lenka Lackóová

    2015-09-01

    Full Text Available There are various methods to assess soil erodibility for wind erosion. This paper focuses on aggregate analysis by a laser particle sizer ANALYSETTE 22 (FRITSCH GmbH, made to determine the size distribution of soil particles detached by wind (deflated particles. Ten soil samples, trapped along the same length of the erosion surface (150–155 m but at different wind speeds, were analysed. The soil was sampled from a flat, smooth area without vegetation cover or soil crust, not affected by the impact of windbreaks or other barriers, from a depth of maximum 2.5 cm. Prior to analysis the samples were prepared according to the relevant specifications. An experiment was also conducted using a device that enables characterisation of the vertical movement of the deflated material. The trapped samples showed no differences in particle size and the proportions of size fractions at different hourly average wind speeds. It was observed that most of particles travelling in saltation mode (size 50–500 μm – 58–70% – moved vertically up to 26 cm above the soil surface. At greater heights, particles moving in suspension mode (floating in the air; size < 100 μm accounted for up to 90% of the samples. This result suggests that the boundary between the two modes of the vertical movement of deflated soil particles lies at about 25 cm above the soil surface.

  9. Focused-microwave-assisted sample preparation (M8)

    International Nuclear Information System (INIS)

    Nobrega, J.A.; Santos, D.M.; Trevizan, L.C.; Costa, L.M.; Nogueira, A.R.A.

    2002-01-01

    Full text: Focused-microwave-assisted sample preparation is a suitable strategy when dealing with high masses of organic samples. However, the final acid concentration of the digestate can difficult routine analytical measurements using spectroscopic techniques. Acids could be evaporated, but this step could be slow even when using microwave-assisted heating and requires a scrubber system for acid vapor collection and neutralization. We are investigating two procedures to decrease the acid concentration of digestates. The first one is based on acid vapor phase digestion of samples contained in PTFE devices' inserted into the microwave flask. The acid solution is heated by absorption of microwave radiation, then the acid vapor partially condenses in the upper part of the reaction flask and it is partially collected in each sample container. Calcium, Fe, Mg, Mn, and Zn were quantitatively recovered in samples of animal and vegetable tissues. Better recoveries were attained when adding a small volume of sodium hypochlorite to the sample. This effect is probably related to the generation of chlorine in the sample container after collecting condensed acid. The second procedure developed is based on the gradual addition of liquid samples to a previously heated acid digestion mixture. This procedure was successfully applied for digestion of milk, fruit juices, and red wine. The main advantage is the possibility of digesting up to four-fold more sample using up to ten-fold lower amounts of concentrated acids. Results obtained using both digestion procedures and measurements by ICP-OES with axial view will be presented. (author)

  10. [Application of simulated annealing method and neural network on optimizing soil sampling schemes based on road distribution].

    Science.gov (United States)

    Han, Zong-wei; Huang, Wei; Luo, Yun; Zhang, Chun-di; Qi, Da-cheng

    2015-03-01

    Taking the soil organic matter in eastern Zhongxiang County, Hubei Province, as a research object, thirteen sample sets from different regions were arranged surrounding the road network, the spatial configuration of which was optimized by the simulated annealing approach. The topographic factors of these thirteen sample sets, including slope, plane curvature, profile curvature, topographic wetness index, stream power index and sediment transport index, were extracted by the terrain analysis. Based on the results of optimization, a multiple linear regression model with topographic factors as independent variables was built. At the same time, a multilayer perception model on the basis of neural network approach was implemented. The comparison between these two models was carried out then. The results revealed that the proposed approach was practicable in optimizing soil sampling scheme. The optimal configuration was capable of gaining soil-landscape knowledge exactly, and the accuracy of optimal configuration was better than that of original samples. This study designed a sampling configuration to study the soil attribute distribution by referring to the spatial layout of road network, historical samples, and digital elevation data, which provided an effective means as well as a theoretical basis for determining the sampling configuration and displaying spatial distribution of soil organic matter with low cost and high efficiency.

  11. The impact of mineral composition on compressibility of saturated soils

    OpenAIRE

    Dolinar, Bojana

    2012-01-01

    This article analyses the impact of soils` mineral composition on their compressibility. Physical and chemical properties of minerals which influence the quantity of intergrain water in soils and, consequently, the compressibility of soils are established by considering the previous theoretical findings. Test results obtained on artificially prepared samples are used to determine the analytical relationship between the water content and stress state, depending on the mineralogical properties ...

  12. Study of lead pollution in air, soil and water samples of Quetta city

    International Nuclear Information System (INIS)

    Khan, M.; Khan, G.M.; Akbar, S.; Panezai, M.A.; Haq, Z.U.

    2011-01-01

    This study briefly presents the collected data of lead pollution in the environment of Quetta City in Balochistan, Pakistan. The samples were collected from different sites. The analysis of lead was carried out in underground water samples, the exhaust of different vehicles, roadside and sewage soils from selected points of Quetta City. The average discharge resulted in deposition by motorcycles (29.12 g/h), cars (44.47 g/h), wagons (176.54 g/h) and buses (141.52 g/h). The maximum deposition was 222.96 g/h from auto-rickshaws. The value for lead in smoke of different vehicles seems quite high when extrapolated to the large number of such vehicles for a longer time. The concentration of lead in roadside soil varied from 73.3 mg/kg (T and T closed colony) to 731.9 mg/kg (Sirki road bus-stop). The average content of lead in sewage soil of City Nala is 1250.6 mg/kg. The level of lead was more than WHO standards for such soils. The lead quantity in all 24 tube- well water samples, was slightly above the WHO standards (10 macro g/L).The results of this study were comparable to similar study in twin cities of Rawalpindi and islamabad. (author)

  13. Ionic liquids: solvents and sorbents in sample preparation.

    Science.gov (United States)

    Clark, Kevin D; Emaus, Miranda N; Varona, Marcelino; Bowers, Ashley N; Anderson, Jared L

    2018-01-01

    The applications of ionic liquids (ILs) and IL-derived sorbents are rapidly expanding. By careful selection of the cation and anion components, the physicochemical properties of ILs can be altered to meet the requirements of specific applications. Reports of IL solvents possessing high selectivity for specific analytes are numerous and continue to motivate the development of new IL-based sample preparation methods that are faster, more selective, and environmentally benign compared to conventional organic solvents. The advantages of ILs have also been exploited in solid/polymer formats in which ordinarily nonspecific sorbents are functionalized with IL moieties in order to impart selectivity for an analyte or analyte class. Furthermore, new ILs that incorporate a paramagnetic component into the IL structure, known as magnetic ionic liquids (MILs), have emerged as useful solvents for bioanalytical applications. In this rapidly changing field, this Review focuses on the applications of ILs and IL-based sorbents in sample preparation with a special emphasis on liquid phase extraction techniques using ILs and MILs, IL-based solid-phase extraction, ILs in mass spectrometry, and biological applications. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Sampling and analysis of soil from the old F-Area effluent ditch and its surrounding wetlands

    International Nuclear Information System (INIS)

    Dixon, K.L.

    1994-06-01

    Four surface soil samples were collected from the wetlands at the old F-Area effluent ditch. All samples were collected near shallow well point locations except FHB012, which was collected from the effluent ditch stream sediment. Samples were analyzed for metals, Target Compound List volatile organic compounds, and gross radiological indicators. Barium, beryllium, and zinc were detected in all four samples and antimony was detected in three of four samples. These metals occur naturally in the wetland soils at the SRS. Comparisons of metals concentrations were male to concentration ranges taken from background wetland soil samples. These comparison, showed that barium and beryllium concentrations were within expected ranges while zinc and antimony concentrations were elevated above expected concentration ranges. Volatile organic compounds were detected in all four samples. Detected compounds included acetone, 2-butanone, chloromethane, cis-1,2-dichloroethene, and toluene. The only radionuclide detected in a significant quantities was tritium which was detected in all four samples

  15. Development of a sample preparation system for AMS radiocarbon dating at CRICH, Korea

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Myung-Jin; Lee, Byeong-Cheol; Lim, Eun-Soo [Cultural Research Institute of Chungcheong Heritage, Gongju (Korea, Republic of); Hong, Duk-Geun [Kangwon National University, Chuncheon (Korea, Republic of); Park, Soon-Bal [Chungnam National University, Daejeon (Korea, Republic of); Youn, Min-Young [Seoul National University, Seoul (Korea, Republic of)

    2010-01-15

    We developed a sample preparation system for radiocarbon dating by using AMS measurement at Cultural Research Institute of Chungcheong Heritage, Korea. From the investigation of the reduction process, the optimum graphitization temperature was chosen as 625 .deg. C. Using Aldrich graphite powder of 0.75 {+-} 0.023 pMC, the background value of our preparation system was controlled at a low level. The robustness against chemical treatment and contamination was also observed from samples of Oxalic acid II and IAEA-C4. The resultant values, 134.04 {+-} 0.99 pMC and 0.38 {+-} 0.043 pMC, were in good agreement with the consensus values. Based on comparison, our conventional ages agreed very well with those of Beta Analytic Co. and SNU-AMS. No memory effect existed in the preparation system. Therefore, we concluded that the sample preparation system was operated in a stable manner and that the basic radiocarbon dating procedures were completely verified.

  16. Soil preparation and nutrient losses by erosion in the culture cucumber

    Directory of Open Access Journals (Sweden)

    Amaral Sobrinho Nelson Moura Brasil do

    2005-01-01

    Full Text Available Minimum tillage reportedly reduce erosion, avoid soil degradation and improve crop productivity. This study aimed to determine how tillage operations may affect either nutrient accumulation or nutrient losses by erosion. The study was, carried out from December, 2000 to March, 2001, in the watershed of the Caetés River, in Rio de Janeiro State, Brazil (22º25'43"S, 43º25'07"W. The experiment was set up in sandy clay Kandiudult soil, 60% slope, under cucumber (Cucumis sativus L. crop. Soil samples were collected before planting and after harvest, on 22.0 X 4.0 m Greeoff plots. After each rainfall, fine sediments carried by runoff were deposited into two collecting tanks in a row, installed at the end of each plot, and were later dried, weighed and stored for analyses. Treatments (n = 4 were characterized by different tillage systems: (i downhill plowing followed by the burning of crop residues (DPB; (ii downhill plowing with no burning of the crop residues (DPNB; (iii animal traction contour plowing, with strips of guinea grass planted at a spacing of 7.0 m (AT; and (iv minimum tillage (MT. Samples of the soil-plowed layer were collected before planting and after harvest, between the rows and from the plants. Total concentration of Ca, Mg, K and P were determined after extraction with nitric perchloride digestion. Labile P and exchangeable K were extracted with the Mehlich 1 extractant solution. The MT system reduced losses of both exchangeable bases (15% and P (8%, and affected the distribution of labile and organic P. Crop residues left on soil surface in the MT system, resulted in increased organic matter content. Downhill plowing, the most used tillage operation in the region, resulted in the greatest losses of Ca, Mg, K, and P.

  17. TCLP Preparation and Analysis of K East Basin Composite Sludge Samples

    International Nuclear Information System (INIS)

    Silvers, K.L.; Wagner, J.J.; Steele, R.T.

    2000-01-01

    Sludge samples from the Hanford K East Basin were analyzed by the Toxicity Characterization Leaching Procedure (TCLP) to assist in the appropriate Resource Conservation and Recovery Act (RCIL4) designation of this material. Sludge samples were collected by Fluor Hanford, Inc. using the consolidated sludge sampling system (system that allows collection of a single sample from multiple sample locations). These samples were shipped to the Postirradiation Testing Laboratory (PTL, 327 Building) and then transferred to the Pacific Northwest National Laboratory (PNNL) Radiochemical Processing Laboratory (RPL, 325 Building) for recovery and testing. Two sludge composites were prepared, using the consolidated sludge samples, to represent K East canister sludge (sample KC Can Comp) and K East floor sludge (sample KC Floor Comp). Each composite was extracted in duplicate and analyzed in duplicate following pre-approved(a) TCLP extraction and analyses procedures. In addition, these samples and duplicates were analyzed for total RCRA metals (via acid digestion preparation). The work was conducted in accordance with the requirements of the Hanford Analytical Quality Assurance Requirements Document (HASQARD). A PNNL Quality Assurance Program compliant with J HASQARD was implemented for this effort. The results from the TCLP analyses showed that all RCRA metal concentrations were less than the TCLP limits for both the canister and floor composite samples and their respective duplicates

  18. Capacitive deionization on-chip as a method for microfluidic sample preparation

    NARCIS (Netherlands)

    Roelofs, Susan Helena; Kim, Bumjoo; Eijkel, Jan C.T.; Han, Jongyoon; van den Berg, Albert; Odijk, Mathieu

    2015-01-01

    Desalination as a sample preparation step is essential for noise reduction and reproducibility of mass spectrometry measurements. A specific example is the analysis of proteins for medical research and clinical applications. Salts and buffers that are present in samples need to be removed before

  19. Soil sampling and analytical strategies for mapping fallout in nuclear emergencies based on the Fukushima Dai-ichi Nuclear Power Plant accident

    International Nuclear Information System (INIS)

    Onda, Yuichi; Kato, Hiroaki; Hoshi, Masaharu; Takahashi, Yoshio; Nguyen, Minh-Long

    2015-01-01

    The Fukushima Dai-ichi Nuclear Power Plant (FDNPP) accident resulted in extensive radioactive contamination of the environment via deposited radionuclides such as radiocesium and 131 I. Evaluating the extent and level of environmental contamination is critical to protecting citizens in affected areas and to planning decontamination efforts. However, a standardized soil sampling protocol is needed in such emergencies to facilitate the collection of large, tractable samples for measuring gamma-emitting radionuclides. In this study, we developed an emergency soil sampling protocol based on preliminary sampling from the FDNPP accident-affected area. We also present the results of a preliminary experiment aimed to evaluate the influence of various procedures (e.g., mixing, number of samples) on measured radioactivity. Results show that sample mixing strongly affects measured radioactivity in soil samples. Furthermore, for homogenization, shaking the plastic sample container at least 150 times or disaggregating soil by hand-rolling in a disposable plastic bag is required. Finally, we determined that five soil samples within a 3 m × 3-m area are the minimum number required for reducing measurement uncertainty in the emergency soil sampling protocol proposed here. - Highlights: • Emergency soil sampling protocol was proposed for nuclear hazards. • Various sampling procedures were tested and evaluated in Fukushima area. • Soil sample mixing procedure was of key importance for measured radioactivity. • Minimum number of sampling was determined for reducing measurement uncertainty

  20. Radon exhalation rates from soil and sand samples collected from the vicinity of Yamuna river

    International Nuclear Information System (INIS)

    Garg, A.K.; Sushil Kumar; Chauhan, Pooja; Chauhan, R.P.

    2011-01-01

    Soil, sand and stones are the most popular building materials for Indian dwellings. Radon is released into ambient air from these materials due to ubiquitous uranium and radium in them, thus increasing the airborne radon concentration. The radioactivity in sand and soils is related to radioactivity in the rocks from which they are formed. These materials contain varying amount of uranium. In the present investigation, the radon emanated from soil and sand samples from different locations in the vicinity of Yamuna river has been estimated. The samples have been collected from different locations near the Yamuna river. The samples collecting sites are from Yamunanagar in Haryana to Delhi. The radon concentration in different samples has been calculated, based upon the data, the mass and the surface exhalation rates of radon emanated from them have also been calculated