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Sample records for terrestrial samples determined

  1. The determination of environmental levels of uranium and thorium series isotopes and 137Cs in aquatic and terrestrial samples

    International Nuclear Information System (INIS)

    Wilkinson, P.

    1985-01-01

    This publication details the analytical methods used at the Freshwater Institute for the radiochemical analysis of aquatic and terrestrial samples. Sample collection methods are described with emphasis on water sampling. A detailed 'Calculations' section contains the mathematical formulae used to determine the absolute activity of each isotope analyzed. 25 refs

  2. Neutron activation determination of noble metals in samples of terrestrial and cosmic origin using microfire assay concentration

    International Nuclear Information System (INIS)

    Kolesov, G.M.; Sapozhnikov, D.Yu.

    1995-01-01

    The effects of various factors (composition of mixture, relationship between the mass of mixture and sample, value of the Ni:S ratio, fusion time, and temperature) on the conditions of the fire assay concentration of the noble metals with nickel sulfide were investigated, and a method proposed for their quantitative separation from different geological matrices with a neutron activation determination for up to 10 -1 -10 -3 ppb. The proposed method is used to analyse geological samples, i.e. ores, stones, iron meteorites, chromites, soil and lunar rocks. (author)

  3. Sampling supraglacial debris thickness using terrestrial photogrammetry

    Science.gov (United States)

    Nicholson, Lindsey; Mertes, Jordan

    2017-04-01

    The melt rate of debris-covered ice differs to that of clean ice primarily as a function of debris thickness. The spatial distribution of supraglacial debris thickness must therefore be known in order to understand how it is likely to impact glacier behaviour, and meltwater contribution to local hydrological resources and global sea level rise. However, practical means of determining debris cover thickness remain elusive. In this study we explore the utility of terrestrial photogrammetry to produce high resolution, scaled and texturized digital terrain models of debris cover exposures above ice cliffs as a means of quantifying and characterizing debris thickness. Two Nikon D5000 DSLRs with Tamron 100mm lenses were used to photograph a sample area of the Ngozumpa glacier in the Khumbu Himal of Nepal in April 2016. A Structure from Motion workflow using Agisoft Photoscan software was used to generate a surface models with <10cm resolution. A Trimble Geo7X differential GPS with Zephyr antenna, along with a local base station, was used to precisely measure marked ground control points to scale the photogrammetric surface model. Measurements of debris thickness along the exposed cliffline were made from this scaled model, assuming that the ice surface at the debris-ice boundary is horizontal, and these data are compared to 50 manual point measurements along the same clifftops. We conclude that sufficiently high resolution photogrammetry, with precise scaling information, provides a useful means to determine debris thickness at clifftop exposures. The resolution of the possible measurements depends on image resolution, the accuracy of the ground control points and the computational capacity to generate centimetre scale surface models. Application of such techniques to sufficiently high resolution imagery from UAV-borne cameras may offer a powerful means of determining debris thickness distribution patterns over debris covered glacier termini.

  4. Sampling Terrestrial Environments for Bacterial Polyketides

    Directory of Open Access Journals (Sweden)

    Patrick Hill

    2017-04-01

    Full Text Available Bacterial polyketides are highly biologically active molecules that are frequently used as drugs, particularly as antibiotics and anticancer agents, thus the discovery of new polyketides is of major interest. Since the 1980s discovery of polyketides has slowed dramatically due in large part to the repeated rediscovery of known compounds. While recent scientific and technical advances have improved our ability to discover new polyketides, one key area has been under addressed, namely the distribution of polyketide-producing bacteria in the environment. Identifying environments where producing bacteria are abundant and diverse should improve our ability to discover (bioprospect new polyketides. This review summarizes for the bioprospector the state-of-the-field in terrestrial microbial ecology. It provides insight into the scientific and technical challenges limiting the application of microbial ecology discoveries for bioprospecting and summarizes key developments in the field that will enable more effective bioprospecting. The major recent efforts by researchers to sample new environments for polyketide discovery is also reviewed and key emerging environments such as insect associated bacteria, desert soils, disease suppressive soils, and caves are highlighted. Finally strategies for taking and characterizing terrestrial samples to help maximize discovery efforts are proposed and the inclusion of non-actinomycetal bacteria in any terrestrial discovery strategy is recommended.

  5. Sampling methods for terrestrial amphibians and reptiles.

    Science.gov (United States)

    Paul Stephen Corn; R. Bruce. Bury

    1990-01-01

    Methods described for sampling amphibians and reptiles in Douglas-fir forests in the Pacific Northwest include pitfall trapping, time-constrained collecting, and surveys of coarse woody debris. The herpetofauna of this region differ in breeding and nonbreeding habitats and vagility, so that no single technique is sufficient for a community study. A combination of...

  6. Trends and Future Challenges in Sampling the Deep Terrestrial Biosphere

    Directory of Open Access Journals (Sweden)

    Michael J Wilkins

    2014-09-01

    Full Text Available Research in the deep terrestrial biosphere is driven by interest in novel biodiversity and metabolisms, biogeochemical cycling, and the impact of human activities on this ecosystem. As this interest continues to grow, it is important to ensure that when subsurface investigations are proposed, materials recovered from the subsurface are sampled and preserved in an appropriate manner to limit contamination and ensure preservation of accurate microbial, geochemical, and mineralogical signatures. On February 20th, 2014, a workshop on Trends and Future Challenges in Sampling The Deep Subsurface was coordinated in Columbus, Ohio by The Ohio State University and West Virginia University faculty, and sponsored by The Ohio State University and the Sloan Foundation’s Deep Carbon Observatory. The workshop aims were to identify and develop best practices for the collection, preservation, and analysis of terrestrial deep rock samples. This document summarizes the information shared during this workshop.

  7. Trends and future challenges in sampling the deep terrestrial biosphere.

    Science.gov (United States)

    Wilkins, Michael J; Daly, Rebecca A; Mouser, Paula J; Trexler, Ryan; Sharma, Shihka; Cole, David R; Wrighton, Kelly C; Biddle, Jennifer F; Denis, Elizabeth H; Fredrickson, Jim K; Kieft, Thomas L; Onstott, Tullis C; Peterson, Lee; Pfiffner, Susan M; Phelps, Tommy J; Schrenk, Matthew O

    2014-01-01

    Research in the deep terrestrial biosphere is driven by interest in novel biodiversity and metabolisms, biogeochemical cycling, and the impact of human activities on this ecosystem. As this interest continues to grow, it is important to ensure that when subsurface investigations are proposed, materials recovered from the subsurface are sampled and preserved in an appropriate manner to limit contamination and ensure preservation of accurate microbial, geochemical, and mineralogical signatures. On February 20th, 2014, a workshop on "Trends and Future Challenges in Sampling The Deep Subsurface" was coordinated in Columbus, Ohio by The Ohio State University and West Virginia University faculty, and sponsored by The Ohio State University and the Sloan Foundation's Deep Carbon Observatory. The workshop aims were to identify and develop best practices for the collection, preservation, and analysis of terrestrial deep rock samples. This document summarizes the information shared during this workshop.

  8. A survey of natural terrestrial and airborne radionuclides in moss samples from the peninsular Thailand.

    Science.gov (United States)

    Wattanavatee, Komrit; Krmar, Miodrag; Bhongsuwan, Tripob

    2017-10-01

    The aim of this study was to determine the activity concentrations of natural terrestrial radionuclides ( 238 U, 226 Ra, 232 Th and 40 K) and airborne radionuclides ( 210 Pb, 210 Pb ex and 7 Be) in natural terrestrial mosses. The collected moss samples (46) representing 17 species were collected from 17 sampling localities in the National Parks and Wildlife Sanctuaries of Thailand, situated in the mountainous areas between the northern and the southern ends of peninsular Thailand (∼7-12 °N, 99-102 °E). Activity concentrations of radionuclides in the samples were measured using a low background gamma spectrometer. The results revealed non-uniform spatial distributions of all the radionuclides in the study area. Principal component analysis and cluster analysis revealed two distinct origins for the studied radionuclides, and furthermore, the Pearson correlations were strong within 226 Ra, 232 Th, 238 U and 40 K as well as within 210 Pb and 210 Pb ex , but there was no significant correlation between these two groups. Also 7 Be was uncorrelated to the others, as expected due to different origins of the airborne and terrestrial radionuclides. The radionuclide activities of moss samples varied by moss species, topography, geology, and meteorology of each sampling area. The observed abnormally high concentrations of some radionuclides probably indicate that the concentrations of airborne and terrestrial radionuclides in moss samples were directly related to local geological features of the sampling site, or that high levels of 7 Be were most probably linked with topography and regional NE monsoonal winds from mainland China. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. Uranium determinations by 133Xe in terrestrial zircon, apatite and chromite; comparative study of thermal releases of fissiogenic xenon from terrestrial and meteoritic minerals

    International Nuclear Information System (INIS)

    Sakamoto, K.; Hamajima, Y.; Itoh, K.; Yamazaki, K.

    1980-01-01

    Terrestrial zircon and apatite, as examples of uranium rich refractory minerals, and chromite, also highly refractory but uranium poor, were neutron-irradiated for their 133 Xe release studies. Uranium determination by 133 Xe was found not to be successful in these refractory samples, due to incomplete fissiogenic-xenon release at 1600 deg C as revealed by stepwise heating experiment. In these terrestrial materials the high temperature release peaks appeared at >=1500 deg C, but in meteoritic whitlockite and chromite values of 1000 approximately 1200 deg C were reported. (author)

  10. Sodium sampling and impurities determination

    International Nuclear Information System (INIS)

    Docekal, J.; Kovar, C.; Stuchlik, S.

    1980-01-01

    Samples may be obtained from tubes in-built in the sodium facility and further processed or they are taken into crucibles, stored and processed later. Another sampling method is a method involving vacuum distillation of sodium, thus concentrating impurities. Oxygen is determined by malgamation, distillation or vanadium balance methods. Hydrogen is determined by the metal diaphragm extraction, direct extraction or amalgamation methods. Carbon is determined using dry techniques involving burning a sodium sample at 1100 degC or using wet techniques by dissolving the sample with an acid. Trace amounts of metal impurities are determined after dissolving sodium in ethanol. The trace metals are concentrated and sodium excess is removed. (M.S.)

  11. Sample size determination and power

    CERN Document Server

    Ryan, Thomas P, Jr

    2013-01-01

    THOMAS P. RYAN, PhD, teaches online advanced statistics courses for Northwestern University and The Institute for Statistics Education in sample size determination, design of experiments, engineering statistics, and regression analysis.

  12. Excess 129Xe in terrestrial samples: A non-primordial hypothesis

    International Nuclear Information System (INIS)

    Caffee, M.W.; Hudson, G.B.

    1987-03-01

    Excesses of 129 Xe relative to the isotopic composition in air are observed in some terrestrial samples. Traditionally these 129 Xe excesses have been thought to be related to 129 I that was present in abundance in the early solar system. We propose an alternative hypothesis to explain terrestrial 129 Xe excesses based on the production of 129 I from the spontaneous fission of 238 U

  13. NEON terrestrial field observations: designing continental scale, standardized sampling

    Science.gov (United States)

    R. H. Kao; C.M. Gibson; R. E. Gallery; C. L. Meier; D. T. Barnett; K. M. Docherty; K. K. Blevins; P. D. Travers; E. Azuaje; Y. P. Springer; K. M. Thibault; V. J. McKenzie; M. Keller; L. F. Alves; E. L. S. Hinckley; J. Parnell; D. Schimel

    2012-01-01

    Rapid changes in climate and land use and the resulting shifts in species distributions and ecosystem functions have motivated the development of the National Ecological Observatory Network (NEON). Integrating across spatial scales from ground sampling to remote sensing, NEON will provide data for users to address ecological responses to changes in climate, land use,...

  14. Origin of spherule samples recovered from antarctic ice sheet-Terrestrial or extraterrestrial?

    Energy Technology Data Exchange (ETDEWEB)

    Sekimoto, Shun; Takamiya, Koichi; Shibata, Seiichi [Research Reactor Institute, Kyoto University, Osaka (Japan); Kobayashi, Takayuki [College of Humanities and Sciences, Nihon University, Tokyo (Japan); Ebihara, Mitsuru [Dept. of Chemistry, Tokyo Metropolitan University, Tokyo (Japan)

    2016-04-15

    Thirty-eight spherules from the Antarctic ice sheet were analyzed using neutron activation analysis under two different conditions to investigate their origin. In almost all of these spherules, the contents of iron, cobalt, and manganese were determined to be 31% to 88%, 17 mg/kg to 810 mg/kg, and 0.017% to 7%, respectively. A detectable iridium content of 0.84 mg/kg was found in only one spherule, which was judged to be extraterrestrial in origin. A comparison of elemental compositions of the Antarctic spherules analyzed in this study with those of deep-sea sediment spherules and those of terrestrial materials revealed that most of the Antarctic spherules except for the sample in which iridium was detected could not be identified as extraterrestrial in origin.

  15. Concepts in sample size determination

    Directory of Open Access Journals (Sweden)

    Umadevi K Rao

    2012-01-01

    Full Text Available Investigators involved in clinical, epidemiological or translational research, have the drive to publish their results so that they can extrapolate their findings to the population. This begins with the preliminary step of deciding the topic to be studied, the subjects and the type of study design. In this context, the researcher must determine how many subjects would be required for the proposed study. Thus, the number of individuals to be included in the study, i.e., the sample size is an important consideration in the design of many clinical studies. The sample size determination should be based on the difference in the outcome between the two groups studied as in an analytical study, as well as on the accepted p value for statistical significance and the required statistical power to test a hypothesis. The accepted risk of type I error or alpha value, which by convention is set at the 0.05 level in biomedical research defines the cutoff point at which the p value obtained in the study is judged as significant or not. The power in clinical research is the likelihood of finding a statistically significant result when it exists and is typically set to >80%. This is necessary since the most rigorously executed studies may fail to answer the research question if the sample size is too small. Alternatively, a study with too large a sample size will be difficult and will result in waste of time and resources. Thus, the goal of sample size planning is to estimate an appropriate number of subjects for a given study design. This article describes the concepts in estimating the sample size.

  16. Terrestrial gamma radiation baseline mapping using ultra low density sampling methods

    International Nuclear Information System (INIS)

    Kleinschmidt, R.; Watson, D.

    2016-01-01

    Baseline terrestrial gamma radiation maps are indispensable for providing basic reference information that may be used in assessing the impact of a radiation related incident, performing epidemiological studies, remediating land contaminated with radioactive materials, assessment of land use applications and resource prospectivity. For a large land mass, such as Queensland, Australia (over 1.7 million km 2 ), it is prohibitively expensive and practically difficult to undertake detailed in-situ radiometric surveys of this scale. It is proposed that an existing, ultra-low density sampling program already undertaken for the purpose of a nationwide soil survey project be utilised to develop a baseline terrestrial gamma radiation map. Geoelement data derived from the National Geochemistry Survey of Australia (NGSA) was used to construct a baseline terrestrial gamma air kerma rate map, delineated by major drainage catchments, for Queensland. Three drainage catchments (sampled at the catchment outlet) spanning low, medium and high radioelement concentrations were selected for validation of the methodology using radiometric techniques including in-situ measurements and soil sampling for high resolution gamma spectrometry, and comparative non-radiometric analysis. A Queensland mean terrestrial air kerma rate, as calculated from the NGSA outlet sediment uranium, thorium and potassium concentrations, of 49 ± 69 nGy h −1 (n = 311, 3σ 99% confidence level) is proposed as being suitable for use as a generic terrestrial air kerma rate background range. Validation results indicate that catchment outlet measurements are representative of the range of results obtained across the catchment and that the NGSA geoelement data is suitable for calculation and mapping of terrestrial air kerma rate. - Highlights: • A baseline terrestrial air kerma map of Queensland, Australia was developed using geochemical data from a major drainage catchment ultra-low density sampling program

  17. Application of the Monte Carlo method for the efficiency calibration of CsI and NaI detectors for gamma-ray measurements from terrestrial samples

    International Nuclear Information System (INIS)

    Baccouche, S.; Al-Azmi, D.; Karunakara, N.; Trabelsi, A.

    2012-01-01

    Gamma-ray measurements in terrestrial/environmental samples require the use of high efficient detectors because of the low level of the radionuclide activity concentrations in the samples; thus scintillators are suitable for this purpose. Two scintillation detectors were studied in this work; CsI(Tl) and NaI(Tl) with identical size for measurement of terrestrial samples for performance study. This work describes a Monte Carlo method for making the full-energy efficiency calibration curves for both detectors using gamma-ray energies associated with the decay of naturally occurring radionuclides 137 Cs (661 keV), 40 K (1460 keV), 238 U ( 214 Bi, 1764 keV) and 232 Th ( 208 Tl, 2614 keV), which are found in terrestrial samples. The magnitude of the coincidence summing effect occurring for the 2614 keV emission of 208 Tl is assessed by simulation. The method provides an efficient tool to make the full-energy efficiency calibration curve for scintillation detectors for any samples geometry and volume in order to determine accurate activity concentrations in terrestrial samples. - Highlights: ► CsI (Tl) and NaI (Tl) detectors were studied for the measurement of terrestrial samples. ► Monte Carlo method was used for efficiency calibration using natural gamma emitting terrestrial radionuclides. ► The coincidence summing effect occurring for the 2614 keV emission of 208 Tl is assessed by simulation.

  18. Terrestrial gamma radiation baseline mapping using ultra low density sampling methods.

    Science.gov (United States)

    Kleinschmidt, R; Watson, D

    2016-01-01

    Baseline terrestrial gamma radiation maps are indispensable for providing basic reference information that may be used in assessing the impact of a radiation related incident, performing epidemiological studies, remediating land contaminated with radioactive materials, assessment of land use applications and resource prospectivity. For a large land mass, such as Queensland, Australia (over 1.7 million km(2)), it is prohibitively expensive and practically difficult to undertake detailed in-situ radiometric surveys of this scale. It is proposed that an existing, ultra-low density sampling program already undertaken for the purpose of a nationwide soil survey project be utilised to develop a baseline terrestrial gamma radiation map. Geoelement data derived from the National Geochemistry Survey of Australia (NGSA) was used to construct a baseline terrestrial gamma air kerma rate map, delineated by major drainage catchments, for Queensland. Three drainage catchments (sampled at the catchment outlet) spanning low, medium and high radioelement concentrations were selected for validation of the methodology using radiometric techniques including in-situ measurements and soil sampling for high resolution gamma spectrometry, and comparative non-radiometric analysis. A Queensland mean terrestrial air kerma rate, as calculated from the NGSA outlet sediment uranium, thorium and potassium concentrations, of 49 ± 69 nGy h(-1) (n = 311, 3σ 99% confidence level) is proposed as being suitable for use as a generic terrestrial air kerma rate background range. Validation results indicate that catchment outlet measurements are representative of the range of results obtained across the catchment and that the NGSA geoelement data is suitable for calculation and mapping of terrestrial air kerma rate. Crown Copyright © 2015. Published by Elsevier Ltd. All rights reserved.

  19. Substrate attributes determine gait in a terrestrial gastropod.

    Science.gov (United States)

    McKee, Amberle; Voltzow, Janice; Pernet, Bruno

    2013-02-01

    Some terrestrial gastropods are able to move using two gaits: adhesive crawling, where the entire foot is separated from the substrate only by a thin layer of mucus and the snail leaves a continuous mucus trail; and loping, where regions of the foot arch above the substrate and the snail leaves a discontinuous mucus trail. Loping has been interpreted as a means of rapidly escaping predators. We found that the pulmonate Cornu aspersum moved using adhesive crawling on dry acrylic or glass substrates, but loped on dry concrete or wood. Loping snails did not move more rapidly than snails using adhesive crawling. Snails moving on concrete secreted a greater volume of pedal mucus per area of trail than those moving on acrylic; locomotion on concrete thus requires greater expenditure of mucus than does locomotion on acrylic. Because loping snails deposit a smaller area of mucus per distance traveled than do snails using adhesive crawling, loping may conserve mucus when moving on porous, absorbent substrates. Members of several other terrestrial pulmonate taxa can also lope on concrete, suggesting that this plasticity in gait is widespread among terrestrial snails.

  20. 2017 Annual Terrestrial Sampling Plan for Sandia National Laboratories/New Mexico on Kirtland Air Force Base

    Energy Technology Data Exchange (ETDEWEB)

    Griffith, Stacy R. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2017-02-01

    The 2017 Annual Terrestrial Sampling Plan for Sandia National Laboratories/New Mexico on Kirtland Air Force Base has been prepared in accordance with the “Letter of Agreement Between Department of Energy, National Nuclear Security Administration, Sandia Field Office (DOE/NNSA/SFO) and 377th Air Base Wing (ABW), Kirtland Air Force Base (KAFB) for Terrestrial Sampling” (signed January 2017), Sandia National Laboratories, New Mexico (SNL/NM). The Letter of Agreement requires submittal of an annual terrestrial sampling plan.

  1. 2018 Annual Terrestrial Sampling Plan for Sandia National Laboratories/New Mexico on Kirtland Air Force Base.

    Energy Technology Data Exchange (ETDEWEB)

    Griffith, Stacy R. [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2018-01-01

    The 2018 Annual Terrestrial Sampling Plan for Sandia National Laboratories/New Mexico on Kirtland Air Force Base has been prepared in accordance with the “Letter of Agreement Between Department of Energy, National Nuclear Security Administration, Sandia Field Office (DOE/NNSA/SFO) and 377th Air Base Wing (ABW), Kirtland Air Force Base (KAFB) for Terrestrial Sampling” (signed January 2017), Sandia National Laboratories, New Mexico (SNL/NM). The Letter of Agreement requires submittal of an annual terrestrial sampling plan.

  2. Comparison of Directionally Solidified Samples Solidified Terrestrially and Aboard the International Space Station

    Science.gov (United States)

    Angart, S.; Lauer, M.; Tewari, S. N.; Grugel, R. N.; Poirier, D. R.

    2014-01-01

    This article reports research that has been carried out under the aegis of NASA as part of a collaboration between ESA and NASA for solidification experiments on the International Space Station (ISS). The focus has been on the effect of convection on the microstructural evolution and macrosegregation in hypoeutectic Al-Si alloys during directional solidification (DS). Terrestrial DS-experiments have been carried out at Cleveland State University (CSU) and under microgravity on the International Space Station (ISS). The thermal processing-history of the experiments is well defined for both the terrestrially processed samples and the ISS-processed samples. As of this writing, two dendritic metrics was measured: primary dendrite arm spacings and primary dendrite trunk diameters. We have observed that these dendrite-metrics of two samples grown in the microgravity environment show good agreements with models based on diffusion controlled growth and diffusion controlled ripening, respectively. The gravity-driven convection (i.e., thermosolutal convection) in terrestrially grown samples has the effect of decreasing the primary dendrite arm spacings and causes macrosegregation. Dendrite trunk diameters also show differences between the earth- and space-grown samples. In order to process DS-samples aboard the ISS, the dendritic seed crystals were partially remelted in a stationary thermal gradient before the DS was carried out. Microstructural changes and macrosegregation effects during this period are described and have modeled.

  3. [Determination by high performance chromatography, steroid saponins in a biologically active food supplements containing the extract of Tribulus terrestris].

    Science.gov (United States)

    Kozlova, O I; Perederiaev, O I; Ramenskaia, G V

    2011-01-01

    Steroidal saponins are bioactive substances of Tribulus terrestris and can be used to assess the quality of raw materials and processed products from them. For this purpose has been developed the method of qualitative and quantitative determination of steroidal saponins by high performance liquid chromatography with spectrophotometric and mass-selective detection and optimal conditions of sample preparation (70% methanol extraction with sonication and heating); also has been studied steroidal saponins composition of Tribulus terrestris (protodioscin, tribulosaponin B, metilprotodiostsin, terrestrozin H, prototribestin, gracillin and others were found).

  4. Comparison between EDXRF and FAAS for Zn determination in terrestrial molluscs

    International Nuclear Information System (INIS)

    Melo, Julyanne T.B.; Cantinha, Rebeca S.; Santos, Mariana L.O.; Santos, Katarine M.B.; Franca, Elvis J.; Melo, Ana M.M.A.

    2015-01-01

    Even with the most advanced analytical techniques, achieving the true values of a given analyte in a sample cannot be an easy task. Energy Dispersive X-Ray Fluorescence (EDXRF) and Flame Atomic Absorption Spectrometry (FAAS) have been widely used for analysis of the chemical composition of biological matrices in environmental studies. However, depending on the sample matrix, a combination of techniques could be needed for the correct determination of the analyte. Zinc distribution in Littoraria angulifera and Melampus coffea is quite dependent on the environment, so that, diverse methods could be necessary to evaluate the chemical composition of these mollusks. This study aimed at the comparison between EDXRF and FAAS techniques for determining Zn in the soft tissues of terrestrial mollusks. The animals were collected in three mangroves in the State of Pernambuco, Brazil. After shell removal, tissues were lyophilized and milled in a mortar. Test portions of 500 mg were analyzed by EDXRF, followed by chemical treatment for FAAS analysis. For the quality of the analytical procedure, the standard reference material SRM 2976 Mussel Tissue was analyzed together with the samples. The results for the analysis of the certified reference material SRM 2976 indicated the quality of the analytical procedure for both techniques. Adjusted-R 2 between EDXRF and FAAS results was 0.95, indicating a good equivalence of Zn determination by both techniques. However, some improvement of EDXRF determination could be necessary because of the tendency of lower results compared to FAAS, probably related to spectral interferences during the analysis. (author)

  5. Glacier Snowline Determination from Terrestrial Laser Scanning Intensity Data

    Directory of Open Access Journals (Sweden)

    Hannah Prantl

    2017-07-01

    Full Text Available Accurately identifying the extent of surface snow cover on glaciers is important for extrapolating end of year mass balance measurements, constraining the glacier surface radiative energy balance and evaluating model simulations of snow cover. Here, we use auxiliary information from Riegl VZ-6000 Terrestrial Laser Scanner (TLS return signals to accurately map the snow cover over a glacier throughout an ablation season. Three classification systems were compared, and we find that supervised classification based on TLS signal intensity alone is outperformed by a rule-based classification employing intensity, surface roughness and an associated optical image, which achieves classification accuracy of 68–100%. The TLS intensity signal shows no meaningful relationship with surface or bulk snow density. Finally, we have also compared our Snow Line Altitude (SLA derived from TLS with SLA derived from the model output, as well as one Landsat image. The results of the model output track the SLA from TLS well, however with a positive bias. In contrast, automatic Landsat-derived SLA slightly underestimates the SLA from TLS. To conclude, we demonstrate that the snow cover extent can be mapped successfully using TLS, although the snow mass remains elusive.

  6. A strategy to sample nutrient dynamics across the terrestrial-aquatic interface at NEON sites

    Science.gov (United States)

    Hinckley, E. S.; Goodman, K. J.; Roehm, C. L.; Meier, C. L.; Luo, H.; Ayres, E.; Parnell, J.; Krause, K.; Fox, A. M.; SanClements, M.; Fitzgerald, M.; Barnett, D.; Loescher, H. W.; Schimel, D.

    2012-12-01

    The construction of the National Ecological Observatory Network (NEON) across the U.S. creates the opportunity for researchers to investigate biogeochemical transformations and transfers across ecosystems at local-to-continental scales. Here, we examine a subset of NEON sites where atmospheric, terrestrial, and aquatic observations will be collected for 30 years. These sites are located across a range of hydrological regimes, including flashy rain-driven, shallow sub-surface (perched, pipe-flow, etc), and deep groundwater, which likely affect the chemical forms and quantities of reactive elements that are retained and/or mobilized across landscapes. We present a novel spatial and temporal sampling design that enables researchers to evaluate long-term trends in carbon, nitrogen, and phosphorus biogeochemical cycles under these different hydrological regimes. This design focuses on inputs to the terrestrial system (atmospheric deposition, bulk precipitation), transfers (soil-water and groundwater sources/chemistry), and outputs (surface water, and evapotranspiration). We discuss both data that will be collected as part of the current NEON design, as well as how the research community can supplement the NEON design through collaborative efforts, such as providing additional datasets, including soil biogeochemical processes and trace gas emissions, and developing collaborative research networks. Current engagement with the research community working at the terrestrial-aquatic interface is critical to NEON's success as we begin construction, to ensure that high-quality, standardized and useful data are not only made available, but inspire further, cutting-edge research.

  7. COMPARATIVE AND QUANTITATIVE DETERMINATION OF QUERCETIN AND RUTIN IN TRIBULUS TERRESTRIS L. FRUITS FROM DIFFERENT SEASONAL AND GEOGRAPHICAL POPULATIONS OF SOUTH INDIA

    OpenAIRE

    Suresh Reddy Yanala* and D. Sathyanarayana

    2018-01-01

    The objective of the present research work was comparative and quantitative determination of quercetin and rutin in Tribulus terrestirs fruits from different geographical regions and seasons by using HPLC. The Tribulus terrestris fruit samples collected from three different geographical regions of south India in June and December months. In the current HPLC analysis flavonoids in Tribulus terrestris Linn fruits were quantified at 360 nm with help of peak area by comparing to a calibration cur...

  8. Application of the Monte Carlo method for the efficiency calibration of CsI and NaI detectors for gamma-ray measurements from terrestrial samples

    Energy Technology Data Exchange (ETDEWEB)

    Baccouche, S., E-mail: souad.baccouche@cnstn.rnrt.tn [UR-MDTN, National Center for Nuclear Sciences and Technology, Technopole Sidi Thabet, 2020 Sidi Thabet (Tunisia); Al-Azmi, D., E-mail: ds.alazmi@paaet.edu.kw [Department of Applied Sciences, College of Technological Studies, Public Authority for Applied Education and Training, Shuwaikh, P.O. Box 42325, Code 70654 (Kuwait); Karunakara, N., E-mail: karunakara_n@yahoo.com [University Science Instrumentation Centre, Mangalore University, Mangalagangotri 574199 (India); Trabelsi, A., E-mail: adel.trabelsi@fst.rnu.tn [UR-MDTN, National Center for Nuclear Sciences and Technology, Technopole Sidi Thabet, 2020 Sidi Thabet (Tunisia); UR-UPNHE, Faculty of Sciences of Tunis, El-Manar University, 2092 Tunis (Tunisia)

    2012-01-15

    Gamma-ray measurements in terrestrial/environmental samples require the use of high efficient detectors because of the low level of the radionuclide activity concentrations in the samples; thus scintillators are suitable for this purpose. Two scintillation detectors were studied in this work; CsI(Tl) and NaI(Tl) with identical size for measurement of terrestrial samples for performance study. This work describes a Monte Carlo method for making the full-energy efficiency calibration curves for both detectors using gamma-ray energies associated with the decay of naturally occurring radionuclides {sup 137}Cs (661 keV), {sup 40}K (1460 keV), {sup 238}U ({sup 214}Bi, 1764 keV) and {sup 232}Th ({sup 208}Tl, 2614 keV), which are found in terrestrial samples. The magnitude of the coincidence summing effect occurring for the 2614 keV emission of {sup 208}Tl is assessed by simulation. The method provides an efficient tool to make the full-energy efficiency calibration curve for scintillation detectors for any samples geometry and volume in order to determine accurate activity concentrations in terrestrial samples. - Highlights: Black-Right-Pointing-Pointer CsI (Tl) and NaI (Tl) detectors were studied for the measurement of terrestrial samples. Black-Right-Pointing-Pointer Monte Carlo method was used for efficiency calibration using natural gamma emitting terrestrial radionuclides. Black-Right-Pointing-Pointer The coincidence summing effect occurring for the 2614 keV emission of {sup 208}Tl is assessed by simulation.

  9. Comparison between EDXRF and FAAS for Zn determination in terrestrial molluscs

    Energy Technology Data Exchange (ETDEWEB)

    Melo, Julyanne T.B.; Cantinha, Rebeca S.; Santos, Mariana L.O.; Santos, Katarine M.B.; Franca, Elvis J., E-mail: julyanne.melo@ufpe.br, E-mail: rebecanuclear@gmail.com, E-mail: marianasantos_ufpe@hotmail.com, E-mail: katarine.mizan@gmail.com, E-mail: ejfranca@cnen.gov.br [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil); Melo, Ana M.M.A., E-mail: amdemelo@hotmail.com [Universidade Federal de Pernambuco (UFPE), Recife, PE (Brazil). Departamento de Biofisica e Radiobiologia

    2015-07-01

    Even with the most advanced analytical techniques, achieving the true values of a given analyte in a sample cannot be an easy task. Energy Dispersive X-Ray Fluorescence (EDXRF) and Flame Atomic Absorption Spectrometry (FAAS) have been widely used for analysis of the chemical composition of biological matrices in environmental studies. However, depending on the sample matrix, a combination of techniques could be needed for the correct determination of the analyte. Zinc distribution in Littoraria angulifera and Melampus coffea is quite dependent on the environment, so that, diverse methods could be necessary to evaluate the chemical composition of these mollusks. This study aimed at the comparison between EDXRF and FAAS techniques for determining Zn in the soft tissues of terrestrial mollusks. The animals were collected in three mangroves in the State of Pernambuco, Brazil. After shell removal, tissues were lyophilized and milled in a mortar. Test portions of 500 mg were analyzed by EDXRF, followed by chemical treatment for FAAS analysis. For the quality of the analytical procedure, the standard reference material SRM 2976 Mussel Tissue was analyzed together with the samples. The results for the analysis of the certified reference material SRM 2976 indicated the quality of the analytical procedure for both techniques. Adjusted-R{sup 2} between EDXRF and FAAS results was 0.95, indicating a good equivalence of Zn determination by both techniques. However, some improvement of EDXRF determination could be necessary because of the tendency of lower results compared to FAAS, probably related to spectral interferences during the analysis. (author)

  10. Determination of tritium in wine yeast samples

    International Nuclear Information System (INIS)

    Cotarlea, Monica-Ionela; Paunescu Niculina; Galeriu, D; Mocanu, N.; Margineanu, R.; Marin, G.

    1998-01-01

    Analytical procedures were developed to determine tritium in wine and wine yeast samples. The content of organic compounds affecting the LSC measurement is reduced by fractioning distillation for wine samples and azeotropic distillation/fractional distillation for wine yeast samples. Finally, the water samples were normally distilled with K MO 4 . The established procedures were successfully applied for wine and wine samples from Murfatlar harvests of the years 1995 and 1996. (authors)

  11. Tellurium stable isotope fractionation in chondritic meteorites and some terrestrial samples

    Science.gov (United States)

    Fehr, Manuela A.; Hammond, Samantha J.; Parkinson, Ian J.

    2018-02-01

    New methodologies employing a 125Te-128Te double-spike were developed and applied to obtain high precision mass-dependent tellurium stable isotope data for chondritic meteorites and some terrestrial samples by multiple-collector inductively coupled plasma mass spectrometry. Analyses of standard solutions produce Te stable isotope data with a long-term reproducibility (2SD) of 0.064‰ for δ130/125Te. Carbonaceous and enstatite chondrites display a range in δ130/125Te of 0.9‰ (0.2‰ amu-1) in their Te stable isotope signature, whereas ordinary chondrites present larger Te stable isotope fractionation, in particular for unequilibrated ordinary chondrites, with an overall variation of 6.3‰ for δ130/125Te (1.3‰ amu-1). Tellurium stable isotope variations in ordinary chondrites display no correlation with Te contents or metamorphic grade. The large Te stable isotope fractionation in ordinary chondrites is likely caused by evaporation and condensation processes during metamorphism in the meteorite parent bodies, as has been suggested for other moderately and highly volatile elements displaying similar isotope fractionation. Alternatively, they might represent a nebular signature or could have been produced during chondrule formation. Enstatite chondrites display slightly more negative δ130/125Te compared to carbonaceous chondrites and equilibrated ordinary chondrites. Small differences in the Te stable isotope composition are also present within carbonaceous chondrites and increase in the order CV-CO-CM-CI. These Te isotope variations within carbonaceous chondrites may be due to mixing of components that have distinct Te isotope signatures reflecting Te stable isotope fractionation in the early solar system or on the parent bodies and potentially small so-far unresolvable nucleosynthetic isotope anomalies of up to 0.27‰. The Te stable isotope data of carbonaceous and enstatite chondrites displays a general correlation with the oxidation state and hence might

  12. Isotopic studies of rare gases in terrestrial samples and natural nucleosynthesis

    International Nuclear Information System (INIS)

    1990-07-01

    This project is concerned with research in rare gas mass spectrometry. We read the natural record that isotopes of the rare gases provide. We study fluids using a system (RARGA) that is sometimes deployed in the field. In 1990 there was a strong effort to reduce the backlog of RARGA samples on hand, so that it was a year of intensive data gathering. Samples from five different areas in the western United States and samples from Guatemala and Australia were analyzed. In a collaborative study we also began analyzing noble gases from rocks associated with the fluids. An important objective, continuing in 1991, is to understand better the reasons for somewhat elevated 3 He/ 4 He ratios in regions where there is no contemporary volcanism which could produce the effect by addition of mantle helium. Our helium data have given us and our collaborators some insights, which are to be followed up, into gold mineralization in geothermal regions. Our DOE work in calibrating a sensitive laser microprobe mass spectrometer for noble gases in fluid inclusions continues. Having completed a series of papers on noble gases in diamonds, we next will attempt to make precise isotopic measurements on xenon from mantle sources, in search of evidence for terrestrially elusive 244 Pu decay

  13. Isotopic studies of rare gases in terrestrial samples and natural nucleosynthesis

    International Nuclear Information System (INIS)

    Reynolds, J.H.

    1991-01-01

    This project is concerned with research in rare gas mass spectrometry. We read the natural record that isotopes of the rate gases provide. We study fluids using a system (RARGA) that is sometimes deployed in the field. In 1990 there was a strong effort to reduce the backlog of RARGA samples on hand, so that it was a year of intensive data gathering. Samples from five different areas in the Western United States and samples from Guatemala and Australia were analyzed. In a collaborative study we also began analyzing noble gases from rocks associated with the fluids. An important objective, continuing in 1991, is to understand better the reasons for somewhat elevated 3 He/ 4 He ratios in regions where there is no contemporary volcanism which could produce the effect by addition of mantle helium. Our helium data have given us and our collaborators some insights, which are to be followed up, into gold mineralization in geothermal regions. Our DOE work in calibrating a sensitive laser microprobe mass spectrometer for noble gases in fluid inclusions continues. Having completed a series of papers on noble gases in diamonds, we next will attempt to make precise isotopic measurements on xenon from mantle sources in search of evidence for terrestrially elusive 244 Pu decay. 41 refs., 3 figs

  14. The roles of productivity and ecosystem size in determining food chain length in tropical terrestrial ecosystems.

    Science.gov (United States)

    Young, Hillary S; McCauley, Douglas J; Dunbar, Robert B; Hutson, Michael S; Ter-Kuile, Ana Miller; Dirzo, Rodolfo

    2013-03-01

    Many different drivers, including productivity, ecosystem size, and disturbance, have been considered to explain natural variation in the length of food chains. Much remains unknown about the role of these various drivers in determining food chain length, and particularly about the mechanisms by which they may operate in terrestrial ecosystems, which have quite different ecological constraints than aquatic environments, where most food chain length studies have been thus far conducted. In this study, we tested the relative importance of ecosystem size and productivity in influencing food chain length in a terrestrial setting. We determined that (1) there is no effect of ecosystem size or productive space on food chain length; (2) rather, food chain length increases strongly and linearly with productivity; and (3) the observed changes in food chain length are likely achieved through a combination of changes in predator size, predator behavior, and consumer diversity along gradients in productivity. These results lend new insight into the mechanisms by which productivity can drive changes in food chain length, point to potential for systematic differences in the drivers of food web structure between terrestrial and aquatic systems, and challenge us to consider how ecological context may control the drivers that shape food chain length.

  15. Study of phosphors determination in biological samples

    International Nuclear Information System (INIS)

    Oliveira, Rosangela Magda de.

    1994-01-01

    In this paper, phosphors determination by neutron activation analysis in milk and bone samples was studied employing both instrumental and radiochemical separation methods. The analysis with radiochemistry separation consisted of the simultaneous irradiation of the samples and standards during 30 minutes, dissolution of the samples, hold back carrier, addition precipitation of phosphorus with ammonium phosphomolibdate (A.M.P.) and phosphorus-32 by counting by using Geiger-Mueller detector. The instrumental analysis consisted of the simultaneous irradiation of the samples and standards during 30 minutes, transfer of the samples into a counting planchet and measurement of the beta radiation emitted by phosphorus-32, after a suitable decay period. After the phosphorus analysis methods were established they were applied to both commercial milk and animal bone samples, and data obtained in the instrumental and radiochemical separation methods for each sample, were compared between themselves. In this work, it became possible to obtain analysis methods for phosphorus that can be applied independently of the sample quantity available, and the phosphorus content in the samples or interference that can be present in them. (author). 51 refs., 7 figs., 4 tabs

  16. In vitro cytotoxic activity of five commercial samples of Tribulus terrestris Linn in Espírito Santo (Brazil

    Directory of Open Access Journals (Sweden)

    Claudio Costa Oliveira Filho

    2018-04-01

    Full Text Available ABSTRACT The objective was to investigate the total saponin and protodioscin concentrations and the cytotoxicity in vitro, of five samples of the plant Tribulus terrestris, commercially available in the metropolitan region of Vitória - Espirito Santo, Brazil, and to compare them with the aqueous extract of the plant. The chromatographic profile and quantification of protodioscin in commercial samples and plant extract were evaluated by LC-MS/MS. The percentage of total saponins were determined by the colorimetric method. Extracts and protodioscin cytotoxicity were analyzed by the MTT assay in three cell lineages: fibroblasts (L929, ovarian cancer (Ovcar3 and murine hepatoma (Hepa1c1c7. All extracts displayed high levels of total saponins (207.2 to 780.3 mg g-1 of dry extract. The chromatographic profile revealed a wide diversity of compounds, and the saponin protodioscin was detected in only two extracts. One extract displayed high cytotoxicity, with IC50 values of 157.0, 38.2 and 7.4 µg mL-1 for the Ovcar3, Hepa1c1c7 and L929 cell lines, respectively. The other extracts displayed cytotoxic effects only at concentrations equal to or greater than 125.0 µg mL-1. Surprisingly, the most cytotoxic extract displayed the highest protodioscin concentration. Therefore, it is suggested that these products be marketed with caution, and followed-up by a certified healthcare professional.

  17. Rapid determination of actinides in seawater samples

    International Nuclear Information System (INIS)

    Maxwell, S.L.; Culligan, B.K.; Hutchison, J.B.; Utsey, R.C.; McAlister, D.R.

    2014-01-01

    A new rapid method for the determination of actinides in seawater samples has been developed at the Savannah River National Laboratory. The actinides can be measured by alpha spectrometry or inductively-coupled plasma mass spectrometry. The new method employs novel pre-concentration steps to collect the actinide isotopes quickly from 80 L or more of seawater. Actinides are co-precipitated using an iron hydroxide co-precipitation step enhanced with Ti +3 reductant, followed by lanthanum fluoride co-precipitation. Stacked TEVA Resin and TRU Resin cartridges are used to rapidly separate Pu, U, and Np isotopes from seawater samples. TEVA Resin and DGA Resin were used to separate and measure Pu, Am and Cm isotopes in seawater volumes up to 80 L. This robust method is ideal for emergency seawater samples following a radiological incident. It can also be used, however, for the routine analysis of seawater samples for oceanographic studies to enhance efficiency and productivity. In contrast, many current methods to determine actinides in seawater can take 1-2 weeks and provide chemical yields of ∼30-60 %. This new sample preparation method can be performed in 4-8 h with tracer yields of ∼85-95 %. By employing a rapid, robust sample preparation method with high chemical yields, less seawater is needed to achieve lower or comparable detection limits for actinide isotopes with less time and effort. (author)

  18. 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.

  19. Determination of radium-226 in environmental samples

    International Nuclear Information System (INIS)

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

    1980-01-01

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

  20. 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)

  1. Methods and considerations to determine sphere center from terrestrial laser scanner point cloud data

    International Nuclear Information System (INIS)

    Rachakonda, Prem; Muralikrishnan, Bala; Lee, Vincent; Shilling, Meghan; Sawyer, Daniel; Cournoyer, Luc; Cheok, Geraldine

    2017-01-01

    The Dimensional Metrology Group at the National Institute of Standards and Technology is performing research to support the development of documentary standards within the ASTM E57 committee. This committee is addressing the point-to-point performance evaluation of a subclass of 3D imaging systems called terrestrial laser scanners (TLSs), which are laser-based and use a spherical coordinate system. This paper discusses the usage of sphere targets for this effort, and methods to minimize the errors due to the determination of their centers. The key contributions of this paper include methods to segment sphere data from a TLS point cloud, and the study of some of the factors that influence the determination of sphere centers. (paper)

  2. Determination of radioactivity in meat samples

    International Nuclear Information System (INIS)

    Malik, G.M.; Atta, M.A.; Shafiq, M.; Zafar, M.S.

    1993-01-01

    The presence of radionuclides in edibles can create harmful effects in the human body. It is, therefore, essential that the radioactivity must be searched in the food stuff specially in those items which are available near the nuclear installations. The radioactivity in the meat samples obtained from the surroundings of PINSTECH (Pakistan Institute of Nuclear Science and Technology), PINSTECH Complex has been determined using high resolution Ge(Li) gamma ray spectrometer and a low level beta counting system. The results show that the measured values of the radioactivity are below the maximum permissible levels. (author)

  3. Determination of uranium in liquid samples

    International Nuclear Information System (INIS)

    Macefat, Martina R.; Grahek, Zeljko; Ivsic, Astrid G.

    2008-01-01

    Full text: Uranium is a natural occurring radionuclide and the first member of natural radioactive chains which makes its determination in natural materials interesting from geochemical and radioecological aspect. It can be quantitatively determined as element and/or its radioisotopes by different spectrometric methods (ICP-MS, spectrophotometry, alpha spectrometry). It is necessary to develop inexpensive, rapid and sensitive methods for the routine analysis. Therefore, in this paper, development of a new method for the isolation of uranium from liquid samples and subsequent determination by spectrophotometry and ICP-MS will be described. It is possible to isolate uranium from drinking and seawater using extraction chromatography or mixed solvent ion exchange. Uranium can be strongly bound on the TRU extraction chromatographic resin from nitric acid (chemical recovery is 100%) and can be separated from other interfering elements, while separation from thorium, which can be also strongly bound on this resin, is possible with hydrochloric acid. It is also possible to separate uranium from thorium on the anion exchanger Amberlite CG-400 (NO 3 - form) because uranium is much more weakly bound on this exchanger from alcoholic solutions of nitric acid. After the separation uranium is determined by ICP-MS and by spectrophotometric method with arsenazo III (λ max =652 nm). Developed method enables selection of the optimal mode of isolation for the given purposes. (author)

  4. Microstructure and Macrosegregation Study of Directionally Solidified Al-7Si Samples Processed Terrestrially and Aboard the International Space Station

    Science.gov (United States)

    Angart, Samuel; Erdman, R. G.; Poirier, David R.; Tewari, S.N.; Grugel, R. N.

    2014-01-01

    This talk reports research that has been carried out under the aegis of NASA as part of a collaboration between ESA and NASA for solidification experiments on the International Space Station (ISS). The focus has been on the effect of convection on the microstructural evolution and macrosegregation in hypoeutectic Al-Si alloys during directional solidification (DS). The DS-experiments have been carried out under 1-g at Cleveland State University (CSU) and under low-g on the International Space Station (ISS). The thermal processing-history of the experiments is well defined for both the terrestrially-processed samples and the ISS-processed samples. We have observed that the primary dendrite arm spacings of two samples grown in the low-g environment of the ISS show good agreement with a dendrite-growth model based on diffusion controlled growth. The gravity-driven convection (i.e., thermosolutal convection) in terrestrially grown samples has the effect of decreasing the primary dendrite arm spacings and causes macrosgregation. In order to process DS-samples aboard the ISS, dendritic-seed crystals have to partially remelted in a stationary thermal gradient before the DS is carried out. Microstructural changes and macrosegregation effects during this period are described.

  5. Isotopic studies of rare gases in terrestrial samples and in natural nucleosynthesis

    International Nuclear Information System (INIS)

    Reynolds, J.H.

    1988-08-01

    This project is concerned with research in rare gas mass spectrometry. The broad objective is to read the natural record that isotopes of the rare gases comprise as trace constituents of natural gases, rocks, and meteorites. In past years, these interests have led to the study of such diverse problems as the dating of rocks, the early chronology and isotopic structure of the solar system as revealed by extinct radioactivities, and the elemental and isotopic composition of trapped primordial rare gases in meteorites. In recent years, the project has focused progressively more on terrestrial problems

  6. Isotopic studies of rare gases in terrestrial samples and in natural nucleosynthesis

    International Nuclear Information System (INIS)

    1987-07-01

    This project is concerned with research in rare gas mass spectrometry. The broad objective is to read the natural record that isotopes of the rare gases comprise as trace constituents of natural gases, rocks, and meteorites. In past years, these interests have led to the study of such diverse problems as the dating of rocks, the early chronology and isotopic structure of the solar system as revealed by extinct radioactivities, and the elemental and isotopic composition of trapped primordial rare gases in meteorites. In recent years, the project has focused progressively more on terrestrial problems

  7. Determination of I-131 in milk samples

    International Nuclear Information System (INIS)

    Fernandez G, I.; Rodriguez C, G.; Quevedo A, J. L.

    1996-01-01

    In our country, in the near future, an isotope center will be in operation, and due to its characteristics, it is possible the discharge of radionuclides to the atmosphere during its normal exploitation, as well as in case of accident. Considering the kind and the concentration of the radioactive material released to the atmosphere, the possible ways of contamination were determined, playing the milk the most significant role, because the Iodine-131 is in the radionuclide inventory of this center, being possible to pass to the food-chain soil-grass-milk, due to the fact that the center is located in a cattle zone. Owing to these facts, it is necessary to rely on a method for determining Iodine-131 that allows to control its presence in milk samples, when the isotope center start to operate. The direct absorption of Iodine-131 in an anionic exchange resin and the subsequent analysis of this resin for gamma spectrometry with a Nal (Tl) detector is a cheap, simple and fast method with a recovery average greater than the 95%. (authors). 5 refs., 3 tabs

  8. Improved sample size determination for attributes and variables sampling

    International Nuclear Information System (INIS)

    Stirpe, D.; Picard, R.R.

    1985-01-01

    Earlier INMM papers have addressed the attributes/variables problem and, under conservative/limiting approximations, have reported analytical solutions for the attributes and variables sample sizes. Through computer simulation of this problem, we have calculated attributes and variables sample sizes as a function of falsification, measurement uncertainties, and required detection probability without using approximations. Using realistic assumptions for uncertainty parameters of measurement, the simulation results support the conclusions: (1) previously used conservative approximations can be expensive because they lead to larger sample sizes than needed; and (2) the optimal verification strategy, as well as the falsification strategy, are highly dependent on the underlying uncertainty parameters of the measurement instruments. 1 ref., 3 figs

  9. Determining Characteristic Vegetation Areas by Terrestrial Laser Scanning for Floodplain Flow Modeling

    Directory of Open Access Journals (Sweden)

    Johanna Jalonen

    2015-01-01

    Full Text Available Detailed modeling of floodplain flows and associated processes requires data on mixed, heterogeneous vegetation at river reach scale, though the collection of vegetation data is typically limited in resolution or lack spatial information. This study investigates physically-based characterization of mixed floodplain vegetation by means of terrestrial laser scanning (TLS. The work aimed at developing an approach for deriving the characteristic reference areas of herbaceous and foliated woody vegetation, and estimating the vertical distribution of woody vegetation. Detailed experimental data on vegetation properties were gathered both in a floodplain site for herbaceous vegetation, and under laboratory conditions for 2–3 m tall trees. The total plant area (Atot of woody vegetation correlated linearly with the TLS-based voxel count, whereas the Atot of herbaceous vegetation showed a linear correlation with TLS-based vegetation mean height. For woody vegetation, 1 cm voxel size was found suitable for estimating both the Atot and its vertical distribution. A new concept was proposed for deriving Atot for larger areas from the point cloud attributes of small sub-areas. The results indicated that the relationships between the TLS attributes and Atot of the sub-areas can be derived either by mm resolution TLS or by manual vegetation sampling.

  10. Autogenic geomorphic processes determine the resolution and fidelity of terrestrial paleoclimate records

    OpenAIRE

    Foreman, Brady Z.; Straub, Kyle M.

    2017-01-01

    Terrestrial paleoclimate records rely on proxies hosted in alluvial strata whose beds are deposited by unsteady and nonlinear geomorphic processes. It is broadly assumed that this renders the resultant time series of terrestrial paleoclimatic variability noisy and incomplete. We evaluate this assumption using a model of oscillating climate and the precise topographic evolution of an experimental alluvial system. We find that geomorphic stochasticity can create aliasing in the time series and ...

  11. Determination of Phthalates in Drinking Water Samples

    African Journals Online (AJOL)

    user

    successfully applied to the analysis of phthalate esters contamination in bottled drinking water samples. ... esters are used in the manufacturing of polyvinyl chloride. (PVC). ... water, soil, air, food products and the human body. (Castillo et al.

  12. Gravimetric determination of uranium in SALE samples

    International Nuclear Information System (INIS)

    Anon.

    1981-01-01

    As a participant in the Safeguards Analytical Laboratory Evaluation (SALE) program, the Analytical Chemistry Laboratory at General Atomic routinely assays uranium dioxide and uranyl nitrate SALE samples for uranium content. Gravimetric methods are relatively easy and inexpensive to apply when the samples for uranium content. Gravimetric methods are relatively easy and inexpensive to apply when the samples are free from substantial amounts of metallic impurities. Clearly the gravimetric procedure alone is not specific for uranium and must be enhanced by the use of impurity corrections. Emission spectrography is used routinely as the technique of choice for making such corrections. In cases where it is essential to assay specifically for uranium, the modified Davies-Gray titration using a weighed titrant method is applied. In this paper some essential features of these gravimetric and titrimetric procedures are discussed

  13. The determination of uranium in pyrite samples

    International Nuclear Information System (INIS)

    Jacobs, J.J.

    1979-01-01

    An existing method for the determination of uranium in rocks and minerals is examined for the determination of uranium in materials containing pyrite. The results are comparable with those obtained by a spectrophotometric method, the precision (relative standard deviation) of the method for standards with U 3 O 8 contents of 1500 and 300 p.p.m. being 0,03 and 0,08 respectively when prepared in pyrite, and 0,15 and 0,06 respectively when made up with inert diluent. Full details of the procedure are given in accompanying appendices [af

  14. Energy and speleogenesis: Key determinants of terrestrial species richness in caves.

    Science.gov (United States)

    Jiménez-Valverde, Alberto; Sendra, Alberto; Garay, Policarp; Reboleira, Ana Sofia P S

    2017-12-01

    The aim of this study was to unravel the relative role played by speleogenesis (i.e., the process in which a cave is formed), landscape-scale variables, and geophysical factors in the determination of species richness in caves. Biological inventories from 21 caves located in the southeastern Iberian Peninsula along with partial least square (PLS) regression analysis were used to assess the relative importance of the different explanatory variables. The caves were grouped according to the similarity in their species composition; the effect that spatial distance could have on similarity was also studied using correlation between matrices. The energy and speleogenesis of caves accounted for 44.3% of the variation in species richness. The trophic level of each cave was the most significant factor in PLS regression analysis, and epigenic caves (i.e., those formed by the action of percolating water) had significantly more species than hypogenic ones (i.e., those formed by the action of upward flows in confined aquifers). Dissimilarity among the caves was very high (multiple-site β sim  = 0.92). Two main groups of caves were revealed through the cluster analysis, one formed by the western caves and the other by the eastern ones. The significant-but low-correlation found between faunistic dissimilarity and geographical distance ( r  =   .16) disappeared once the caves were split into the two groups. The extreme beta-diversity suggests a very low connection among the caves and/or a very low dispersal capacity of the species. In the region under study, two main factors are intimately related to the richness of terrestrial subterranean species in caves: the amount of organic material (trophic level) and the formation process (genesis). This is the first time that the history of a cave genesis has been quantitatively considered to assess its importance in explaining richness patterns in comparison with other factors more widely recognized.

  15. Spectrophotometric determination of chromium in geological samples

    International Nuclear Information System (INIS)

    Rathore, D.P.S.; Tarafder, P.K.

    1992-01-01

    A method for the determination of chromium is presented, based on the oxidation of hydroxylamine hydrochloride to nitrous acid by chromium(VI) in acetic acid medium followed by diazotization of the nitrite produced with p-aminophenylmercaptoacetic acid and subsequent coupling of the diazonium salt with N-(1-naphthyl)ethylenediamine di-hydrochloride in acidic medium to form a stable blueish azo dye. The method is suitable for the determination of chromium(VI) from 0.04 to 1.2 mg l -1 in a 1.0-cm cuvette. The molar absorptivity and Sandell's sensitivity are 3.65x10 4 l mol -1 cm -1 and 0.0014μg cm -2 , respectively. (author). 17 refs.; 3 figs

  16. Accelerated tests for the soft error rate determination of single radiation particles in components of terrestrial and avionic electronic systems

    International Nuclear Information System (INIS)

    Flament, O.; Baggio, J.

    2010-01-01

    This paper describes the main features of the accelerated test procedures used to determine reliability data of microelectronics devices used in terrestrial environment.This paper focuses on the high energy particle test that could be performed through spallation neutron source or quasi-mono-energetic neutron or proton. Improvements of standards are illustrated with respect to the state of the art of knowledge in radiation effects and scaling down of microelectronics technologies. (authors)

  17. Determination of 40K in water samples

    International Nuclear Information System (INIS)

    Delgado, C. E.; Miranda C, L.; Cuevas J, A. K.; Vega C, H. R.

    2014-10-01

    The natural water used for human consumption comes from different sources, which may contain suspended solids in varying proportions. In groundwater, the source of suspended solids is related to the dissolution of mineral strata by the waters and leaching of rocks. Also, the radioactivity could concentrate on the bodies of slow-moving water that eventually could present a risk to ecosystems, as well as for the consumer. The water usually contains several natural radionuclides as: tritium, radon, radio, uranium isotopes, etc. The objective of this study was to evaluate the concentration of 40 K in water from different areas of Zacatecas state (Mexico). Four water samples were taken in triplicate from different areas; the 40 K concentration was measured with a spectrum metric system of gamma radiation with NaI (Tl) scintillation detector of 7.62 cm. In the measuring process a standard was prepared using water and KCl analytic grade where the 40 K concentration is 6.25 mol/Lt adding 250 mg/ml of potassium. Also the system was calibrated in energy using 3 point sources of 137 Cs, diameter 22 Na and 7.62 cm of height, using containers Marinelli and 60 Co. In the obtained spectra was observed that the photon of 1.432 MeV that emits the 40 K when decaying is the most important. The highest concentration was of 123 ± 5.2 Bq/lt and the lowest was of 9 ± 0.4 Bq/lt. Under the standards of drinking water, an amount of 40 K deposits an effective dose which contributes to annual dose received by people. (Author)

  18. Determination of volatile trace elements in terrestrial minerals and lunar soils by RNAA

    International Nuclear Information System (INIS)

    Kraehenbuehl, U.; Wegmueller, F.

    1978-01-01

    A procedure is reported for the simultaneous determination of Au, Cd, Ge, Hg, In, Sb, Te and Zn in 5-50 mg aliquots of minerals and lunar soils. After irradiation with thermal neutrons the samples are dissolved in digestion bombs by HF/HClO 4 . Sulfide precipitates provide the necessary group separations. The purified elements are measured on Ge(Li) detectors. Accuracy and precision are generally better than 10%. (author)

  19. Isotopic studies of rare gases in terrestrial samples and natural nucleosynthesis

    International Nuclear Information System (INIS)

    1991-05-01

    This project is concerned with research in rare gas mass spectrometry. Using a two-pronged attack, we study fluids using a system (RARGA) designed for fluid analysis in bulk which is sometimes deployed in the field and a laser microprobe mass spectrometer for fluid inclusion studies. In 1991 the RARGA project continued monitoring helium isotope variations associated with renewed seismic activity in Long Valley Caldera and expanded our geothermal data base to include Lassen National Park. An important objective, continuing in 1992, is to understand better the reasons for somewhat elevated 3 He/ 4 He ratios in regions where there is no contemporary volcanism which could produce the effect by addition of mantle helium. To this end, 1991 saw continued efforts to understand variations in composition between fluids and associated reservoir rocks and extended the data base to include fluids from the Gulf of Mexico. Our DOE work in calibrating a sensitive laser microprobe mass spectrometer for noble gases in fluid inclusions continues with successful returns particularly in calibrating neutron irradiated samples for tracing halogen ratios. In connection with observations of neutron-produced noble gas nuclides in granites, we have begun comparing measurements with calculations for both thermal and epithermal neutrons. We submitted a third paper on noble gases in diamonds, concentrating on observed effects of 4 He, 3 He, and fission xenon implantation from nuclear processes in adjacent material in the matrix rock. 16 refs., 1 tab

  20. Autogenic geomorphic processes determine the resolution and fidelity of terrestrial paleoclimate records.

    Science.gov (United States)

    Foreman, Brady Z; Straub, Kyle M

    2017-09-01

    Terrestrial paleoclimate records rely on proxies hosted in alluvial strata whose beds are deposited by unsteady and nonlinear geomorphic processes. It is broadly assumed that this renders the resultant time series of terrestrial paleoclimatic variability noisy and incomplete. We evaluate this assumption using a model of oscillating climate and the precise topographic evolution of an experimental alluvial system. We find that geomorphic stochasticity can create aliasing in the time series and spurious climate signals, but these issues are eliminated when the period of climate oscillation is longer than a key time scale of internal dynamics in the geomorphic system. This emergent autogenic geomorphic behavior imparts regularity to deposition and represents a natural discretization interval of the continuous climate signal. We propose that this time scale in nature could be in excess of 10 4 years but would still allow assessments of the rates of climate change at resolutions finer than the existing age model techniques in isolation.

  1. Parameters of electromagnetic weather in near-terrestrial space determining the effects on biosystems

    International Nuclear Information System (INIS)

    Oraevskij, V.N.; Golyshev, S.A.; Levitin, A.E.; Breus, T.K.; Ivanova, S.V.; Komarov, F.I.; Rapoport, S.I.

    1995-01-01

    Space and time distribution of the electric and magnetic fields and current systems in the near terrestrial space (electromagnetic weather) were studied in connection with ambulance calls in Moscow, Russia, related to the cardia-vascular diseases. The some examples of the correlations between the solar activity parameters and geomagnetic variations and the events of the extreme number of ambulance calls were presented. 4 refs., 5 figs., 2 tabs

  2. Mapping Vineyard Leaf Area Using Mobile Terrestrial Laser Scanners: Should Rows be Scanned On-the-Go or Discontinuously Sampled?

    Directory of Open Access Journals (Sweden)

    Ignacio del-Moral-Martínez

    2016-01-01

    Full Text Available The leaf area index (LAI is defined as the one-side leaf area per unit ground area, and is probably the most widely used index to characterize grapevine vigor. However, LAI varies spatially within vineyard plots. Mapping and quantifying this variability is very important for improving management decisions and agricultural practices. In this study, a mobile terrestrial laser scanner (MTLS was used to map the LAI of a vineyard, and then to examine how different scanning methods (on-the-go or discontinuous systematic sampling may affect the reliability of the resulting raster maps. The use of the MTLS allows calculating the enveloping vegetative area of the canopy, which is the sum of the leaf wall areas for both sides of the row (excluding gaps and the projected upper area. Obtaining the enveloping areas requires scanning from both sides one meter length section along the row at each systematic sampling point. By converting the enveloping areas into LAI values, a raster map of the latter can be obtained by spatial interpolation (kriging. However, the user can opt for scanning on-the-go in a continuous way and compute 1-m LAI values along the rows, or instead, perform the scanning at discontinuous systematic sampling within the plot. An analysis of correlation between maps indicated that MTLS can be used discontinuously in specific sampling sections separated by up to 15 m along the rows. This capability significantly reduces the amount of data to be acquired at field level, the data storage capacity and the processing power of computers.

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

    International Nuclear Information System (INIS)

    2010-01-01

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

  4. 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.

  5. The Use of Terrestrial Analogs in Preparing for Planetary Surface Exploration: Sampling and Radioisotopic Dating of Impactites and Deployment of In Situ Analytical Technologies

    Science.gov (United States)

    Young, Kelsey

    Impact cratering has played a crucial role in the surface development of the inner planets. Constraining the timing of this bombardment history is important in understanding the origins of life and our planet's evolution. Plate tectonics, active volcanism, and vegetation hinder the preservation and identification of existing impact craters on Earth. Providing age constraints on these elusive structures will provide a deeper understanding of our planet's development. To do this, (U-Th)/He thermochronology and in situ 40 Ar/39Ar laser microprobe geochronology are used to provide ages for the Haughton and Mistastin Lake impact structures, both located in northern Canada. While terrestrial impact structures provide accessible laboratories for deciphering Earth's impact history, the ultimate goal for understanding the history of the reachable inner Solar System is to acquire robust, quantitative age constraints for the large lunar impact basins. The oldest of these is the South Pole-Aitken basin (SPA), located on the lunar farside. While it is known that this basin is stratigraphically the oldest on the Moon, its absolute age has yet to be determined. Several reports released in the last decade have highlighted sampling and dating SPA as a top priority for inner Solar System exploration. This is no easy task as the SPA structure has been modified by four billion subsequent years of impact events. Informed by studies at Mistastin---which has target lithologies analogous to those at SPA---sampling strategies are discussed that are designed to optimize the probability of a high science return with regard to robust geochronology of the SPA basin. Planetary surface missions, like one designed to explore and sample SPA, require the integration of engineering constraints with scientific goals and traverse planning. The inclusion of in situ geochemical technology, such as the handheld X-ray fluorescence spectrometer (hXRF), into these missions will provide human crews with the

  6. A laboratory evaluation to determine the compatibility of microbiological control agents with the pollinator Bombus terrestris.

    Science.gov (United States)

    Mommaerts, Veerle; Sterk, Guido; Hoffmann, Lucien; Smagghe, Guy

    2009-09-01

    This study was undertaken to identify any potential adverse side effects of the use of seven microbiological control agents (MCAs) on the bumblebee, Bombus terrestris L., in the context of combined use in integrated pest management (IPM). AQ10 (Ampelomyces quisqualis), Binab-T-vector (Hypocrea parapilulifera + T. atroviride; 1/1), Prestop-Mix (Gliocladium catenulatum J1446), Serenade (Bacillus subtilis QST713), Trianum-P (Trichoderma harzianum T22), Botanigard (Beauveria bassiana GHA) and Granupom (Cydia pomonella granulovirus), comprising five biofungicides and two bioinsecticides, were investigated. Bumblebee workers were exposed under laboratory conditions to each MCA at its maximum field recommended concentration (MFRC) via three different routes of exposure: dermal contact and orally via either treated sugar water or pollen. The tested MCAs were found to be safe for workers of B. terrestris, with the exception of Botanigard and Serenade. Exposure to Botanigard via contact at its MFRC caused 92% mortality after 11 weeks, while the 1/10 MFRC killed 46% of exposed workers. For Serenade, topical contact and oral delivery via sugar water resulted in 88 and 100% worker mortality respectively. With lower concentrations (1/2, 1/5 and 1/10 MFRC) the toxicity decreased, but the effect depended on the route of exposure. In addition to lethal effects, nests were also evaluated for sublethal effects after treatment with the seven MCAs at their respective MFRCs over 11 weeks. In these bioassays, only Botanigard and Serenade gave rise to a significant (P drone production. Sublethal effects on foraging behaviour were also evaluated, and only Botanigard at its MFRC delivered via treated sugar water induced negative effects. The results demonstrated that most of the MCAs tested can be considered safe for use in combination with B. terrestris, based on the International Organisation for Biological Control of Noxious Animals and Plants (IOBC) classification. However, some can be

  7. Determination of the isotopic (C-13/C-12) discrimination by terrestrial biology from a global network of observations

    International Nuclear Information System (INIS)

    Bakwin, P.S.; Tans, P.P.; White, J.W.C.; Andres, R.J.

    1998-01-01

    Data from the National Oceanic and Atmospheric Administration/Climate Monitoring and Diagnostics Laboratory global air sampling network are analysed in order to extract the signatures of isotopic (C-13/C-12) discrimination by the terrestrial iota and of fossil fuel combustion for the regions surrounding the sampling sites. Measurements of carbon monoxide (CO) are used to give an estimate of the contribution of fossil fuel combustion to the short-term variability of carbon dioxide. In general, variations of CO 2 are more strongly dominated by biological exchange, so the isotopic signature of fossil fuel combustion, while consistent with inventory estimates, is not well constrained by the observations. Conversely, results for isotope discrimination by the terrestrial biosphere are not strongly dependent on assumptions about fossil fuel combustion. The analysis appears valid primarily for stations fairly near continental source/sink regions, particularly for midlatitude regions of the northern hemisphere. For these stations a mean discrimination of -16.8 per mil (%) is derived, with site-to-site variability of 0.8% and with little or no consistent latitudinal gradient

  8. STATISTICALLY DETERMINED DISPERSION RELATIONS OF MAGNETIC FIELD FLUCTUATIONS IN THE TERRESTRIAL FORESHOCK

    International Nuclear Information System (INIS)

    Hnat, B.; O’Connell, D.; Nakariakov, V. M.; Sundberg, T.

    2016-01-01

    We obtain dispersion relations of magnetic field fluctuations for two crossings of the terrestrial foreshock by Cluster spacecraft. These crossings cover plasma conditions that differ significantly in their plasma β and in the density of the reflected ion beam, but not in the properties of the encountered ion population, both showing shell-like distribution function. Dispersion relations are reconstructed using two-point instantaneous wave number estimations from pairs of Cluster spacecraft. The accessible range of wave vectors, limited by the available spacecraft separations, extends to ≈2 × 10 4 km. Results show multiple branches of dispersion relations, associated with different powers of magnetic field fluctuations. We find that sunward propagating fast magnetosonic waves and beam resonant modes are dominant for the high plasma β interval with a dense beam, while the dispersions of the interval with low beam density include Alfvén and fast magnetosonic modes propagating sunward and anti-sunward.

  9. STATISTICALLY DETERMINED DISPERSION RELATIONS OF MAGNETIC FIELD FLUCTUATIONS IN THE TERRESTRIAL FORESHOCK

    Energy Technology Data Exchange (ETDEWEB)

    Hnat, B.; O’Connell, D.; Nakariakov, V. M. [Centre for Fusion, Space and Astrophysics, University of Warwick (United Kingdom); Sundberg, T., E-mail: B.Hnat@warwick.ac.uk [School of Physics and Astronomy, Queen Mary University of London (United Kingdom)

    2016-08-20

    We obtain dispersion relations of magnetic field fluctuations for two crossings of the terrestrial foreshock by Cluster spacecraft. These crossings cover plasma conditions that differ significantly in their plasma β and in the density of the reflected ion beam, but not in the properties of the encountered ion population, both showing shell-like distribution function. Dispersion relations are reconstructed using two-point instantaneous wave number estimations from pairs of Cluster spacecraft. The accessible range of wave vectors, limited by the available spacecraft separations, extends to ≈2 × 10{sup 4} km. Results show multiple branches of dispersion relations, associated with different powers of magnetic field fluctuations. We find that sunward propagating fast magnetosonic waves and beam resonant modes are dominant for the high plasma β interval with a dense beam, while the dispersions of the interval with low beam density include Alfvén and fast magnetosonic modes propagating sunward and anti-sunward.

  10. Determination of plutonium in air and smear samples

    International Nuclear Information System (INIS)

    Hinton, E.R. Jr.; Tucker, W.O.

    1981-01-01

    A method has been developed for the determination of plutonium in air samples and smear samples that were collected on filter papers. The sample papers are digested in nitric acid, extracted into 2-thenoyltrifluoroacetone (TTA)-xylene, and evaporated onto stainless steel disks. Alpha spectrometry is employed to determine the activity of each plutonium isotope. Each sample is spiked with plutonium-236. All glassware used in the procedure is disposable. The detection limits are 3 and 5 dpm (disintegrations per minute) for air and smear samples, respectively, with an average recovery of 87%

  11. Simultaneous determination of plutonium and uranium in environmental samples

    International Nuclear Information System (INIS)

    Jiao Shufen

    1993-01-01

    Plutonium and uranium in a plant sample ash was simultaneously determined by using anion exchange resin columns, and concentrated hydrochloric acid and nitric acid. At the final stage of the determination of the nuclides, each of them was electrodeposited together with a little amount of molybdenum carrier onto a stainless steel plate and measured by α-ray spectrometer. The recoveries of uranium and plutonium from the plant samples determined by adding internal standard 236 Pu which was 100% and 63%, respectively

  12. Sample Size Determination for One- and Two-Sample Trimmed Mean Tests

    Science.gov (United States)

    Luh, Wei-Ming; Olejnik, Stephen; Guo, Jiin-Huarng

    2008-01-01

    Formulas to determine the necessary sample sizes for parametric tests of group comparisons are available from several sources and appropriate when population distributions are normal. However, in the context of nonnormal population distributions, researchers recommend Yuen's trimmed mean test, but formulas to determine sample sizes have not been…

  13. AAS determination of total mercury content in environmental samples

    International Nuclear Information System (INIS)

    Moskalova, M.; Zemberyova, M.

    1997-01-01

    Two methods for determination of total mercury content in environmental samples soils, and sediments, were compared. Dissolution procedure of soils, sediments, and biological material under elevated pressure followed by determination of mercury by cold vapour atomic absorption spectrometry using a MHS-1 system and direct total mercury determination without any chemical pretreatment from soil samples using a Trace Mercury Analyzer TMA-254 were compared. TMA-254 was also applied for the determination of mercury in various further standard reference materials. Good agreement with certified values of environmental reference materials was obtained. (authors)

  14. Spectrophotometric Determination of Boron in Environmental Water Samples

    International Nuclear Information System (INIS)

    San San; Khin Win Kyi; Kwaw Naing

    2002-02-01

    The present paper deals with the study on the methods for the determination of boron in the environmental water samples. The standard methods which are useful for this determination are discussed thoroughly in this work. Among the standard methods approved by American Public Health Association, the carmine method was selected for this study. Prior to the determination of boron in the water samples, the precision and accuracy of the methods of choice were examined by using standard boron solutions. The determination of Boron was carried out by using water samples, waste water from Aquaculture Research Centre, University of Yangon, the Ayeyarwady River water near Magway Myathalon Pagoda in Magway Division, ground water from Sanchaung Township, and tap water from Universities' Research Centre, University of Yangon. Analyses of these water samples were done and statistical treatment of the results was carried out. (author)

  15. Sample size determination in clinical trials with multiple endpoints

    CERN Document Server

    Sozu, Takashi; Hamasaki, Toshimitsu; Evans, Scott R

    2015-01-01

    This book integrates recent methodological developments for calculating the sample size and power in trials with more than one endpoint considered as multiple primary or co-primary, offering an important reference work for statisticians working in this area. The determination of sample size and the evaluation of power are fundamental and critical elements in the design of clinical trials. If the sample size is too small, important effects may go unnoticed; if the sample size is too large, it represents a waste of resources and unethically puts more participants at risk than necessary. Recently many clinical trials have been designed with more than one endpoint considered as multiple primary or co-primary, creating a need for new approaches to the design and analysis of these clinical trials. The book focuses on the evaluation of power and sample size determination when comparing the effects of two interventions in superiority clinical trials with multiple endpoints. Methods for sample size calculation in clin...

  16. Neuromuscular dose-response studies: determining sample size.

    Science.gov (United States)

    Kopman, A F; Lien, C A; Naguib, M

    2011-02-01

    Investigators planning dose-response studies of neuromuscular blockers have rarely used a priori power analysis to determine the minimal sample size their protocols require. Institutional Review Boards and peer-reviewed journals now generally ask for this information. This study outlines a proposed method for meeting these requirements. The slopes of the dose-response relationships of eight neuromuscular blocking agents were determined using regression analysis. These values were substituted for γ in the Hill equation. When this is done, the coefficient of variation (COV) around the mean value of the ED₅₀ for each drug is easily calculated. Using these values, we performed an a priori one-sample two-tailed t-test of the means to determine the required sample size when the allowable error in the ED₅₀ was varied from ±10-20%. The COV averaged 22% (range 15-27%). We used a COV value of 25% in determining the sample size. If the allowable error in finding the mean ED₅₀ is ±15%, a sample size of 24 is needed to achieve a power of 80%. Increasing 'accuracy' beyond this point requires increasing greater sample sizes (e.g. an 'n' of 37 for a ±12% error). On the basis of the results of this retrospective analysis, a total sample size of not less than 24 subjects should be adequate for determining a neuromuscular blocking drug's clinical potency with a reasonable degree of assurance.

  17. A terrestrial lidar-based workflow for determining three-dimensional slip vectors and associated uncertainties

    Science.gov (United States)

    Gold, Peter O.; Cowgill, Eric; Kreylos, Oliver; Gold, Ryan D.

    2012-01-01

    Three-dimensional (3D) slip vectors recorded by displaced landforms are difficult to constrain across complex fault zones, and the uncertainties associated with such measurements become increasingly challenging to assess as landforms degrade over time. We approach this problem from a remote sensing perspective by using terrestrial laser scanning (TLS) and 3D structural analysis. We have developed an integrated TLS data collection and point-based analysis workflow that incorporates accurate assessments of aleatoric and epistemic uncertainties using experimental surveys, Monte Carlo simulations, and iterative site reconstructions. Our scanning workflow and equipment requirements are optimized for single-operator surveying, and our data analysis process is largely completed using new point-based computing tools in an immersive 3D virtual reality environment. In a case study, we measured slip vector orientations at two sites along the rupture trace of the 1954 Dixie Valley earthquake (central Nevada, United States), yielding measurements that are the first direct constraints on the 3D slip vector for this event. These observations are consistent with a previous approximation of net extension direction for this event. We find that errors introduced by variables in our survey method result in <2.5 cm of variability in components of displacement, and are eclipsed by the 10–60 cm epistemic errors introduced by reconstructing the field sites to their pre-erosion geometries. Although the higher resolution TLS data sets enabled visualization and data interactivity critical for reconstructing the 3D slip vector and for assessing uncertainties, dense topographic constraints alone were not sufficient to significantly narrow the wide (<26°) range of allowable slip vector orientations that resulted from accounting for epistemic uncertainties.

  18. Determining the numbers of a landscape architect species (Tapirus terrestris), using footprints.

    Science.gov (United States)

    Moreira, Danielle O; Alibhai, Sky K; Jewell, Zoe C; da Cunha, Cristina J; Seibert, Jardel B; Gatti, Andressa

    2018-01-01

    As a landscape architect and a major seed disperser, the lowland tapir ( Tapirus terrestris ) is an important indicator of the ecological health of certain habitats. Therefore, reliable data regarding tapir populations are fundamental in understanding ecosystem dynamics, including those associated with the Atlantic Forest in Brazil. Currently, many population monitoring studies use invasive tagging with radio or satellite/Global Positioning System (GPS) collars. These techniques can be costly and unreliable, and the immobilization required carries physiological risks that are undesirable particularly for threatened and elusive species such as the lowland tapir. We collected data from one of the last regions with a viable population of lowland tapir in the south-eastern Atlantic Forest, Brazil, using a new non-invasive method for identifying species, the footprint identification technique (FIT). We identified the minimum number of tapirs in the study area and, in addition, we observed that they have overlapping ranges. Four hundred and forty footprints from 46 trails collected from six locations in the study area in a landscape known to contain tapir were analyzed, and 29 individuals were identified from these footprints. We demonstrate a practical application of FIT for lowland tapir censusing. Our study shows that FIT is an effective method for the identification of individuals of a threatened species, even when they lack visible natural markings on their bodies. FIT offers several benefits over other methods, especially for tapir management. As a non-invasive method, it can be used to census or monitor species, giving rapid feedback to managers of protected areas.

  19. Determining the numbers of a landscape architect species (Tapirus terrestris, using footprints

    Directory of Open Access Journals (Sweden)

    Danielle O. Moreira

    2018-03-01

    Full Text Available Background As a landscape architect and a major seed disperser, the lowland tapir (Tapirus terrestris is an important indicator of the ecological health of certain habitats. Therefore, reliable data regarding tapir populations are fundamental in understanding ecosystem dynamics, including those associated with the Atlantic Forest in Brazil. Currently, many population monitoring studies use invasive tagging with radio or satellite/Global Positioning System (GPS collars. These techniques can be costly and unreliable, and the immobilization required carries physiological risks that are undesirable particularly for threatened and elusive species such as the lowland tapir. Methods We collected data from one of the last regions with a viable population of lowland tapir in the south-eastern Atlantic Forest, Brazil, using a new non-invasive method for identifying species, the footprint identification technique (FIT. Results We identified the minimum number of tapirs in the study area and, in addition, we observed that they have overlapping ranges. Four hundred and forty footprints from 46 trails collected from six locations in the study area in a landscape known to contain tapir were analyzed, and 29 individuals were identified from these footprints. Discussion We demonstrate a practical application of FIT for lowland tapir censusing. Our study shows that FIT is an effective method for the identification of individuals of a threatened species, even when they lack visible natural markings on their bodies. FIT offers several benefits over other methods, especially for tapir management. As a non-invasive method, it can be used to census or monitor species, giving rapid feedback to managers of protected areas.

  20. Determination of atmospheric nitrogen dioxide by sampling with impregnated filters

    International Nuclear Information System (INIS)

    Galiano, J.A.; Palomares, F.

    1978-01-01

    The performance of filters impregnated with triethanolamine for the collection and subsequent determination of atmospheric nitrogen dioxide is studied taking into account the influence of several parameters: storage of filters, reagents, elapsed time, sampling efficiency, etc. The results obtained for sampling times of 24 hours are satisfactory. (author) [es

  1. A flexible method for multi-level sample size determination

    International Nuclear Information System (INIS)

    Lu, Ming-Shih; Sanborn, J.B.; Teichmann, T.

    1997-01-01

    This paper gives a flexible method to determine sample sizes for both systematic and random error models (this pertains to sampling problems in nuclear safeguard questions). In addition, the method allows different attribute rejection limits. The new method could assist achieving a higher detection probability and enhance inspection effectiveness

  2. Determination of Phenols in Water Samples using a Supported ...

    African Journals Online (AJOL)

    The sample preparation method was tested for the determination of phenols in river water samples and landfill leachate. Concentrations of phenols in river water were found to be in the range 4.2 μg L–1 for 2-chlorophenol to 50 μg L–1 for 4-chlorophenol. In landfill leachate, 4-chlorophenol was detected at a concentration ...

  3. Determination of average activating thermal neutron flux in bulk samples

    International Nuclear Information System (INIS)

    Doczi, R.; Csikai, J.; Doczi, R.; Csikai, J.; Hassan, F. M.; Ali, M.A.

    2004-01-01

    A previous method used for the determination of the average neutron flux within bulky samples has been applied for the measurements of hydrogen contents of different samples. An analytical function is given for the description of the correlation between the activity of Dy foils and the hydrogen concentrations. Results obtained by the activation and the thermal neutron reflection methods are compared

  4. Trace determination of uranium in fertilizer samples by total ...

    Indian Academy of Sciences (India)

    the fertilizers is important because it can be used as fuel in nuclear reactors and also because of en- vironmental concerns. ... The amounts of uranium in four fertilizer samples of Hungarian origin were determined by ... TXRF determination of uranium from phosphate fertilizers of Hungarian origin and the preliminary results ...

  5. An improved facile method for extraction and determination of steroidal saponins in Tribulus terrestris by focused microwave-assisted extraction coupled with GC-MS.

    Science.gov (United States)

    Li, Tianlin; Zhang, Zhuomin; Zhang, Lan; Huang, Xinjian; Lin, Junwei; Chen, Guonan

    2009-12-01

    An improved fast method for extraction of steroidal saponins in Tribulus terrestris based on the use of focus microwave-assisted extraction (FMAE) is proposed. Under optimized conditions, four steroidal saponins were extracted from Tribulus terrestris and identified by GC-MS, which are Tigogenin (TG), Gitogenin (GG), Hecogenin (HG) and Neohecogenin (NG). One of the most important steroidal saponins, namely TG was quantified finally. The recovery of TG was in the range of 86.7-91.9% with RSDTribulus terrestris from different areas of occurrence. The difference in chromatographic characteristics of steroidal saponins was proved to be related to the different areas of occurrence. The results showed that FMAE-GC-MS is a simple, rapid, solvent-saving method for the extraction and determination of steroidal saponins in Tribulus terrestris.

  6. Determination of uranium in industrial and environmental samples. Vol. 4

    Energy Technology Data Exchange (ETDEWEB)

    El-Sweify, F H; Shehata, M K; Metwally, E M; El-Shazly, E A.A.; El-Naggar, H A [Nuclear Chemistry Department, Hot Laborities Center, Atomic Energy Authority, Cairo (Egypt)

    1996-03-01

    The phosphate ores used at `Abu zaabal fertilizer and chemical company` for the production of some chemicals and fertilizers contain detectable amounts of uranium. In this study, the content of uranium in samples of different products of fertilizers, gypsum, and phosphate ore were determined using NAA, and gamma ray spectroscopy of the irradiated samples. Another method based on measuring the natural radioactivity of {sup 238} U series for non-irradiated samples using gamma-ray spectroscopy was also used for determine uranium content in the samples. In the NAA method, the content of U(ppm) in the samples was been computed from the photopeak activity of the lines = 106.1, 228.2, and 277.5 KeV of {sup 239} Np induced in the irradiated samples, and the uranium standard simultaneously irradiated. the gamma-ray spectra, and the decay curves are given. In the second method the gamma-ray spectra of the natural radioactivity of the samples and uranium standard were measured. The gamma-transition of energies 295.1, 251.9 KeV for {sup 214} Pb; 609.3, 768.4, 1120.3, 1238.1 KeV for {sup 214} Bi were determined. The uranium {sup 23U} traces in drainage water was also determined spectrophotometrically using arsenazo-III after preconcentration of uranium from the pretreated drainage water in column packed with chelex-100 resin. The recovery was found to be 90 {+-} 5%. 11 figs., 3 tabs.

  7. The determination of irradiation and so-called terrestrial ageing of rock meteorites based on the cosmogenic resulting radionuclides 53Mn and 26Al

    International Nuclear Information System (INIS)

    Englert, P.

    1979-01-01

    The contents of cosmogenic occuring 53 Mn was determined by neutron activation in over 90 samples of 75 individual rock meteorites. The distinct depth effect of the 53 Mn production rate in rock meteorites could be measured by a depth profile at LL6 chondrite St. Severin (falling weight 271 kg). The experimental results confirm the present model concepts. By comparing with the spallogenic 22 Ne/ 21 Ne and 3 He/ 21 Ne ratios applicable as depth indicators, one could derive linear relationships suitable for correcting 53 Mn. They enable the determination of the average 53 Mn production rate from the saturation activities of long-term irradiated meteorites. Using this method it was possible to calculate the irradiation age of 40 rock meteorites. As 26 Al is formed with a similar effective cross-section to 53 Mn, the production rate ratio 53 Mn: 26 Al was also taken to derive the depth-independent irradiation ages. A method to determine the depth-independent terrestrial ageing of meteriorites has been developed based on the same isotope ratio, the effective field of application is between 0.10 to 2x10 6 a. Furthermore, an attempt was made to draw up the dependence of noble gas contents of 53 Mn resp. 53 Mn/ 26 Al irradiation age for the new determination of the 3 He, 21 Ne and 38 Ar production rates by means of a linear regression analysis. (orig./RB) [de

  8. 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)

  9. Determination of uranium and its isotopic ratios in environmental samples

    International Nuclear Information System (INIS)

    Flues Szeles, M.S.M.

    1990-01-01

    A method for the determination of uranium and its isotopic ratios ( sup(235)U/ sup(238)U and sup(234U/ sup(238)U) is established in the present work. The method can be applied in environmental monitoring programs of uranium enrichment facilities. The proposed method is based on the alpha spectrometry technique which is applied after a purification of the sample by using an ionic exchange resin. The total yield achieved was (91 + 5)% with a precision of 5%, an accuracy of 8% and a lower limit of detection of 7,9 x 10 sup(-4)Bq. The uranium determination in samples containing high concentration of iron, which is an interfering element present in environmental samples, particularly in soil and sediment, was also studied. The results obtained by using artificial samples containing iron and uranium in the ratio 1000:1, were considered satisfactory. (author)

  10. 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)

  11. Sample size determination for mediation analysis of longitudinal data.

    Science.gov (United States)

    Pan, Haitao; Liu, Suyu; Miao, Danmin; Yuan, Ying

    2018-03-27

    Sample size planning for longitudinal data is crucial when designing mediation studies because sufficient statistical power is not only required in grant applications and peer-reviewed publications, but is essential to reliable research results. However, sample size determination is not straightforward for mediation analysis of longitudinal design. To facilitate planning the sample size for longitudinal mediation studies with a multilevel mediation model, this article provides the sample size required to achieve 80% power by simulations under various sizes of the mediation effect, within-subject correlations and numbers of repeated measures. The sample size calculation is based on three commonly used mediation tests: Sobel's method, distribution of product method and the bootstrap method. Among the three methods of testing the mediation effects, Sobel's method required the largest sample size to achieve 80% power. Bootstrapping and the distribution of the product method performed similarly and were more powerful than Sobel's method, as reflected by the relatively smaller sample sizes. For all three methods, the sample size required to achieve 80% power depended on the value of the ICC (i.e., within-subject correlation). A larger value of ICC typically required a larger sample size to achieve 80% power. Simulation results also illustrated the advantage of the longitudinal study design. The sample size tables for most encountered scenarios in practice have also been published for convenient use. Extensive simulations study showed that the distribution of the product method and bootstrapping method have superior performance to the Sobel's method, but the product method was recommended to use in practice in terms of less computation time load compared to the bootstrapping method. A R package has been developed for the product method of sample size determination in mediation longitudinal study design.

  12. Preconcentration NAA for simultaneous multielemental determination in water sample

    International Nuclear Information System (INIS)

    Chatt, A.

    1999-01-01

    Full text: Environment concerns with water, air, land and their interrelationship viz., human beings, fauna and flora. One of the important environmental compartments is water. Elements present in water might face a whole lot of physico-chemical conditions. This poses challenges to measure their total concentrations as well as different species. Preconcentration of the elements present in water samples is a necessary requisites in water analysis. For multi elements concentration measurements, Neutron Activation Analysis (NAA) is one of the preferred analytical techniques due to its sensitivity and selectivity. In this talk preconcentration NAA for multielemental determination in water sample determination will be discussed

  13. Determination and optimization of spatial samples for distributed measurements.

    Energy Technology Data Exchange (ETDEWEB)

    Huo, Xiaoming (Georgia Institute of Technology, Atlanta, GA); Tran, Hy D.; Shilling, Katherine Meghan; Kim, Heeyong (Georgia Institute of Technology, Atlanta, GA)

    2010-10-01

    There are no accepted standards for determining how many measurements to take during part inspection or where to take them, or for assessing confidence in the evaluation of acceptance based on these measurements. The goal of this work was to develop a standard method for determining the number of measurements, together with the spatial distribution of measurements and the associated risks for false acceptance and false rejection. Two paths have been taken to create a standard method for selecting sampling points. A wavelet-based model has been developed to select measurement points and to determine confidence in the measurement after the points are taken. An adaptive sampling strategy has been studied to determine implementation feasibility on commercial measurement equipment. Results using both real and simulated data are presented for each of the paths.

  14. Fluorimetrich determination of uranium in mineral samples and phosphoric solutions

    International Nuclear Information System (INIS)

    Pupo Gonzales, I.; Cuevillas, J.; Estevez, J.

    1991-01-01

    In this paper an analytical technique for the determination of uranium in different cuban minerals and acid leaching liquors of phosphorites is proposed. The method used for solid samples includes their disolution and further dilution of the solution obtained. For liquid samples dilution is the only intermediate step used. A study of HNO3 concentration (pH) was made in fluorimetric measurements. The method was applied to the uranium analysis in two IAEA standard reference samples (phosphate base), in natural phosphorites and a synthetic one, in clays and phosphoric liquors. The results agree with those obtained by other methods

  15. Determination of Pu, Am and Cm in Environmental Samples

    Energy Technology Data Exchange (ETDEWEB)

    Lujaniene, G. [SRI Centre for Physical Sciences and Technology, Vilnius (Lithuania)

    2013-07-15

    The determination of actinides in the environmental samples at a lower detection limit is required for monitoring purposes and for environmental research. The method for Pu, Am and Cm measurements in soil and sediment samples provides high recoveries and good decontamination from interfering radionuclides. The main steps of the method involve digestion of the samples, separation of radionuclides from matrix using the TOPO /cyclohexane extraction and final purification using extraction Eichrom resins (TEVA, TRU). The accuracy and precision of Pu, Am and Cm analyses were tested using IAEA RM No 135, NIST SRM No 4350b, No 4357 and in intercomparison runs organized by the Riso National Laboratory, Denmark, and in the proficiency tests organized by National Physical Laboratory, UK. The method was applied for measurement of radionuclides in aerosol samples (ashes {approx}30 g), bottom sediments (50-80 g dr. wt) and soil (including Chernobyl soil) samples. (author)

  16. Determination of tritium in wine and wine yeast samples

    International Nuclear Information System (INIS)

    Cotarlea, Monica-Ionela; Paunescu, Niculina; Galeriu, D.; Mocanu, N.; Margineanu, R.; Marin, G.

    1997-01-01

    A sensitive method for evaluating the tritium content in wine and wine yeast was applied to estimate tritium impact on the environment in the surrounding area of nuclear power plant Cernavoda, where the vineyards are part of representative agricultural ecosystem. Analytical procedures were developed to determine HTO in wine and wine yeast samples. The content of organic compounds affecting the LSC measurement is reduced by fractionating distillation for wine samples and azeotropic distillation followed by fractional distillation for wine yeast samples. Finally, the water samples obtained after fractional distillation were normally distilled with KMO 4 . The established procedures were successfully applied for wine and wine yeast samples from Mulfatlar harvests of the years 1995 and 1996. (authors)

  17. Sample size determination for equivalence assessment with multiple endpoints.

    Science.gov (United States)

    Sun, Anna; Dong, Xiaoyu; Tsong, Yi

    2014-01-01

    Equivalence assessment between a reference and test treatment is often conducted by two one-sided tests (TOST). The corresponding power function and sample size determination can be derived from a joint distribution of the sample mean and sample variance. When an equivalence trial is designed with multiple endpoints, it often involves several sets of two one-sided tests. A naive approach for sample size determination in this case would select the largest sample size required for each endpoint. However, such a method ignores the correlation among endpoints. With the objective to reject all endpoints and when the endpoints are uncorrelated, the power function is the production of all power functions for individual endpoints. With correlated endpoints, the sample size and power should be adjusted for such a correlation. In this article, we propose the exact power function for the equivalence test with multiple endpoints adjusted for correlation under both crossover and parallel designs. We further discuss the differences in sample size for the naive method without and with correlation adjusted methods and illustrate with an in vivo bioequivalence crossover study with area under the curve (AUC) and maximum concentration (Cmax) as the two endpoints.

  18. [Progress on Determination and Analysis of Zopiclone in Biological Samples].

    Science.gov (United States)

    Shu, C X; Gong, D; Zhang, L P; Zhao, J X

    2017-12-01

    As a new hypnotic, zopiclone is widely used in clinical treatment. There are many methods for determination of zopiclone, including spectrophotometry, chromatography and chromatography mass spectrum, etc. Present paper reviews different kinds of biological samples associated with zopiclone, extraction and purification methods, and determination and analysis methods, which aims to provide references for the relevant research and practice. Copyright© by the Editorial Department of Journal of Forensic Medicine.

  19. Terrestrial laser scanning and a degenerated cylinder model to determine gross morphological change of cadavers under conditions of natural decomposition.

    Science.gov (United States)

    Zhang, Xiao; Glennie, Craig L; Bucheli, Sibyl R; Lindgren, Natalie K; Lynne, Aaron M

    2014-08-01

    Decomposition can be a highly variable process with stages that are difficult to quantify. Using high accuracy terrestrial laser scanning a repeated three-dimensional (3D) documentation of volumetric changes of a human body during early decomposition is recorded. To determine temporal volumetric variations as well as 3D distribution of the changed locations in the body over time, this paper introduces the use of multiple degenerated cylinder models to provide a reasonable approximation of body parts against which 3D change can be measured and visualized. An iterative closest point algorithm is used for 3D registration, and a method for determining volumetric change is presented. Comparison of the laser scanning estimates of volumetric change shows good agreement with repeated in-situ measurements of abdomen and limb circumference that were taken diurnally. The 3D visualizations of volumetric changes demonstrate that bloat is a process with a beginning, middle, and end rather than a state of presence or absence. Additionally, the 3D visualizations show conclusively that cadaver bloat is not isolated to the abdominal cavity, but also occurs in the limbs. Detailed quantification of the bloat stage of decay has the potential to alter how the beginning and end of bloat are determined by researchers and can provide further insight into the effects of the ecosystem on decomposition. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

  20. Sample processing method for the determination of perchlorate in milk

    International Nuclear Information System (INIS)

    Dyke, Jason V.; Kirk, Andrea B.; Kalyani Martinelango, P.; Dasgupta, Purnendu K.

    2006-01-01

    In recent years, many different water sources and foods have been reported to contain perchlorate. Studies indicate that significant levels of perchlorate are present in both human and dairy milk. The determination of perchlorate in milk is particularly important due to its potential health impact on infants and children. As for many other biological samples, sample preparation is more time consuming than the analysis itself. The concurrent presence of large amounts of fats, proteins, carbohydrates, etc., demands some initial cleanup; otherwise the separation column lifetime and the limit of detection are both greatly compromised. Reported milk processing methods require the addition of chemicals such as ethanol, acetic acid or acetonitrile. Reagent addition is undesirable in trace analysis. We report here an essentially reagent-free sample preparation method for the determination of perchlorate in milk. Milk samples are spiked with isotopically labeled perchlorate and centrifuged to remove lipids. The resulting liquid is placed in a disposable centrifugal ultrafilter device with a molecular weight cutoff of 10 kDa, and centrifuged. Approximately 5-10 ml of clear liquid, ready for analysis, is obtained from a 20 ml milk sample. Both bovine and human milk samples have been successfully processed and analyzed by ion chromatography-mass spectrometry (IC-MS). Standard addition experiments show good recoveries. The repeatability of the analytical result for the same sample in multiple sample cleanup runs ranged from 3 to 6% R.S.D. This processing technique has also been successfully applied for the determination of iodide and thiocyanate in milk

  1. Determining sample size for assessing species composition in ...

    African Journals Online (AJOL)

    Species composition is measured in grasslands for a variety of reasons. Commonly, observations are made using the wheel-point apparatus, but the problem of determining optimum sample size has not yet been satisfactorily resolved. In this study the wheel-point apparatus was used to record 2 000 observations in each of ...

  2. Determination of thiobencarb in water samples by gas ...

    African Journals Online (AJOL)

    Homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA) coupled with gas chromatography-flame ionization detection (GC-FID) was applied for the extraction and determination of thiobencarb in water samples. In this study, a special extraction cell was designed to facilitate collection of the ...

  3. Determination of lead at nanogram level in water samples by ...

    African Journals Online (AJOL)

    A novel method of chemistry applicable to the determination of trace lead in water samples based on the resonance light scattering (RLS) technique has been developed. In dilute phosphoric acid medium, in the presence of a large excess of I-, Pb(II) can form [PbI4]2-, which further reacts with tetrabutyl ammonium bromide ...

  4. Improved sample capsule for determination of oxygen in hemolyzed blood

    Science.gov (United States)

    Malik, W. M.

    1967-01-01

    Sample capsule for determination of oxygen in hemolyzed blood consists of a measured section of polytetrafluoroethylene tubing equipped at each end with a connector and a stopcock valve. This method eliminates errors from air entrainment or from the use of mercury or syringe lubricant.

  5. 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] ...

  6. Experimental determination of size distributions: analyzing proper sample sizes

    International Nuclear Information System (INIS)

    Buffo, A; Alopaeus, V

    2016-01-01

    The measurement of various particle size distributions is a crucial aspect for many applications in the process industry. Size distribution is often related to the final product quality, as in crystallization or polymerization. In other cases it is related to the correct evaluation of heat and mass transfer, as well as reaction rates, depending on the interfacial area between the different phases or to the assessment of yield stresses of polycrystalline metals/alloys samples. The experimental determination of such distributions often involves laborious sampling procedures and the statistical significance of the outcome is rarely investigated. In this work, we propose a novel rigorous tool, based on inferential statistics, to determine the number of samples needed to obtain reliable measurements of size distribution, according to specific requirements defined a priori. Such methodology can be adopted regardless of the measurement technique used. (paper)

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

    DEFF Research Database (Denmark)

    Shi, Keliang; Hou, Xiaolin; Roos, Per

    2012-01-01

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

  8. Biomass Thermogravimetric Analysis: Uncertainty Determination Methodology and Sampling Maps Generation

    Science.gov (United States)

    Pazó, Jose A.; Granada, Enrique; Saavedra, Ángeles; Eguía, Pablo; Collazo, Joaquín

    2010-01-01

    The objective of this study was to develop a methodology for the determination of the maximum sampling error and confidence intervals of thermal properties obtained from thermogravimetric analysis (TG), including moisture, volatile matter, fixed carbon and ash content. The sampling procedure of the TG analysis was of particular interest and was conducted with care. The results of the present study were compared to those of a prompt analysis, and a correlation between the mean values and maximum sampling errors of the methods were not observed. In general, low and acceptable levels of uncertainty and error were obtained, demonstrating that the properties evaluated by TG analysis were representative of the overall fuel composition. The accurate determination of the thermal properties of biomass with precise confidence intervals is of particular interest in energetic biomass applications. PMID:20717532

  9. Quality Control Samples for the Radiological Determination of Tritium in Urine Samples

    International Nuclear Information System (INIS)

    Ost'pezuk, P.; Froning, M.; Laumen, S.; Richert, I.; Hill, P.

    2004-01-01

    The radioactive decay product of tritium is a low energy beta that cannot penetrate the outer dead layer of human skin. Therefore , the main hazard associated with tritium is internal exposure. In addition, due to the relatively long half life and short biological half life, tritium must be ingested in large amounts to pose a significant health risk. On the other hand, the internal exposure should be kept as low as practical. For incorporation monitoring of professional radiation workers the quality control is of utmost importance. In the Research Centre Juelich GmbH (FZJ) a considerable fraction of monitoring by excretion analysis relates to the isotope Tritium. Usually an aliquot of an urine sample is mixed with a liquid scintillator and measured in a liquid scintillation counter. Quality control samples in the form of three kind of internal reference samples (blank, reference samples with low activity and reference sample with elevated activity) were prepared from a mixed, Tritium (free) urine samples. 1 ml of these samples were pipetted into a liquid scintillation vial. In the part of theses vials a known amounts of Tritium were added. All these samples were stored at 20 degrees. Based on long term use of all these reference samples it was possible to construct appropriate control charts with the upper and lower alarm limits. Daily use of these reference samples decrease significantly the risk for false results in original urine with no significant increase of the determination time. (Author) 2 refs

  10. Conservative Sample Size Determination for Repeated Measures Analysis of Covariance.

    Science.gov (United States)

    Morgan, Timothy M; Case, L Douglas

    2013-07-05

    In the design of a randomized clinical trial with one pre and multiple post randomized assessments of the outcome variable, one needs to account for the repeated measures in determining the appropriate sample size. Unfortunately, one seldom has a good estimate of the variance of the outcome measure, let alone the correlations among the measurements over time. We show how sample sizes can be calculated by making conservative assumptions regarding the correlations for a variety of covariance structures. The most conservative choice for the correlation depends on the covariance structure and the number of repeated measures. In the absence of good estimates of the correlations, the sample size is often based on a two-sample t-test, making the 'ultra' conservative and unrealistic assumption that there are zero correlations between the baseline and follow-up measures while at the same time assuming there are perfect correlations between the follow-up measures. Compared to the case of taking a single measurement, substantial savings in sample size can be realized by accounting for the repeated measures, even with very conservative assumptions regarding the parameters of the assumed correlation matrix. Assuming compound symmetry, the sample size from the two-sample t-test calculation can be reduced at least 44%, 56%, and 61% for repeated measures analysis of covariance by taking 2, 3, and 4 follow-up measures, respectively. The results offer a rational basis for determining a fairly conservative, yet efficient, sample size for clinical trials with repeated measures and a baseline value.

  11. Radionuclide Concentrations in Terrestrial Vegetation and Soil Samples On and Around the Hanford Site, 1971 Through 2008

    Energy Technology Data Exchange (ETDEWEB)

    Simmons, Mary Ann; Poston, Ted M.; Fritz, Brad G.; Bisping, Lynn E.

    2011-07-29

    Environmental monitoring is conducted on the U.S. Department of Energy (DOE) Hanford Site to comply with DOE Orders and federal and state regulations. Major objectives of the monitoring are to characterize contaminant levels in the environment and to determine site contributions to the contaminant inventory. This report focuses on surface soil and perennial vegetation samples collected between 1971 and 2008 as part of the Pacific Northwest National Laboratory Surface Environmental Surveillance Project performed under contract to DOE. Areas sampled under this program are located on the Hanford Site but outside facility boundaries and on public lands surrounding the Hanford Site. Additional samples were collected during the past 8 years under DOE projects that evaluated parcels of land for radiological release. These data were included because the same sampling methodology and analytical laboratory were used for the projects. The spatial and temporal trends of six radionuclides collected over a 38-year period were evaluated. The radionuclides----cobalt-60, cesium-137, strontium-90, plutonium-238, plutonium-239/240, and uranium (reported either as uranium-238 or total uranium)----were selected because they persist in the environment and are still being monitored routinely and reported in Hanford Site environmental reports. All these radionuclides were associated with plutonium production and waste management of activities occurring on the site. Other sources include fallout from atmospheric testing of nuclear weapons, which ended in 1980, and the Chernobyl explosion in 1986. Uranium is also a natural component of the soil. This assessment of soil and vegetation data provides important information on the distribution of radionuclides in areas adjacent to industrial areas, established perimeter locations and buffer areas, and more offsite nearby and distant locations. The concentrations reflect a tendency for detection of some radionuclides close to where they were

  12. Multiple determinants of whole and regional brain volume among terrestrial carnivorans.

    Directory of Open Access Journals (Sweden)

    Eli M Swanson

    Full Text Available Mammalian brain volumes vary considerably, even after controlling for body size. Although several hypotheses have been proposed to explain this variation, most research in mammals on the evolution of encephalization has focused on primates, leaving the generality of these explanations uncertain. Furthermore, much research still addresses only one hypothesis at a time, despite the demonstrated importance of considering multiple factors simultaneously. We used phylogenetic comparative methods to investigate simultaneously the importance of several factors previously hypothesized to be important in neural evolution among mammalian carnivores, including social complexity, forelimb use, home range size, diet, life history, phylogeny, and recent evolutionary changes in body size. We also tested hypotheses suggesting roles for these variables in determining the relative volume of four brain regions measured using computed tomography. Our data suggest that, in contrast to brain size in primates, carnivoran brain size may lag behind body size over evolutionary time. Moreover, carnivore species that primarily consume vertebrates have the largest brains. Although we found no support for a role of social complexity in overall encephalization, relative cerebrum volume correlated positively with sociality. Finally, our results support negative relationships among different brain regions after accounting for overall endocranial volume, suggesting that increased size of one brain regions is often accompanied by reduced size in other regions rather than overall brain expansion.

  13. Determination of nitrite, nitrate and total nitrogen in vegetable samples

    Directory of Open Access Journals (Sweden)

    Manas Kanti Deb

    2007-04-01

    Full Text Available Yellow diazonium cation formed by reaction of nitrite with 6-amino-1-naphthol-3-sulphonic acid is coupled with β-naphthol in strong alkaline medium to yield a pink coloured azo dye. The azo-dyes shows absorption maximum at 510 nm with molar absorptivity of 2.5 ×104 M-1 cm-1. The dye product obeys Beer's law (correlation coefficient = 0.997, in terms of nitrite concentration, up to 2.7 μg NO2 mL-1. The above colour reaction system has been applied successfully for the determination of nitrite, nitrate and total nitrogen in vegetable samples. Unreduced samples give direct measure for nitrite whilst reduction of samples by copperized-cadmium column gives total nitrogen content and their difference shows nitrate content in the samples. Variety of vegetables have been tested for their N-content (NO2-/NO3-/total-N with % RSD ranging between 1.5 to 2.5 % for nitrite determination. The effects of foreign ions in the determination of the nitrite, nitrate, and total nitrogen have been studied. Statistical comparison of the results with those of reported method shows good agreement and indicates no significant difference in precision.

  14. Determination of sampling constants in NBS geochemical standard reference materials

    International Nuclear Information System (INIS)

    Filby, R.H.; Bragg, A.E.; Grimm, C.A.

    1986-01-01

    Recently Filby et al. showed that, for several elements, National Bureau of Standards (NBS) Fly Ash standard reference material (SRM) 1633a was a suitable reference material for microanalysis (sample weights 2 , and the mean sample weight, W vector, K/sub s/ = (S/sub s/%) 2 W vector, could not be determined from these data because it was not possible to quantitate other sources of error in the experimental variances. K/sub s/ values for certified elements in geochemical SRMs provide important homogeneity information for microanalysis. For mineralogically homogeneous SRMs (i.e., small K/sub s/ values for associated elements) such as the proposed clays, it is necessary to determine K/sub s/ by analysis of very small sample aliquots to maximize the subsampling variance relative to other sources of error. This source of error and the blank correction for the sample container can be eliminated by determining K/sub s/ from radionuclide activities of weighed subsamples of a preirradiated SRM

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  16. System to determine present elements in oily samples

    International Nuclear Information System (INIS)

    Mendoza G, Y.

    2004-11-01

    In the Chemistry Department of the National Institute of Nuclear Investigations of Mexico, dedicated to analyze samples of oleaginous material and of another origin, to determine the elements of the periodic table present in the samples, through the Neutron activation analysis technique (NAA). This technique has been developed to determine majority elements in any solid, aqueous, industrial and environmental sample, which consists basically on to irradiate a sample with neutrons coming from the TRIGA Mark III reactor and to carry out the analysis to obtain those gamma spectra that it emits, for finally to process the information, the quantification of the analysis it is carried out in a manual way, which requires to carry out a great quantity of calculations. The main objective of this project is the development of a software that allows to carry out the quantitative analysis of the NAA for the multielemental determination of samples in an automatic way. To fulfill the objective of this project it has been divided in four chapters: In the first chapter it is shortly presented the history on radioactivity and basic concepts that will allow us penetrate better to this work. In the second chapter the NAA is explained which is used in the sample analysis, the description of the process to be carried out, its are mentioned the characteristics of the used devices and an example of the process is illustrated. In the third chapter it is described the development of the algorithm and the selection of the programming language. The fourth chapter it is shown the structure of the system, the general form of operation, the execution of processes and the obtention of results. Later on the launched results are presented in the development of the present project. (Author)

  17. Determination of 210Pb and 210Po in water samples

    International Nuclear Information System (INIS)

    Ayranov, M.; Tosheva, Z.; Kies, A.

    2004-01-01

    Lead-210 and Polonium-210 are naturally occurring members of the Uranium-238 decay series. They could be found in various environmental samples, such as groundwater, fish and shellfish, contributing an important component of the human natural radiation background. For this reason the development of a fast, reproducible and sensitive method for determination of 210 Pb and 210 Po is of a great concern. The aims of our study were to adopt procedures for radiochemical separation of these radionuclides and radioanalytical methods for their determination. The combination of electrochemical deposition, co-precipitation and extraction chromatography gives the opportunity for fast and effective radiochemical separation of the analytes. Polonium was spontaneously plated on copper disk from the stock solution. Lead was co-precipitated with Fe(OH) 3 and further purified by extraction chromatography on Sr Spec columns. Alpha spectra of polonium were collected on Canberra PIPS detectors with 900 mm 2 active surface. The activities of lead were determined by LSC (Gardian Wallac Oy). The minimum detectable activities for sample size 1000 mL and chemical yield of 88 % for the polonium and 85 % for the lead are presented. The proposed method proved to be fast, accurate and reproducible for routine determination of lead and polonium in environmental water samples. (authors)

  18. Determination of Sr-90 in rain water samples

    International Nuclear Information System (INIS)

    Lima, M.F.; Cunha, I.I.L.

    1988-01-01

    A work that aim is to establish radiochemical method for the determination of Sr-90 in rain water samples has been studied, as a step in an environmental monitoring program of radioactive elements. The analysis includes the preconcentration of strontium diluted in a large volume sample by precipitation of strontium as carbonate, separation of strontium from interfering elements (calcium, barium and rare earths), separation of strontium from ytrium, precipitation of purified strontium and ytrium respectively as carbonate and oxalate, and counting of Sr-90 and Y-90 activities in a low background anticoincidence beta counter. (author) [pt

  19. 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.

  20. A review of sample preparation and its influence on pH determination in concrete samples

    Directory of Open Access Journals (Sweden)

    S. Manso

    2017-01-01

    Full Text Available 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.

  1. In vitro assessment of Tribulus terrestris aqueous extract and Benzoxacin fraction against Helicobacter pylori isolates from biopsy samples of Iranian patients

    Directory of Open Access Journals (Sweden)

    Mojdeh Hakemi vala

    2014-02-01

    Full Text Available Background & Objectives:  Helicobacter pylori (Hp is related to gastritis, gastric ulcer, duodenal ulcer, and mucosal carcinoma. Emergence of multidrug resistant Hp strains encouraged the researchers to find new effective drugs. Especially medicinal herbs and plants which usually shows less side effects. The aim of this study was in vitro assessment of anti Hp activity of total extract of Tribulus terrestris (T. terrestris Benzoxacin, a local Iranian medicinal plant and its fraction Benzoxacin.Methods: total aqueous extract of aerial parts of the plant was prepared and liquid extraction with petroleum ether was used to separate its components. LC/MS system proved the existence of Benzoxazine derivative in the water fraction and the third's fraction. Anti (Hp effects of total extract and its third fraction were examined by cup plate method and using standard MacFarland. 50 biopsy samples of antrum were detected from patients who were endoscopic candidates in Milad and Fayazbakhsh  hospitals of Tehran during 2011. All samples were isolated, diagnosed based on standard methods and biochemical tests and confirmed by PCR method for ureC gene, too.  Different dilutions (250, 500,750 and 1000 mg/ml of total extract were prepared. Clarythromycin (Clr E-test strips and an identified Hp OC1096 was used, simultaneously.Results: Of 50 biopsy samples, 12 Hp strains were isolated. Rapid urease test were positive in all expect one biopsy sample. Existence of ureC gene in all isolates were confirmed expect one strain by PCR. By cup plate method, resistant to concentrations of 1000 and 750mg/ml were detected in 50% of Hp isolates and 66.6% of them were resistant to concentrations 250 and 500 mg/ml .Also, 83.3% of Hp strains were resistant to Benzoxacin fraction. Clarythromycin sensitivity detected in 83% of Hp isolates, simultaneously.Conclusion: This study was done as a pilot study for in vitro evaluation of antibacterial effect of total extract of T

  2. Determination of the spallogenic radionuclides 26Al and 53Mn in Antartic meteorites with respect to cosmic ray exposure and terrestrial ages

    International Nuclear Information System (INIS)

    Herpers, U.; Sarafin, R.

    1987-01-01

    The spallogenic radionuclides 26 Al (T=7.18x10 5 a) and 53 Mn (T=3.8x10 6 a) were determined in 11 ordinary chondrites and 7 achondrites from Antarctica by nondestructive coincidence counting techniques and radiochemical neutron activation analysis. The results are discussed with respect to exposure ages, terrestrial residence times and possible genetic relationships of the meteorites investigated. The high terrestrial ages of some specimens (up to 800 000 years) are of importance for the study of the ice flow in Antarctica. (author)

  3. Using the modified sample entropy to detect determinism

    Energy Technology Data Exchange (ETDEWEB)

    Xie Hongbo, E-mail: xiehb@sjtu.or [Department of Health Technology and Informatics, The Hong Kong Polytechnic University, Hung Hom, Kowloon (Hong Kong); Department of Biomedical Engineering, Jiangsu University, Zhenjiang (China); Guo Jingyi [Department of Health Technology and Informatics, Hong Kong Polytechnic University, Hung Hom, Kowloon (Hong Kong); Zheng Yongping, E-mail: ypzheng@ieee.or [Department of Health Technology and Informatics, Hong Kong Polytechnic University, Hung Hom, Kowloon (Hong Kong); Reseach Institute of Innovative Products and Technologies, Hong Kong Polytechnic University (Hong Kong)

    2010-08-23

    A modified sample entropy (mSampEn), based on the nonlinear continuous and convex function, has been proposed and proven to be superior to the standard sample entropy (SampEn) in several aspects. In this Letter, we empirically investigate the ability of the mSampEn statistic combined with surrogate data method to detect determinism. The effects of the datasets length and noise on the proposed method to differentiate between deterministic and stochastic dynamics are tested on several benchmark time series. The noise performance of the mSampEn statistic is also compared with the singular value decomposition (SVD) and symplectic geometry spectrum (SGS) based methods. The results indicate that the mSampEn statistic is a robust index for detecting determinism in short and noisy time series.

  4. Problem of cadmium, arsenic and zinc determination in enviroment samples

    International Nuclear Information System (INIS)

    Malyugin, M.S.; Luzhnova, M.A.; Lontsikh, S.V.

    1983-01-01

    Using the emission spectroscopy technique new information has been obtained on cadmium-, arsenic and zinc content in some reference samples (RS) of rocks and soils not previously certified as to the content of the elements, as well as in nealy issued RS of soils. Metrologic estimation of the results obtained is carried out. A comparison with the atomic-absorption analysis data as well as with those of the neutron-activation-, colorimetric and other methods of the analysis permits to refer to the advantages of using the spectrographic determination technique based on fractionated evaporation, in case of determining cadmium and arsenic in rocks and soils. Consideration of the results of cadmium, arsenic and zinc spectrography contributed greatly to the certification of reference samples of soils

  5. {sup 32}P-postlabeling determination of DNA adducts in the earthworm Lumbricus terrestris exposed to PAH-contaminated soils

    Energy Technology Data Exchange (ETDEWEB)

    Walsh, P. [Laval Univ. Research Center, Quebec (Canada)]|[Ministere de l`Environnement et de la Faune du Quebec (Canada); El Adlouni, C.; Mukhopadhyay, M.J.; Nadeau, D.; Poirier, G.G. [Laval Univ. Research Center, Quebec (Canada); Viel, G. [CreaLab., Quebec (Canada)

    1995-05-01

    The importance of the search for reliable biomarkers of DNA damage in environmental health assessment is well recognized by the scientific community and regulatory agencies. Among the major biomarkers of DNA damage is the measurement of DNA adducts in target cells or tissues. Up to now, DNA adduct determinations have been directed mostly toward human exposure to toxic substances from the workplace and environment. Moreover, techniques for measuring DNA adducts, and in particular the {sup 32}P-postlabelling technique, presented also the possibility of determining DNA adduct levels in endogenous animal populations exposed to polluted environments as early warning monitors of ecotoxicity. Soil contamination is becoming a major environmental issue. Therefore, numerous contaminated sites must now be remediated to protect human health and to permit new uses of these sites as agricultural, residential, or industrial areas. Fulfillment of this task requires standardized and sensitive bioassays to carry out site evaluations and to establish scientifically defensible soil quality criteria. To that effect, the earthworm appears to be one of the best organisms for use in soil toxicity evaluation. Earthworms are probably the most relevant soil species, representing 60 to 80% of the total animal biomass in soil. Present soil bioassays focus mostly on plant species with end points like seed germination, root elongation, seedling growth and seedling emergence, and on acute toxicity evaluation (re: LC 50) on the earthworm Eisenia fetida. As yet, a standardized soil invertebrate test for teratogenic or mutagenic end points has not been developed. In this paper, we report the feasibility of DNA adduct determination by {sup 32}P-postlabelling in the earthworm Lumbricus terrestris as a way to detect the presence of genotoxic substances in soils. 20 refs., 1 fig., 1 tab.

  6. Determination of platinum in biological samples by NAA

    International Nuclear Information System (INIS)

    Okada, Yukiko; Hirai, Shoji; Sakurai, Hiromu; Haraguchi, Hiroki.

    1990-01-01

    Recently, a Pt compound, Cisplatin (cis-dichlorodiamine platinum) has been used therapeutically as an effective anti-malignant-cancer drug. However, since this drug has a harmful aftereffect on kidney, an urgent study of how to reduce its toxicity without influencing the therapeutic effect is needed. We have to understand the behavior of Pt in biological organs in order to elucidate the mechanism of its toxicity reduction. In this study, the analytical conditions for the determination of Pt in biological samples by neutron activation analysis, such as cooling time, counting time and sample weight, are optimized. Freeze-dried samples of the liver, kidney and whole blood of a rat treated with Cisplatin were prepared to evaluate the precision of the analysis and the lower limit of determination. 199 Au (t 1/2 = 3.15 d) produced from 199 Pt (n, γ, β - ) was selected as the analytical radionuclide. A concentration of ca. 1 ppm Pt was determinable under the optimal conditions: a cooling time of 5 d and a counting time of 1 h. Pt in the respective organs of the control rat was not detected under the same analytical conditions. The concentrations of Pt in the liver, kidney, spleen, pancreas and lung of a rat treated with both Cisplatin and sodium selenite were higher than those of a rat treated only with Cisplatin. (author)

  7. Determination of copper in powdered chocolate samples by slurry-sampling flame atomic-absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Walter N.L. dos; Silva, Erik G.P. da; Fernandes, Marcelo S.; Araujo, Rennan G.O.; Costa, Anto' ' enio C.S.; Ferreira, Sergio L.C. [Nucleo de Excelencia em Quimica Analitica da Bahia, Universidade Federal da Bahia, Instituto de Quimica, Salvador, Bahia (Brazil); Vale, M.G.R. [Instituto de Quimica, Universidade Federal da Bahia do Rio Grande do Sul, Porto Alegre, Rio Grande do Sul (Brazil)

    2005-06-01

    Chocolate is a complex sample with a high content of organic compounds and its analysis generally involves digestion procedures that might include the risk of losses and/or contamination. The determination of copper in chocolate is important because copper compounds are extensively used as fungicides in the farming of cocoa. In this paper, a slurry-sampling flame atomic-absorption spectrometric method is proposed for determination of copper in powdered chocolate samples. Optimization was carried out using univariate methodology involving the variables nature and concentration of the acid solution for slurry preparation, sonication time, and sample mass. The recommended conditions include a sample mass of 0.2 g, 2.0 mol L{sup -1} hydrochloric acid solution, and a sonication time of 15 min. The calibration curve was prepared using aqueous copper standards in 2.0 mol L{sup -1} hydrochloric acid. This method allowed determination of copper in chocolate with a detection limit of 0.4 {mu}g g{sup -1} and precision, expressed as relative standard deviation (RSD), of 2.5% (n=10) for a copper content of approximately 30 {mu}g g{sup -1}, using a chocolate mass of 0.2 g. The accuracy was confirmed by analyzing the certified reference materials NIST SRM 1568a rice flour and NIES CRM 10-b rice flour. The proposed method was used for determination of copper in three powdered chocolate samples, the copper content of which varied between 26.6 and 31.5 {mu}g g{sup -1}. The results showed no significant differences with those obtained after complete digestion, using a t-test for comparison. (orig.)

  8. Terrestrial gamma radioactivity levels and their corresponding external exposure of some soil samples from Elba protective area, Southeastern of Egypt

    International Nuclear Information System (INIS)

    El Arabi, A.M.; Ahmed, N.K.; Salahel Din, K.; Tykva, R.

    2007-01-01

    The study of natural gamma radioactivity was made to determine the concentrations of natural radionuclides in soil. Fifty four surface soil samples collected from three different cites (Wadi Daeeb , Wadi Sarara and Wadi Hodein) in Elba protective area, Southeastern of Egypt, were analyzed by Nal(Tl) detector to determine the activity concentrations of 226 Ra, 232 Th and 40 K. The mean activity concentration of radionuclides 226 Ra, 232 Th and 40 K are 20.9±1.6, 13.5 ± 1.1 and 477 ± 24 Bq kg -1 , respectively for Wadi Daeeb soils. The corresponding values for Wadi Sarara and Wadi Hodein soils are 27.8 ± 2.6, 17.8 ± 1.4 and 735.3 ± 29.8 Bq kg -1 and 20.3 ± 1.5, 12 ± 1 and 664.2 ± 20 Bq kg -1 , respectively. In order to evaluate the radiological hazard of the natural radioactivity, the radium equivalent activity (Ra eq ) and gamma activity concentration index (I) have been calculated and compared with the internationally approved values. The average annual effective doses outdoors, indoors and in total are estimated to be 0.046, 0.26 and 0.30 mSv, respectively for Wadi Daeeb soils. For Wadi Sarara and Wadi Hodein soils the corresponding values are 0.066, 0.37 and 0.44 mSv and 0.054, 0.30 and 0.36 mSv, respectively. Also the annual gonadal dose equivalent was calculated and found to be within safe limit

  9. Determination of the stoichiometric ratio uranium dioxide samples

    International Nuclear Information System (INIS)

    Moura, Sergio Carvalho

    1999-01-01

    The determination of the O/U stoichiometric ratio in uranium dioxide is an important parameter in order to qualify nuclear fuels. The excess oxygen in the crystallographic structure can cause changes in the physico-chemical properties of this compound such as variation of the thermal conductivity alterations, fuel plasticity and others, affecting the efficiency of this material when it is utilized as nuclear fuel in the reactor core. The purpose of this work is to evaluate methods for the determination of uranium oxide samples from two different production processes, using gravimetric, voltammetric and X-ray diffraction techniques. After the evaluation of these techniques, the main aspect of this work is to define a reliable methodology in order to characterize the behavior of uranium oxide. The methodology used in this work consisted of two different steps: utilization of gravimetric and volumetric methods in order to determine the ratio in uranium dioxide samples; utilization of X-ray diffraction technique in order to determine the lattice parameters using patterns and application of the Rietveld method during refining of the structural data. As a result of the experimental part of this work it was found that the X-ray diffraction analysis performs better and detects the presence of more phases than gravimetric and voltammetric techniques, not sensitive enough in this detection. (author)

  10. Determination of radiostrontium in soil samples using a crown ether

    Energy Technology Data Exchange (ETDEWEB)

    Vajda, N; Ghods-Esphahani, A; Danesi, P R [International Atomic Energy Agency, Agency' s Laboratories, Chemistry Unit, PCI Laboratory, Seibersdorf (Austria)

    1995-07-01

    A simple and rapid method has been developed for the separation and successive determination of total radiostrontium in soil. The method consists of three basic steps: oxalate precipitation to remove bulk potassium, chromatographic separation of strontium from most inactive and radioactive interferences utilizing a crown ether (Sr. Spec, EIChroM Industries, II. USA), oxalate precipitation of strontium to evaluate the chemical yield. Radiostrontium is then determined by liquid scintillation counting of the dissolved precipitate. When 10 g samples of soil are used the sensitivity of the method is about 10 Bq/kg. The chemical yield is about 80%. The separation and determination of radiostrontium can be carried out in about 8 hours. (author)

  11. Determination of radiostrontium in soil samples using a crown ether

    International Nuclear Information System (INIS)

    Vajda, N.; Ghods-Esphahani, A.; Danesi, P.R.

    1995-01-01

    A simple and rapid method has been developed for the separation and successive determination of total radiostrontium in soil. The method consists of three basic steps: oxalate precipitation to remove bulk potassium, chromatographic separation of strontium from most inactive and radioactive interferences utilizing a crown ether (Sr. Spec, EIChroM Industries, II. USA), oxalate precipitation of strontium to evaluate the chemical yield. Radiostrontium is then determined by liquid scintillation counting of the dissolved precipitate. When 10 g samples of soil are used the sensitivity of the method is about 10 Bq/kg. The chemical yield is about 80%. The separation and determination of radiostrontium can be carried out in about 8 hours. (author)

  12. Optical methods for microstructure determination of doped samples

    Science.gov (United States)

    Ciosek, Jerzy F.

    2008-12-01

    The optical methods to determine refractive index profile of layered materials are commonly used with spectroscopic ellipsometry or transmittance/reflectance spectrometry. Measurements of spectral reflection and transmission usually permit to characterize optical materials and determine their refractive index. However, it is possible to characterize of samples with dopants, impurities as well as defects using optical methods. Microstructures of a hydrogenated crystalline Si wafer and a layer of SiO2 - ZrO2 composition are investigated. The first sample is a Si(001):H Czochralski grown single crystalline wafer with 50 nm thick surface Si02 layer. Hydrogen dose implantation (D continue to be an important issue in microelectronic device and sensor fabrication. Hydrogen-implanted silicon (Si: H) has become a topic of remarkable interest, mostly because of the potential of implantation-induced platelets and micro-cavities for the creation of gettering -active areas and for Si layer splitting. Oxygen precipitation and atmospheric impurity are analysed. The second sample is the layer of co-evaporated SiO2 and ZrO2 materials using simultaneously two electron beam guns in reactive evaporation methods. The composition structure was investigated by X-Ray photoelectron spectroscopy (XPS), and spectroscopic ellipsometry methods. A non-uniformity and composition of layer are analysed using average density method.

  13. Isotope determination of sulfur by mass spectrometry in soil samples

    Directory of Open Access Journals (Sweden)

    Alexssandra Luiza Rodrigues Molina Rossete

    2012-12-01

    Full Text Available Sulphur plays an essential role in plants and is one of the main nutrients in several metabolic processes. It has four stable isotopes (32S, 33S, 34S, and 36S with a natural abundance of 95.00, 0.76, 4.22, and 0.014 in atom %, respectively. A method for isotopic determination of S by isotope-ratio mass spectrometry (IRMS in soil samples is proposed. The procedure involves the oxidation of organic S to sulphate (S-SO4(2-, which was determined by dry combustion with alkaline oxidizing agents. The total S-SO4(2- concentration was determined by turbidimetry and the results showed that the conversion process was adequate. To produce gaseous SO2 gas, BaSO4 was thermally decomposed in a vacuum system at 900 ºC in the presence of NaPO3. The isotope determination of S (atom % 34S atoms was carried out by isotope ratio mass spectrometry (IRMS. In this work, the labeled material (K2(34SO4 was used to validate the method of isotopic determination of S; the results were precise and accurate, showing the viability of the proposed method.

  14. On-capillary sample cleanup method for the electrophoretic determination of carbohydrates in juice samples.

    Science.gov (United States)

    Morales-Cid, Gabriel; Simonet, Bartolomé M; Cárdenas, Soledad; Valcárcel, Miguel

    2007-05-01

    On many occasions, sample treatment is a critical step in electrophoretic analysis. As an alternative to batch procedures, in this work, a new strategy is presented with a view to develop an on-capillary sample cleanup method. This strategy is based on the partial filling of the capillary with carboxylated single-walled carbon nanotube (c-SWNT). The nanoparticles retain interferences from the matrix allowing the determination and quantification of carbohydrates (viz glucose, maltose and fructose). The precision of the method for the analysis of real samples ranged from 5.3 to 6.4%. The proposed method was compared with a method based on a batch filtration of the juice sample through diatomaceous earth and further electrophoretic determination. This method was also validated in this work. The RSD for this other method ranged from 5.1 to 6%. The results obtained by both methods were statistically comparable demonstrating the accuracy of the proposed methods and their effectiveness. Electrophoretic separation of carbohydrates was achieved using 200 mM borate solution as a buffer at pH 9.5 and applying 15 kV. During separation, the capillary temperature was kept constant at 40 degrees C. For the on-capillary cleanup method, a solution containing 50 mg/L of c-SWNTs prepared in 300 mM borate solution at pH 9.5 was introduced for 60 s into the capillary just before sample introduction. For the electrophoretic analysis of samples cleaned in batch with diatomaceous earth, it is also recommended to introduce into the capillary, just before the sample, a 300 mM borate solution as it enhances the sensitivity and electrophoretic resolution.

  15. Portable tester for determining gas content within a core sample

    Science.gov (United States)

    Garcia, F. Jr.; Schatzel, S.J.

    1998-04-21

    A portable tester is provided for reading and displaying the pressure of a gas released from a rock core sample stored within a sealed container and for taking a sample of the released pressurized gas for chemical analysis thereof for subsequent use in a modified direct method test which determines the volume of gas and specific type of gas contained within the core sample. The portable tester includes a pair of low and high range electrical pressure transducers for detecting a gas pressure; a pair of low and high range display units for displaying the pressure of the detected gas; a selector valve connected to the low and high range pressure transducers and a selector knob for selecting gas flow to one of the flow paths; control valve having an inlet connection to the sealed container; and outlets connected to: a sample gas canister, a second outlet port connected to the selector valve means for reading the pressure of the gas from the sealed container to either the low range or high range pressure transducers, and a connection for venting gas contained within the sealed container to the atmosphere. A battery is electrically connected to and supplies the power for operating the unit. The pressure transducers, display units, selector and control valve means and the battery is mounted to and housed within a protective casing for portable transport and use. 5 figs.

  16. 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)

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

    Science.gov (United States)

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

    2010-04-01

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

  18. Determination of uranium in samples containing bulk aluminium

    International Nuclear Information System (INIS)

    Das, S.K.; Kannan, R.; Dhami, P.S.; Tripathi, S.C.; Gandhi, P.M.

    2015-01-01

    The determination of uranium is of great importance in PUREX process and need to be analyzed at different concentration ranges depending on the stage of reprocessing. Various techniques like volumetry, spectrophotometry, ICP-OES, fluorimetry, mass spectrometry etc. are used for the measurement of uranium in these samples. Fast and sensitive methods suitable for low level detection of uranium are desirable to cater the process needs. Microgram quantities of uranium are analyzed by spectrophotometric method using 2-(5- bromo-2-pyridylazo-5-diethylaminophenol) (Br-PADAP) as the complexing agent. But, the presence of some of the metal ions viz. Al, Pu, Zr etc. interferes in its analysis. Therefore, separation of uranium from such interfering metal ions is required prior to its analysis. This paper describes the analysis of uranium in samples containing aluminium as major matrix

  19. Fluorescent determination of graphene quantum dots in water samples

    Energy Technology Data Exchange (ETDEWEB)

    Benítez-Martínez, Sandra; Valcárcel, Miguel, E-mail: qa1meobj@uco.es

    2015-10-08

    This work presents a simple, fast and sensitive method for the preconcentration and quantification of graphene quantum dots (GQDs) in aqueous samples. GQDs are considered an object of analysis (analyte) not an analytical tool which is the most frequent situation in Analytical Nanoscience and Nanotechnology. This approach is based on the preconcentration of graphene quantum dots on an anion exchange sorbent by solid phase extraction and their subsequent elution prior fluorimetric analysis of the solution containing graphene quantum dots. Parameters of the extraction procedure such as sample volume, type of solvent, sample pH, sample flow rate and elution conditions were investigated in order to achieve extraction efficiency. The limits of detection and quantification were 7.5 μg L{sup −1} and 25 μg L{sup −1}, respectively. The precision for 200 μg L{sup −1}, expressed as %RSD, was 2.8%. Recoveries percentages between 86.9 and 103.9% were obtained for two different concentration levels. Interferences from other nanoparticles were studied and no significant changes were observed at the concentration levels tested. Consequently, the optimized procedure has great potential to be applied to the determination of graphene quantum dots at trace levels in drinking and environmental waters. - Highlights: • Development of a novel and simple method for determination of graphene quantum dots. • Preconcentration of graphene quantum dots by solid phase extraction. • Fluorescence spectroscopy allows fast measurements. • High sensitivity and great reproducibility are achieved.

  20. Spectrographic determination of impurities in ammonium hydrogen fluoride samples

    International Nuclear Information System (INIS)

    Roca, M.; Capdevila, C.; Alduan, F.A.

    1976-01-01

    The quantitative spectrographic trace determination of Al, B, Cr, Cu, Fe, Mn, Mo, Ni, Pb and Si in ammonium hydrogen fluoride samples is considered. 10 A dc arc excitation and graphite electrodes with crate either 4.5 mm or 8 mm deep are employed. A comparison of various matrices such as graphite, gallium oxide, germanium oxide, magnesium oxide and zinc oxide, in the ratios 1:1 and 1:3, as well as a mixture 50% graphite - 50% zinc oxide in the ratio 1:1 is included. Zinc oxide in the ratio 1:1 and 4x8 mm craters show the best over-all results. (author)

  1. Determination of strontium-90 in the environmental samples at PINSTECH

    International Nuclear Information System (INIS)

    Perveen, N.; Aziz, A.

    1979-01-01

    Strontium-90 a bone seeking radionuclide and a long lived beta emitter is one of the toxic radionuclides detected in the environment arising mainly from the fall out from nuclear detonations. Its concentration in various environmental media such as air, precipitation, surface water, vegetables and other items of diet was measured. This report describes the method of collection, treatment and radiochemical analyses of environmental samples for the determination of Sr-90. The levels of Sr-90 concentration in these media are also recorded. (authors)

  2. Determination of palladium in biological samples applying nuclear analytical techniques

    International Nuclear Information System (INIS)

    Cavalcante, Cassio Q.; Sato, Ivone M.; Salvador, Vera L. R.; Saiki, Mitiko

    2008-01-01

    This study presents Pd determinations in bovine tissue samples containing palladium prepared in the laboratory, and CCQM-P63 automotive catalyst materials of the Proficiency Test, using instrumental thermal and epithermal neutron activation analysis and energy dispersive X-ray fluorescence techniques. Solvent extraction and solid phase extraction procedures were also applied to separate Pd from interfering elements before the irradiation in the nuclear reactor. The results obtained by different techniques were compared against each other to examine sensitivity, precision and accuracy. (author)

  3. Accelerator mass analyses of meteorites - carbon-14 terrestrial ages

    International Nuclear Information System (INIS)

    Miura, Y.; Rucklidge, J.; Beukens, R.; Fireman, E.

    1988-01-01

    Carbon-14 terrestrial ages of ten Antarctic meteorites have been measured by the IsoTrace accelerator mass spectrometry (AMS). The 14 C terrestrial age of 1 gram sample was determined from 14 C concentrations collected at melt and re-melt temperatures, compared with the 14 C concentration of the known Bruderheim chondrite. Yamato-790448 (LL3) chondrite was found to be the oldest terrestrial age of 3x10 4 years in the nine Yamato chondrites, whereas Yamato-791630 (L4) chondrite is considered to be the youngest chondrites less than thousand years. Allan Hills chondrite of ALH-77231 (L6) shows older terrestrial age than the nine Yamato chondrites. New accelerator data of the terrestrial age show higher accuracy with smaller sample than the previous counting method. (author)

  4. Determination of sampling constants for selenium by cyclic INAA

    International Nuclear Information System (INIS)

    Chatt, A.; Jayawickreme, C.K.

    1988-01-01

    Biological reference materials of natural origin and certified elemental composition play an important role in not only evaluating the reliability of a new method but also assuring the quality of data produced in routine analysis. In fact, it has become a common practice to include an appropriate certified reference material (CRM) in every batch of samples analyzed for the purpose of quality assurance. One of the most important properties of a CRM or reference material (RM) should be its degree of homogeneity. For biological materials, inhomogeneity is inherently associated with their intricate structures. In order to justify the usage of a CRM or RM at a mass lower than that recommended by the issuing agency, is necessary to evaluate the homogeneity at lower mass ranges and to determine the sampling constant for the element of interest. The objectives of the present work are to investigate the homogeneity and to calculate the sampling constants for selenium in several biological CRM and RM that are frequently used to evaluate the accuracy of measurements

  5. Analytical methodologies for the determination of benzodiazepines in biological samples.

    Science.gov (United States)

    Persona, Karolina; Madej, Katarzyna; Knihnicki, Paweł; Piekoszewski, Wojciech

    2015-09-10

    Benzodiazepine drugs belong to important and most widely used medicaments. They demonstrate such therapeutic properties as anxiolytic, sedative, somnifacient, anticonvulsant, diastolic and muscle relaxant effects. However, despite the fact that benzodiazepines possess high therapeutic index and are considered to be relatively safe, their use can be dangerous when: (1) co-administered with alcohol, (2) co-administered with other medicaments like sedatives, antidepressants, neuroleptics or morphine like substances, (3) driving under their influence, (4) using benzodiazepines non-therapeutically as drugs of abuse or in drug-facilitated crimes. For these reasons benzodiazepines are still studied and determined in a variety of biological materials. In this article, sample preparation techniques which have been applied in analysis of benzodiazepine drugs in biological samples have been reviewed and presented. The next part of the article is focused on a review of analytical methods which have been employed for pharmacological, toxicological or forensic study of this group of drugs in the biological matrices. The review was preceded by a description of the physicochemical properties of the selected benzodiazepines and two, very often coexisting in the same analyzed samples, sedative-hypnotic drugs. Copyright © 2015. Published by Elsevier B.V.

  6. Micellar electrokinetic chromatographic determination of triazine herbicides in water samples.

    Science.gov (United States)

    Li, Zhi; Zhang, Shuaihua; Yin, Xiaofang; Wang, Chun; Wang, Zhi

    2014-09-01

    Dispersive liquid-liquid microextraction combined with online sweeping preconcentration in micellar electrokinetic chromatography was developed for the simultaneous determination of five triazine herbicides (atrazine, simazine, propazine, prometon and simetryn) in water samples. Several experimental parameters affecting the extraction efficiencies such as the type and volume of both the extraction and dispersive solvents, the addition of salt to sample solution, the extraction time and the pH of the sample solution were investigated. Under optimum conditions, the linearity of the method was good in the range from 0.33 to 20 ng mL(-1) for simazine, propazine, atrazine and simetryn, and from 0.17 to 20 ng mL(-1) for prometon, respectively. The sensitivity enrichment factors were in the range from 1750 to 2100, depending on the compound. The limit of detection (S/N = 3) ranged from 0.05 to 0.10 ng mL(-1). The developed method was successfully applied to the analysis of the five triazines in river, ground and well waters. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  7. Quantitative determination of 210Po in geochemical samples

    International Nuclear Information System (INIS)

    Dyck, W.; Bristow, Q.

    1984-01-01

    To test the usefulness of 210 Po in soils as a means of detecting buried U mineralization, methods for the determination of 210 Po were investigated and adapted for routine production of 210 Po data from geochemical samples. A number of conditions affecting autodeposition and detection of 210 Po were investigated. The optimum area of deposition with a 450 mm 2 solid state detector was found to be 300 mm 2 . Convenience dictated room temperature over-night deposition times, although increased temperature increased speed and efficiency of deposition. A clear inverse relationship was observed between volume of solution and deposition efficiency with stirring times of less than 2 hours. For routine analysis, soil and rock powders were dissolved by leaching 1 g samples in teflon beakers successively with conc. HNO 3 , HF, and HNO 3 -HClO 4 , evaporating the solution to dryness between leaches, and taking the residue up in 20 mL 0.5 M HCl. The 210 Po was deposited on 19 mm diameter Ni discs and counted with an alpha spectrometer system employing 450 mm 2 ruggedized surface barrier detectors. The method achieved 90 percent recovery of 210 Po from solution and a detection efficiency of 30 percent. With a counting time of 3 hours, the method is capable of detecting 0.2 pCi of 210 Po per gram of sample

  8. Sequential determination of important ecotoxic radionuclides in nuclear waste samples

    International Nuclear Information System (INIS)

    Bilohuscin, J.

    2016-01-01

    In the dissertation thesis we focused on the development and optimization of a sequential determination method for radionuclides 93 Zr, 94 Nb, 99 Tc and 126 Sn, employing extraction chromatography sorbents TEVA (R) Resin and Anion Exchange Resin, supplied by Eichrom Industries. Prior to the attestation of sequential separation of these proposed radionuclides from radioactive waste samples, a unique sequential procedure of 90 Sr, 239 Pu, 241 Am separation from urine matrices was tried, using molecular recognition sorbents of AnaLig (R) series and extraction chromatography sorbent DGA (R) Resin. On these experiments, four various sorbents were continually used for separation, including PreFilter Resin sorbent, which removes interfering organic materials present in raw urine. After the acquisition of positive results of this sequential procedure followed experiments with a 126 Sn separation using TEVA (R) Resin and Anion Exchange Resin sorbents. Radiochemical recoveries obtained from samples of radioactive evaporate concentrates and sludge showed high efficiency of the separation, while values of 126 Sn were under the minimum detectable activities MDA. Activity of 126 Sn was determined after ingrowth of daughter nuclide 126m Sb on HPGe gamma detector, with minimal contamination of gamma interfering radionuclides with decontamination factors (D f ) higher then 1400 for 60 Co and 47000 for 137 Cs. Based on the acquired experiments and results of these separation procedures, a complex method of sequential separation of 93 Zr, 94 Nb, 99 Tc and 126 Sn was proposed, which included optimization steps similar to those used in previous parts of the dissertation work. Application of the sequential separation method for sorbents TEVA (R) Resin and Anion Exchange Resin on real samples of radioactive wastes provided satisfactory results and an economical, time sparing, efficient method. (author)

  9. A procedure for the determination of Po-210 in water samples by alpha spectrometry

    International Nuclear Information System (INIS)

    2009-01-01

    Reliable, comparable and 'fit for purpose' results are an essential requirement for any decision based on analytical measurements. For the analyst, the availability of tested and validated analytical procedures is a extremely important tool for production of such analytical measurements. For maximum utility, such procedures should be comprehensive, clearly formulated, and readily available to both the analyst and the customer for reference. Since 2004 the Environment programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. In the case of 210 Po, this started with the collection and review of about 130 papers from the scientific literature. Based on this review, two candidate methods for the chemical separation of 210 Po from water samples were selected for testing, refinement and validation in accordance with ISO guidelines. A comprehensive methodology for calculation of results including quantification of measurement uncertainty was also developed. This report presents the final procedure which was developed based on that work

  10. Determination of technetium-99 in environmental and radioactive waste samples

    International Nuclear Information System (INIS)

    Ferencova, M.; Peter Tkac, P.

    2007-01-01

    Technetium is known for its high mobility in a soil-water system in non-reducing aerobic condition and also high bio-availability for plants, because the most stable form of technetium in natural surface environment is pertechnetate which is highly soluble. The chemical form of technetium changes with environmental conditions. Concentration of technetium in the environment is very low, therefore many separation steps are needed for technetium determination. It has been developed a method for the routine determination of technetium-99 from environmental matrices and radioactive wastes using technetium-99m as an internal yield monitor. Technetium-99 is extracted from the soil samples with nitric acid. Many contaminants are co-precipitated with ferric hydroxide and technetium in the supernatant is pre-concentrated and further purified using anion exchange chromatography. Final separation of technetium was achieved by extraction with tetraphenylarsonium chloride in chloroform from sulphuric acid or pure water. The chemical yield is determined through the measurement of technetium-99m by scintillation counting system and the technetium-99 activity is measured using proportional counter after decay of the technetium-99m activity. Typical recoveries for this method are in the order 50-60 % (authors)

  11. Seed germination from lowland tapir (Tapirus terrestris) fecal samples collected during the dry season in the Northern Brazilian Amazon.

    Science.gov (United States)

    Barcelos, Adriana Renata; Bobrowiec, Paulo Estefano D; Sanaiotti, Tânia Margarete; Gribel, Rogério

    2013-03-01

    This study evaluated the potential of lowland tapirs as seed dispersers in the northern Brazilian Amazon. The study analyzed the viability of seeds after passage through the gut. Fecal samples were collected from 6 different vegetation physiognomies in Viruá National Park during the dry season. The samples were then kept in a greenhouse for 16 months to allow the seeds to germinate. The seedling species were identified and classified according to the type of fruit, plant habit, seed size and type of ingestion. Of the 111 fecal samples, 94 (84.7%) had viable seeds of 75 species. Melastomataceae was the most frequent family with viable seeds in the fecal samples (69.1% of samples, N= 18 species). The data suggest that the importance of the lowland tapirs as dispersers is not restricted to the species consumed actively by frugivory but also extends to species accidentally consumed during browsing. The occurrence of both large and small viable seeds in the fecal samples as well as a number of large drupes, which probably cannot be transported via endozoochory by any other animal species, provide evidence of the ecological importance of lowland tapirs to the dynamics of the forest-campinarana vegetation mosaic in the region. © 2012 Wiley Publishing Asia Pty Ltd, ISZS and IOZ/CAS.

  12. Determination of natural radionuclides in lichen samples of Carnoparmelia Texana

    International Nuclear Information System (INIS)

    Alencar, Marcos M.; Damatto, Sandra R.; Mazzilli, Barbara P.

    2009-01-01

    Lichen plays an important role in studies of environmental pollution. It can be used for the evaluation of air contaminants, including heavy metals and radionuclides. The main objective of this study is to verify the possibility of using the lichen species Canoparmelia Texana for the assessment of natural radionuclides of the U and Th decay series in air in the vicinity of Instituto de Pesquisas Energeticas e Nucleares (IPEN) installations. IPEN has as major activity to perform research in the field of the nuclear fuel cycle, and therefore deals with natural radionuclides of the U and Th series. The content of 238 U, 234 U, 230 Th, 210 Po and 232 Th in lichen samples were determined by alpha spectrometry after a radiochemical separation. Ra isotopes and 210 Pb were determined by gross alpha and beta counting after a radiochemical separation and measurement on a low background gas flow proportional detector. The results obtained for 238 U varied from 2.4 ± 0.4 Bq kg -1 to 6.6 ± 0.1 Bq kg -1 and from 4.4 ± 0.3 Bq kg -1 to 12.1 ± 2.6 Bq kg -1 , for 232 Th. For 226 Ra varied from 13 ± 1 Bq kg -1 to 38 ± 2 Bq kg -1 and from 200 ± 13 Bq kg -1 to 351 ± 12 Bqkg -1 for 228 Ra. The results obtained were compared with data obtained for the same radionuclides in lichen samples in an area affected by TENORM industry and can be considered as background for this lichen species. It can be concluded that the control of atmospheric discharges of IPEN facilities has been effective along the years, giving no evidence of radiological environmental impact. (author)

  13. Determination of trihalomethanes in water samples: A review

    Energy Technology Data Exchange (ETDEWEB)

    Perez Pavon, Jose Luis [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Universidad de Salamanca, 37008 Salamanca (Spain)], E-mail: jlpp@usal.es; Herrero Martin, Sara; Garcia Pinto, Carmelo; Moreno Cordero, Bernardo [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Universidad de Salamanca, 37008 Salamanca (Spain)

    2008-11-23

    This article reviews the most recent literature addressing the analytical methods applied for trihalomethanes (THMs) determination in water samples. This analysis is usually performed with gas chromatography (GC) combined with a preconcentration step. The detectors most widely used in this type of analyses are mass spectrometers (MS) and electron capture detectors (ECD). Here, we review the analytical characteristics, the time required for analysis, and the simplicity of the optimised methods. The main difference between these methods lies in the sample pretreatment step; therefore, special emphasis is placed on this aspect. The techniques covered are direct aqueous injection (DAI), liquid-liquid extraction (LLE), headspace (HS), and membrane-based techniques. We also review the main chromatographic columns employed and consider novel aspects of chromatographic analysis, such as the use of fast gas chromatography (FGC). Concerning the detection step, besides the common techniques, the use of uncommon detectors such as fluorescence detector, pulsed discharge photoionization detector (PDPID), dry electrolytic conductivity detector (DELCD), atomic emission detector (AED) and inductively coupled plasma-mass spectrometry (ICP-MS) for this type of analysis is described.

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

    International Nuclear Information System (INIS)

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

    1998-01-01

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

  15. How Do Terrestrial Determinants Impact the Response of Water Quality to Climate Drivers?—An Elasticity Perspective on the Water–Land–Climate Nexus

    Directory of Open Access Journals (Sweden)

    Afed U. Khan

    2017-11-01

    Full Text Available Investigating water–land–climate interactions is critical for urban development and watershed management. This study examined this nexus by elasticity and statistical approaches through the lens of three watersheds: The Yukon, Mekong and Murray. Here, this study reports the fundamental characteristics, explanations and ecological and management implications of terrestrial determinant influence on the response of water quality to climate drivers. The stability of the response, measured by climate elasticity of water quality (CEWQ, is highly dependent on terrestrial determinants, with strong impacts from anthropogenic biomes and low impacts from surficial geology. Compared to temperature elasticity, precipitation elasticity of water quality is more unstable due to its possible linkages with many terrestrial determinants. Correlation and linear models were developed for the interaction system, which uncovered many interesting scenarios. The results implied that watersheds with a higher ratio of rangeland biomes have a lower risk of instability as compared to watersheds with a higher proportion of dense settlement, cropland and forested biomes. This study discusses some of the most essential pathways where instability might adversely affect CEWQ parameters and recommends suggestions for policy makers to alleviate the instability impacts to bring sustainability to the water environment.

  16. Determination of the fraction of amorphous phases in superconducting samples

    International Nuclear Information System (INIS)

    Gomes Junior, G.G.; Ogasawara, T.; Amorim, H.S.

    2010-01-01

    The study phase formation of high critical temperature superconducting (Bi, Pb) - 2223 by partial melting and recrystallization aims to improve the microstructure of the material. Was used for X-ray diffraction characterization of the phases present. The DDM method (Derivative Difference Minimization) was used for the refinement of structures, quantification of the phases and determination the fraction of this amorphous. The advantage this method is not necessary to introduce an internal standard to determine the amorphous fraction. Were observed in the powder precursor phases (Bi, Pb) 2 Sr 2 Ca 2 Cu 3 O x (Bi, Pb) -2223, 93% of the sample, Bi 2 Sr 2 CaCu 2 O y (Bi-2212) and Bi 2 Sr 2 CuO z (Bi-2201). The powder precursor was heat treated at 820-870 deg C. To minimize volatilization of lead, the material was placed in silver crucibles closed. To get a high recovery of (Bi, Pb) - 2223, the material was cooled slowly, due to slow kinetic of formation of this phase. We observed a partial recovery phase (Bi, Pb) -2223. (author)

  17. Probabilistic determination of the ecological risk from OTNE in aquatic and terrestrial compartments based on US-wide monitoring data.

    Science.gov (United States)

    McDonough, Kathleen; Casteel, Kenneth; Zoller, Ann; Wehmeyer, Kenneth; Hulzebos, Etje; Rila, Jean-Paul; Salvito, Daniel; Federle, Thomas

    2017-01-01

    OTNE [1-(1,2,3,4,5,6,7,8-octahydro-2,3,8,8-tetramethyl-2-naphthyl)ethan-1-one; trade name Iso E Super] is a fragrance ingredient commonly used in consumer products which are disposed down the drain. This research measured effluent and sludge concentrations of OTNE at 44 US wastewater treatment plants (WWTP). The mean effluent and sludge concentrations were 0.69 ± 0.65 μg/L and 20.6 ± 33.8 mg/kg dw respectively. Distribution of OTNE effluent concentrations and dilution factors were used to predict surface water and sediment concentrations and distributions of OTNE sludge concentrations and loading rates were used to predict terrestrial concentrations. The 90th percentile concentration of OTNE in US WWTP mixing zones was predicted to be 0.04 and 0.85 μg/L under mean and 7Q10 low flow (lowest river flow occurring over a 7 day period every 10 years) conditions respectively. The 90th percentile sediment concentrations under mean and 7Q10 low flow conditions were predicted to be 0.081 and 1.6 mg/kg dw respectively. Based on current US sludge application practices, the 90th percentile OTNE terrestrial concentration was 1.38 mg/kg dw. The probability of OTNE concentrations being below the predicted no effect concentration (PNEC) for the aquatic and sediment compartments was greater than 99%. For the terrestrial compartment, the probability of OTNE concentrations being lower than the PNEC was 97% for current US sludge application practices. Based on the results of this study, OTNE concentrations in US WWTP effluent and sludge do not pose an ecological risk to aquatic, sediment and terrestrial organisms. Copyright © 2016 Elsevier Ltd. All rights reserved.

  18. 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.

  19. Terrestrial gamma radiation dose study to determine the baseline for environmental radiological health practices in Melaka state, Malaysia

    International Nuclear Information System (INIS)

    Ramli, Ahmad Termizi; Sahrone, Sallehudin; Wagiran, Husin

    2005-01-01

    Environmental terrestrial gamma radiation dose rates were measured throughout Melaka, Malaysia, over a period of two years, with the objective of establishing baseline data on the background radiation level. Results obtained are shown in tabular, graphic and cartographic form. The values of terrestrial gamma radiation dose rate vary significantly over different soil types and for different underlying geological characteristics present in the study area. The values ranged from 54 ± 5 to 378 ± 38 nGy h -1 . The highest terrestrial gamma dose rates were measured over soil types of granitic origin and in areas with underlying geological characteristics of an acid intrusive (undifferentiated) type. An isodose map of terrestrial gamma dose rate in Melaka was drawn by using the GIS application 'Arc View'. This was based on data collected using a NaI(Tl) scintillation detector survey meter. The measurements were taken at 542 locations. Three small 'hot spots' were found where the dose rates were more than 350 nGy h -1 . The mean dose rates in the main population areas in the mukims (parishes) of Bukit Katil, Sungai Udang, Batu Berendam, Bukit Baru and Bandar Melaka were 154 ± 15, 161 ± 16, 160 ± 16, 175 ± 18 and 176 ± 18 nGy h -1 , respectively. The population-weighted mean dose rate throughout Melaka state is 172 ± 17 nGy h -1 . This is lower than the geographical mean dose rate of 183 ± 54 nGy h -1 . The lower value arises from the fact that most of the population lives in the central area of the state where the lithology is dominated by sedimentary rocks consisting of shale, mudstone, phyllite, slate, hornfels, sandstone and schist of Devonian origin which have lower associated dose rates. The mean annual effective dose to the population from outdoor terrestrial gamma radiation was estimated to be 0.21 mSv. This value is higher than the world average of 0.07 mSv

  20. Export of Terrestrially-Derived Organic Matter from the Mississippi River to the Gulf of Mexico Sediments as Determined by Ultrahigh Resolution Mass Spectrometry

    Science.gov (United States)

    Hatcher, P.; Ware, S. A.; Vaughn, D.; Waggoner, D. C.; Bianchi, T. S.

    2017-12-01

    Sediment samples extending from the main channel of the Mississippi River to edge of the continental shelf of the Gulf of Mexico were extracted to recover humic acids from the organic matter and subjected to molecular level characterization by electrospray ionization coupled to Fourier transform ion cyclotron resonance mass spectrometry (ESI-FTICR-MS). The data show that sedimentary organic matter at the river mouth contains humic substances with a predominantly terrestrial signature resembling those obtained from soils. Condensed aromatic molecules and carboxyl rich alicyclic molecules (CRAM) typify the major structures observed. The CRAM-like molecules persist progressing seaward into the Gulf while the condensed aromatic molecules diminish in relative abundance. This trend is characteristic of traditional mixing of allochthonous terrestrial with autochthonous source materials, consistent with published isotope and lignin phenol biomarker data. Alternatively, the trend could also be explained by oxidative degradation of mainly terrestrial organic matter whereby the condensed aromatic molecules would be selectively oxidized. CRAM molecules would then become selectively enriched as one progresses from the channel to the continental shelf. Laboratory studies show that aromatic molecules (like those in lignin) subjected to oxidative degradation mainly by hydroxyl radical attack, either biologically or non-biologically, undergo molecular rearrangement via ring-opening to form reactive species. These can interact with nucleophilic molecules such as peptides and sulfur-containing species and/or can undergo cycloaddition reactions to produce CRAM-like species. This latter explanation suggests that the main source of organic matter in this coastal depocenter is terrestrial and that autochthonous organic matter contributes little to sedimentary organic matter.

  1. Observing the continental-scale carbon balance: assessment of sampling complementarity and redundancy in a terrestrial assimilation system by means of quantitative network design

    OpenAIRE

    Kaminski, T.; Rayner, P. J.; Vossbeck, M.; Scholze, M.; Koffi, E.

    2012-01-01

    This paper investigates the relationship between the heterogeneity of the terrestrial carbon cycle and the optimal design of observing networks to constrain it. We combine the methods of quantitative network design and carbon-cycle data assimilation to a hierarchy of increasingly heterogeneous descriptions of the European terrestrial biosphere as indicated by increasing diversity of plant functional types. We employ three types of observat...

  2. Sampling procedure, receipt and conservation of water samples to determine environmental radioactivity

    International Nuclear Information System (INIS)

    Herranz, M.; Navarro, E.; Payeras, J.

    2009-01-01

    The present document informs about essential goals, processes and contents that the subgroups Sampling and Samples Preparation and Conservation believe they should be part of the procedure to obtain a correct sampling, receipt, conservation and preparation of samples of continental, marine and waste water before qualifying its radioactive content.

  3. Approximate determination of efficiency for activity measurements of cylindrical samples

    Energy Technology Data Exchange (ETDEWEB)

    Helbig, W [Nuclear Engineering and Analytics Rossendorf, Inc. (VKTA), Dresden (Germany); Bothe, M [Nuclear Engineering and Analytics Rossendorf, Inc. (VKTA), Dresden (Germany)

    1997-03-01

    Some calibration samples are necessary with the same geometrical parameters but of different materials, containing known activities A homogeniously distributed. Their densities are measured, their mass absorption coefficients may be unknown. These calibration samples are positioned in the counting geometry, for instance directly on the detector. The efficiency function {epsilon}(E) for each sample is gained by measuring the gamma spectra and evaluating all usable gamma energy peaks. From these {epsilon}(E) the common valid {epsilon}{sub geom}(E) will be deduced. For this purpose the functions {epsilon}{sub mu}(E) for these samples have to be established. (orig.)

  4. The determination of radionuclides in grass ecosystem samples

    International Nuclear Information System (INIS)

    LaBrecque, J.J.; Schelenz, R.; Perkins, R.W.

    1987-07-01

    The radioactive debris cloud from the Chernobyl reactor accident resulted in some deposition over essentially all of the Northern Hemisphere. Shortly after the accident invitations were sent out by the IAEA to Member States to collect grass samples according to specific instructions so that the ratio of the various radionuclides in the fallout debris could be established over a wide area of Europe. In response to this request, 20 grass samples were provided by Member States. To establish a protocol for analysis of these valuable samples and to recommend a protocol for future sample collection, a Consultants Meeting was called by the IAEA for 23-25 September 1986. This document contains the considerations and recommendations of the consultants

  5. Hydrazine Determination in Sludge Samples by High Performance Liquid Chromatography

    Energy Technology Data Exchange (ETDEWEB)

    G. Elias; G. A. Park

    2006-02-01

    A high-performance liquid chromatographic method using ultraviolet (UV) detection was developed to detect and quantify hydrazine in a variety of environmental matrices. The method was developed primarily for sludge samples, but it is also applicable to soil and water samples. The hydrazine in the matrices was derivatized to their hydrazones with benzaldehyde. The derivatized hydrazones were separated using high performance liquid chromatography (HPLC) with a reversed-phase C-18 column in an isocratic mode with methanol-water (95:5, v/v), and detected with UV detection at 313 nm. The detection limit (25 ml) for the new analytical method is 0.0067 mg ml-1of hydrazine. Hydrazine showed low recovery in soil samples because components in soil oxidized hydrazine. Sludge samples that contained relatively high soil content also showed lower recovery. The technique is relatively simple and cost-effective, and is applicable for hydrazine analysis in different environmental matrices.

  6. 7 CFR 28.25 - Samples for Form A determination.

    Science.gov (United States)

    2010-01-01

    ... shall be at least six (6) inches wide and approximately twelve (12) inches long and shall weigh at least..., trimming, or discarding part of the sample is prohibited. No part of the cotton or pieces of bagging, leaf...

  7. An integrated approach for multi-level sample size determination

    International Nuclear Information System (INIS)

    Lu, M.S.; Teichmann, T.; Sanborn, J.B.

    1997-01-01

    Inspection procedures involving the sampling of items in a population often require steps of increasingly sensitive measurements, with correspondingly smaller sample sizes; these are referred to as multilevel sampling schemes. In the case of nuclear safeguards inspections verifying that there has been no diversion of Special Nuclear Material (SNM), these procedures have been examined often and increasingly complex algorithms have been developed to implement them. The aim in this paper is to provide an integrated approach, and, in so doing, to describe a systematic, consistent method that proceeds logically from level to level with increasing accuracy. The authors emphasize that the methods discussed are generally consistent with those presented in the references mentioned, and yield comparable results when the error models are the same. However, because of its systematic, integrated approach the proposed method elucidates the conceptual understanding of what goes on, and, in many cases, simplifies the calculations. In nuclear safeguards inspections, an important aspect of verifying nuclear items to detect any possible diversion of nuclear fissile materials is the sampling of such items at various levels of sensitivity. The first step usually is sampling by ''attributes'' involving measurements of relatively low accuracy, followed by further levels of sampling involving greater accuracy. This process is discussed in some detail in the references given; also, the nomenclature is described. Here, the authors outline a coordinated step-by-step procedure for achieving such multilevel sampling, and they develop the relationships between the accuracy of measurement and the sample size required at each stage, i.e., at the various levels. The logic of the underlying procedures is carefully elucidated; the calculations involved and their implications, are clearly described, and the process is put in a form that allows systematic generalization

  8. Evaluation of Gravimetric Tar Determination in Particle Samples

    DEFF Research Database (Denmark)

    Hindsgaul, Claus; Henriksen, Ulrik B.; Bentzen, Jens Dall

    2000-01-01

    A comparison of tar determination of particles from a down-draft gasifier using soxhlet extractions (with anisole, dichloromethane and acetone) and pyrolysis of the particles.......A comparison of tar determination of particles from a down-draft gasifier using soxhlet extractions (with anisole, dichloromethane and acetone) and pyrolysis of the particles....

  9. Neutron cross-section determination in geological samples (U)

    International Nuclear Information System (INIS)

    Harris, J.M.; McDaniel, P.J.

    1982-01-01

    The Prompt Gamma Neutron Activation Analysis (PGAA) technique yields elemental composition data which can be used to calculate the macroscopic cross section for any sample. The Small Sample Reactivity Measurements (SSRM) technique yields the macroscopic thermal absorption directly. Experimentally, PGAA is somewhat more difficult because of the calibration and data handling than is SSRM. However, SSRM requires a mathematical model of the reactor which means a rather complicated analysis. Once the model and calibration are completed, data analysis is routine. The SSRM technique is production oriented. 9 figures

  10. On Using a Pilot Sample Variance for Sample Size Determination in the Detection of Differences between Two Means: Power Consideration

    Science.gov (United States)

    Shieh, Gwowen

    2013-01-01

    The a priori determination of a proper sample size necessary to achieve some specified power is an important problem encountered frequently in practical studies. To establish the needed sample size for a two-sample "t" test, researchers may conduct the power analysis by specifying scientifically important values as the underlying population means…

  11. Contaminant exposure in terrestrial vertebrates

    International Nuclear Information System (INIS)

    Smith, Philip N.; Cobb, George P.; Godard-Codding, Celine; Hoff, Dale; McMurry, Scott T.; Rainwater, Thomas R.; Reynolds, Kevin D.

    2007-01-01

    Here we review mechanisms and factors influencing contaminant exposure among terrestrial vertebrate wildlife. There exists a complex mixture of biotic and abiotic factors that dictate potential for contaminant exposure among terrestrial and semi-terrestrial vertebrates. Chemical fate and transport in the environment determine contaminant bioaccessibility. Species-specific natural history characteristics and behavioral traits then play significant roles in the likelihood that exposure pathways, from source to receptor, are complete. Detailed knowledge of natural history traits of receptors considered in conjunction with the knowledge of contaminant behavior and distribution on a site are critical when assessing and quantifying exposure. We review limitations in our understanding of elements of exposure and the unique aspects of exposure associated with terrestrial and semi-terrestrial taxa. We provide insight on taxa-specific traits that contribute, or limit exposure to, transport phenomenon that influence exposure throughout terrestrial systems, novel contaminants, bioavailability, exposure data analysis, and uncertainty associated with exposure in wildlife risk assessments. Lastly, we identify areas related to exposure among terrestrial and semi-terrestrial organisms that warrant additional research. - Both biotic and abiotic factors determine chemical exposure for terrestrial vertebrates

  12. Determination of toxic trace elements in body fluid reference samples

    International Nuclear Information System (INIS)

    Gills, T.E.; McClendon, L.T.; Maienthal, E.J.; Becker, D.A.; Durst, R.A.; LaFleur, P.D.

    1974-01-01

    The measurement of elemental concentration in body fluids has been widely used to give indication of exposures to certain toxic materials and/or a measure of body burden. To understand fully the toxicological effect of these trace elements on our physiological system, meaningful analytical data are required along with accurate standards or reference samples. The National Bureau of Standards has prepared for the National Institute for Occupational Safety and Health (NIOSH) a number of reference samples containing selected toxic trace elements in body fluids. The reference samples produced include mercury in urine at three concentration levels, five elements (Se, Cu, As, Ni and Cr) in freeze-dried urine at two levels, fluorine in freeze-dried urine at two levels and lead in blood at two concentration levels. These reference samples have been found to be extremely useful for the evaluation of field and laboratory analytical methods for the analysis of toxic trace elements. In particular the use of at least two calibration points (i.e., ''normal'' and ''elevated'' levels) for a given matrix provides a more positive calibration for most analytical techniques over the range of interest for occupational toxicological levels of exposure. (U.S.)

  13. Determination of Phenols in Water Samples using a Supported ...

    African Journals Online (AJOL)

    NJD

    This was achieved by pH adjustments in the sample and acceptor phases. The method was ... during wastewater treatment, since chlorine is added as a disinfectant. ... they give a high degree of selectivity and clean-up, use little or no organic ...

  14. Terrestrial magnetosphere

    International Nuclear Information System (INIS)

    Pande, D.C.; Agarwal, D.C.

    1982-01-01

    This paper presents a review about terrestrial magnetosphere. During the last few years considerable investigation have been carried out about the properties of Solar Wind and its interaction with planetary magnetic fields. It is therefore of high importance to accumulate all the investigations in a comprehensive form. The paper reviews the property of earth's magnetosphere, magnetosheath, magneto pause, polar cusps, bow shook and plasma sheath. (author)

  15. Determination of Rn222 in samples of well water and domicile of the cities of Chihuahua and Aldama, Mexico

    International Nuclear Information System (INIS)

    Villalba, L.; Colmenero S, L.; Montero C, M.E.

    2004-01-01

    The study of the content of dissolved Rn 222 is presented in underground water and of domicile of the cities of Chihuahua and Aldama of the State of Chihuahua. The existence of the Rn 222 in the underground waters comes from its constant production in the rocks of the terrestrial bark. It has been determined that the radon is a noble gas of more solubility in the water, this solubility induces high concentrations in underground water, as well as bigger risk to the health in the human body once ingested or inhaled. Of the 32 wells studied in the cities of Chihuahua and Aldama, the content of dissolved Rn 222 in the water of 22 of them is bigger than 11 Bq/l and of 73 studied samples of water of domiciles 47 show bigger values that 11 Bq/l. These radon contents are attributable to the uraniferous rocks present in the aquifers. (Author)

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

    International Nuclear Information System (INIS)

    2014-01-01

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

  17. A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry.

    Science.gov (United States)

    Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S; Korn, Maria G A; Bezerra, Marcos A

    2009-03-15

    A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L(-1) nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 microg L(-1), respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 microg L(-1). The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.

  18. A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Tuzen, Mustafa; Soylak, Mustafa; Citak, Demirhan; Ferreira, Hadla S.; Korn, Maria G.A.; Bezerra, Marcos A.

    2009-01-01

    A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L -1 nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 μg L -1 , respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 μg L -1 . The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish

  19. A preconcentration system for determination of copper and nickel in water and food samples employing flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Tuzen, Mustafa [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Soylak, Mustafa [Department of Chemistry, Erciyes University, 38039 Kayseri (Turkey)], E-mail: soylak@erciyes.edu.tr; Citak, Demirhan [Department of Chemistry, Gaziosmanpasa University, 60250 Tokat (Turkey); Ferreira, Hadla S.; Korn, Maria G.A. [Universidade Federal da Bahia, Instituto de Quimica, 40170-290 Salvador (Brazil); Bezerra, Marcos A. [Universidade Estadual do Sudoeste da Bahia, 45200-190 Jequie (Brazil)

    2009-03-15

    A separation/preconcentration procedure using solid phase extraction has been proposed for the flame atomic absorption spectrometric determination of copper and nickel at trace level in food samples. The solid phase is Dowex Optipore SD-2 resin contained on a minicolumn, where analyte ions are sorbed as 5-methyl-4-(2-thiazolylazo) resorcinol chelates. After elution using 1 mol L{sup -1} nitric acid solution, the analytes are determinate employing flame atomic absorption spectrometry. The optimization step was performed using a full two-level factorial design and the variables studied were: pH, reagent concentration (RC) and amount of resin on the column (AR). Under the experimental conditions established in the optimization step, the procedure allows the determination of copper and nickel with limit of detection of 1.03 and 1.90 {mu}g L{sup -1}, respectively and precision of 7 and 8%, for concentrations of copper and nickel of 200 {mu}g L{sup -1}. The effect of matrix ions was also evaluated. The accuracy was confirmed by analyzing of the followings certified reference materials: NIST SRM 1515 Apple leaves and GBW 07603 Aquatic and Terrestrial Biological Products. The developed method was successfully applied for the determination of copper and nickel in real samples including human hair, chicken meat, black tea and canned fish.

  20. Trace determination of uranium in fertilizer samples by total ...

    Indian Academy of Sciences (India)

    Uranium is reported to be present in phosphate fertilizers. The recovery of uranium from the fertilizers is important because it can be used as fuel in nuclear reactors and also because of environmental concerns. For both these activities suitable method of uranium determinations at trace levels in these fertilizers are required.

  1. The determination of plutonium isotopes in environmental samples

    International Nuclear Information System (INIS)

    Siripirom, Lopchai.

    1983-01-01

    The concentration of plutonium in environmental samples such as soil, water, and surface air in the middle part of Thailand were studied. The surface air were collected only at the fifth floor of the Office of Atomic Energy for Peace (OAEP). Plutonium-242 was used as a tracer. Soil and air samples were dissolved by pyrosulphate fusion, and plutonium was co-precipitated with barium sulfate. Then dissolved the precipitate in perchloric acid. Plutonium was extracted out by using solvent bis-(2-ethylhexyl) phosphoric acid (HDEHP). Plutonium in water samples were coprecipitated with iron (III) hydroxide and were dissolved in 8 M. nitric acid. Then the plutonium was separated out by using anion exchange resin, Dowex 1x4. After the solvent extraction or the anion exchange, plutonium was coprecipitated with cerous hydroxide. The activities of plutonium were measured by a surface barrier detector for about 24 hours. Lower limit of detection for 1,440 minutes is 0.012 pCi. These studies showed that only plutonium-239, 240 was observed. The range of activities of plutonium-239, 240 in soil were 0.002-0.157 pCi/g (dry), in water were 0.1-81 f Ci/l, and in air were 7-330 a Ci/m 3 . However, the plutonium concentrations in these studies are far below the maximum permissible concentration (MPC) recommended by International Commission on Radiological Protection (ICRP) for general population which is equal to 3x10 8 f Ci/l of water and 5x10 6 a Ci/m 3 of air

  2. Determination of Cs-134 and Cs-137 rain water samples

    International Nuclear Information System (INIS)

    Lima, M.F.; Mazzilli, B.

    1988-01-01

    In order to setting an environmental monitoring program at IPEN, was developed a fast and simple methodology for concentration of Cs-134 and Cs-137 in rain water. This procedure consists in the precipitation of cesium and others cathions of its family (NH 4 + , K + and Rb + ) by ammonium molybdophosphate. The measures of the desintegration rates of Cs-134 and Cs-137 was done by gamma spectrometry in a Ge(Li) detector. After setting up the ideal experimental conditions, the procedure was used to analyze four samples of rain water. (author) [pt

  3. Spectrophotometric determination of vanadium in environmental and biological samples

    International Nuclear Information System (INIS)

    Rekha, D.; Krishnapriya, B.; Subrahmanyam, P.; Reddyprasad, P.; Dilip Kumar, J.; Chiranjeevi, P.

    2007-01-01

    The method is based on oxidation of p-nitro aniline by vanadium (V) followed by coupling reaction with N-(1-naphthalene-1-y1)ethane-1, 2-diaminedihydrochloride (NEDA) in basic medium of pH 8 to give purple colored derivative. The derivative having an λ max 525nm is stable for 10 days. Beer's law is obeyed for vanadium (V) in the concentration range of 0.03-4.5 μg ml -1 . The proposed method was successfully applied to the analysis of vanadium in environmental and biological samples. (author)

  4. Samplings of airborne particulates for granulometric determinations following Chernobyl accident

    International Nuclear Information System (INIS)

    Tarroni, G.; Calamosca, M.; Zaiacomo, T. de; Gragnani, R.; Michetti, I.; Testa, L.

    1988-01-01

    Particle size distributions and concentrations of the radioactive aerosol that arose from the Chernobyl accident were determined in Bologna and Rome. The activity Median Aerodynamic Diameters (AMAD) of Ru-103, Te-132, Cs-134 and Cs-137, determined by means of impactors, were in the range 0.8 - 1.4 μm with Geometric Standard Deviations (Sg) in the range 1.6 - 3.7. Lower AMAD and higher Sg values were found for I-131 compared to those for the other radioisotopes. The gaseous fraction of I-131 was 60-70% of the total aerosuspended activity of this isotope. A comparison between direct measurement data concerning internal contamination on volunteers and values derived from air contamination data shows that in Bologna, during May 1986, almost all the contamination was due to inhalation. The data are unable to distinguish between different inhalation models

  5. Determination of the stoichiometric rate in UO2 samples

    International Nuclear Information System (INIS)

    Moura, Sergio C.; Lima, Nelson B. de; Sassine, Andre; Bustillos, Jose Oscar Vega

    2000-01-01

    The gravimetric and voltammetric methods for determination of non-stoichiometric O/U ratio in uranium dioxide used as nuclear fuel are discussed in this work. The oxidation of uranium oxide is very complex due to many phase changes. Gravimetric and voltammetric methods do not detect phase changes. The results of this work shown that, to evaluate both methods is requiring to be done Rietveld methods by X-ray diffraction data to identify the uranium oxide phase changes. (author)

  6. Fluorimetric routine determination of uranium in urine samples

    International Nuclear Information System (INIS)

    Widua, L.; Schieferdecker, H.; Hezel, U.

    With a modified RA 2 reflectance accessory for the Zeiss PMQII/PMQ3 spectrophotometer, uranium in urine was detected with higher sensitivity. A quick method is now available with a detection limit of <2 μg U/1 urine for the determination of possible uranium incorporations, whose sensitivity meets the requirements of radiation protection. Compared with other extraction methods, the instrument outlay and the required working time are small. The total error of the method is below 5 percent

  7. Determinants of renewable energy growth: A global sample analysis

    International Nuclear Information System (INIS)

    Aguirre, Mariana; Ibikunle, Gbenga

    2014-01-01

    We investigate factors influencing country-level renewable energy growth by applying FEVD and PCSE estimation methods in a unique sample analysis. With a longer time series (1990–2010) and a broader sample size of countries (including Brazil, Russia, India, China and South Africa) than previous studies, our results reveal new insights. The results suggest that certain government-backed energy policies impede renewable energy investments, thus implying significant failures in policy design. These policies may be failing mainly because of uncertainty and the likelihood of discontinuity. Weak voluntary approaches are introduced in order to satisfy public demand for more sustainable investments and programmes; we find that these may have negative influences on the growth of renewables as well. The insight gained is consistent over the estimation methods employed. - Highlights: • Some public energy policies are shown to impede renewable energy investments; this implies failure in policy design. • Environmental concern is shown to drive renewables investment but energy security concerns do not seem to influence renewables investment. • Results suggest that countries are likely to reduce renewables commitments when under pressure to ensure energy supply. • Results seem to underscore the policy lobbying strength of the traditional energy mix industries

  8. Determining Sample Size for Accurate Estimation of the Squared Multiple Correlation Coefficient.

    Science.gov (United States)

    Algina, James; Olejnik, Stephen

    2000-01-01

    Discusses determining sample size for estimation of the squared multiple correlation coefficient and presents regression equations that permit determination of the sample size for estimating this parameter for up to 20 predictor variables. (SLD)

  9. Sample preparation combined with electroanalysis to improve simultaneous determination of antibiotics in animal derived food samples.

    Science.gov (United States)

    da Silva, Wesley Pereira; de Oliveira, Luiz Henrique; Santos, André Luiz Dos; Ferreira, Valdir Souza; Trindade, Magno Aparecido Gonçalves

    2018-06-01

    A procedure based on liquid-liquid extraction (LLE) and phase separation using magnetically stirred salt-induced high-temperature liquid-liquid extraction (PS-MSSI-HT-LLE) was developed to extract and pre-concentrate ciprofloxacin (CIPRO) and enrofloxacin (ENRO) from animal food samples before electroanalysis. Firstly, simple LLE was used to extract the fluoroquinolones (FQs) from animal food samples, in which dilution was performed to reduce interference effects to below a tolerable threshold. Then, adapted PS-MSSI-HT-LLE protocols allowed re-extraction and further pre-concentration of target analytes in the diluted acid samples for simultaneous electrochemical quantification at low concentration levels. To improve the peak separation, in simultaneous detection, a baseline-corrected second-order derivative approach was processed. These approaches allowed quantification of target FQs from animal food samples spiked at levels of 0.80 to 2.00 µmol L -1 in chicken meat, with recovery values always higher than 80.5%, as well as in milk samples spiked at 4.00 µmol L -1 , with recovery values close to 70.0%. Copyright © 2018 Elsevier Ltd. All rights reserved.

  10. Determination of Sr-90 and Cs-137 in environmental samples

    International Nuclear Information System (INIS)

    Anon.

    1987-01-01

    The comparison between the Ca concentration in the soil and the transfer factors involved indicates a clear dependence of Sr-90 soil-to-plant transport from the soil's Ca-content with the concentration level of 0.1 g Ca/kg soil appearing to be the limit level. Soil concentrations of Cs-137 determined to-date indicate a very even deposition density of Cs-137. The transfer factors of plant/soil in Chile differ but negligeably from those in Europe. (DG) [de

  11. A procedure for the rapid determination of Pu isotopes and Am-241 in soil and sediment samples by alpha spectrometry

    International Nuclear Information System (INIS)

    2009-01-01

    Reliable, comparable and 'fit for purpose' results are an essential requirement for any decision based on analytical measurements. For the analyst, the availability of tested and validated analytical procedures is a extremely important tool for production of such analytical measurements. For maximum utility, such procedures should be comprehensive, clearly formulated, and readily available to both the analyst and the customer for reference. Since 2004 the Environment Programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. In this report, a rapid procedure for the determination of Pu and Am radionuclides in soil and sediment samples is described that can be used in emergency situations. The method provides accurate and reliable results for the activity concentrations of elevated levels of 239,240 Pu, 238 Pu and 241 Am in soil and sediment samples over the course of 24 hours. The procedure has been validated in accordance with ISO guidelines

  12. Challenging genosensors in food samples: The case of gluten determination in highly processed samples.

    Science.gov (United States)

    Martín-Fernández, Begoña; de-los-Santos-Álvarez, Noemí; Martín-Clemente, Juan Pedro; Lobo-Castañón, María Jesús; López-Ruiz, Beatriz

    2016-01-01

    Electrochemical genosensors have undergone an enormous development in the last decades, but only very few have achieved a quantification of target content in highly processed food samples. The detection of allergens, and particularly gluten, is challenging because legislation establishes a threshold of 20 ppm for labeling as gluten-free but most genosensors expresses the results in DNA concentration or DNA copies. This paper describes the first attempt to correlate the genosensor response and the wheat content in real samples, even in the case of highly processed food samples. A sandwich-based format, comprising a capture probe immobilized onto the screen-printed gold electrode, and a signaling probe functionalized with fluorescein isothiocyanate (FITC), both hybridizing with the target was used. The hybridization event was electrochemically monitored by adding an anti-FITC peroxidase (antiFITC-HRP) and its substrate, tetramethylbenzidine. Binary model mixtures, as a reference material, and real samples have been analyzed. DNA from food was extracted and a fragment encoding the immunodominant peptide of α2-gliadin amplified by a tailored PCR. The sensor was able to selectively detect toxic cereals for celiac patients, such as different varieties of wheat, barley, rye and oats, from non-toxic plants. As low as 0.001% (10 mg/kg) of wheat flour in an inert matrix was reliably detected, which directly compete with the current method of choice for DNA detection, the real-time PCR. A good correlation with the official immunoassay was found in highly processed food samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Potentiometric determination of hexavalent uranium in uranium silicide samples

    International Nuclear Information System (INIS)

    Arlegui, Oscar

    1999-01-01

    The Chilean Nuclear Energy Commission's Department of Nuclear Materials has among its projects the production of fuels elements for nuclear reactors, and, therefore, the Chemical Analysis Laboratory must have a rapid and reliable method for uranium analysis, to control the uranium concentration during each stage of the production process. For this reason the Chilean Nuclear Energy Commission's Chemical Analysis Laboratory has validated a potentiometric method, which is a modification of the Davies and Gray method proposed by A.R. Eberle. This method uses the Potentiometric Titration Technique and is based on the direct and rapid reduction of uranium (VI) to Uranium (IV), in a concentrated phosphoric acid medium, with excess iron (II) used as a reducing agent. In this medium the excess iron (II) selectively oxidizes to iron (III) with nitric acid, using molybdenum (IV) as a catalyzer, the nitrous acid that is produced is eliminated by adding amidosulfuric acid. The solution is diluted with 1M sulfuric acid and the uranium (IV) obtained is titrated potentiometrically with potassium dichromate in the presence of vanadilic sulfate to obtain a better defined final titration point. The samples were softened with hydrochloric acid and nitric acid and later 50 ml were estimated in a 20% sulfuric acid medium. The analytical method was validated by comparing it with Certified Reference Material (C.R.M.) from the New Brunswick Laboratory (NBL), Metallic Uranium, CRM 112-A. The F Test and the T Test show that the value calculated is less than the tabulated value so the result is traceable to the reference material. The quantification limit, sensitivity, precision and accuracy were quantified for the method

  14. Determine the Quality of Bread Samples Used in Qazvin, Iran

    Directory of Open Access Journals (Sweden)

    Peyman Qajarbeygi

    2018-04-01

    Full Text Available In most societies, rich and important source of food considered bread. Some bakeries using sodium bicarbonate as baking soda and extra salt in bread production that his chemical compounds has adverse effects on the public health. That's why in this study we decided to evaluation of In most societies, rich and important source of food considered bread. Some bakeries using sodium bicarbonate as baking soda and extra salt in bread production that his chemical compounds has adverse effects on the public health. That's why in this study we decided to evaluation of produced bread in Qazvin province in terms of sodium bicarbonate and salt. Assessment of pH and salt take place according to Institute of Standards and Industrial Research of Iran (IRIS. Our Results demonstrated the mean±SD of pH for sangak, lavash, taftun, barbari and baguette 5.95±0.37, 5.76±0.54, 5.80±0.71, 6.10±0.68 and 7.86±1.26 respectively, and the mean±SD of salt 1.10±0.47, 1.41±0.57, 1.45±0.36, 1.40±0.32 and 1.55±1.09 respectively and the results demonstrated the value of pH and salt in the samples 65.77% (98 out of 149 and 12.75% (130 out of 149 respectively, out of standard range. Baking Soda in sangak breads and salt in baguette breads, more common of other breads. Although the Ministry of Health has banned officially the use of baking soda in breads production process, but demonstrated in this study baking soda and extra salt used in the process of breads production. Thus require more supervision and training on the non-use of sodium bicarbonate for bakers its necessary.

  15. Transverse micro-erosion meter measurements; determining minimum sample size

    Science.gov (United States)

    Trenhaile, Alan S.; Lakhan, V. Chris

    2011-11-01

    Two transverse micro-erosion meter (TMEM) stations were installed in each of four rock slabs, a slate/shale, basalt, phyllite/schist, and sandstone. One station was sprayed each day with fresh water and the other with a synthetic sea water solution (salt water). To record changes in surface elevation (usually downwearing but with some swelling), 100 measurements (the pilot survey), the maximum for the TMEM used in this study, were made at each station in February 2010, and then at two-monthly intervals until February 2011. The data were normalized using Box-Cox transformations and analyzed to determine the minimum number of measurements needed to obtain station means that fall within a range of confidence limits of the population means, and the means of the pilot survey. The effect on the confidence limits of reducing an already small number of measurements (say 15 or less) is much greater than that of reducing a much larger number of measurements (say more than 50) by the same amount. There was a tendency for the number of measurements, for the same confidence limits, to increase with the rate of downwearing, although it was also dependent on whether the surface was treated with fresh or salt water. About 10 measurements often provided fairly reasonable estimates of rates of surface change but with fairly high percentage confidence intervals in slowly eroding rocks; however, many more measurements were generally needed to derive means within 10% of the population means. The results were tabulated and graphed to provide an indication of the approximate number of measurements required for given confidence limits, and the confidence limits that might be attained for a given number of measurements.

  16. Determination of Optimal Double Sampling Plan using Genetic Algorithm

    Directory of Open Access Journals (Sweden)

    Sampath Sundaram

    2012-03-01

    Full Text Available Normal 0 false false false EN-US X-NONE X-NONE MicrosoftInternetExplorer4 Designing double sampling plan requires identification of sample sizes and acceptance numbers. In this paper a genetic algorithm has been designed for the selection of optimal acceptance numbers and sample sizes for the specified producer’s risk and consumer’s risk. Implementation of the algorithm has been illustrated numerically for different choices of quantities involved in a double sampling plan   

  1. FLAVONOIDS IN THE GRASS OF TRIBULUS TERRESTRIS L.

    Directory of Open Access Journals (Sweden)

    P. E. Khudenko

    2015-01-01

    Full Text Available The article presents active parts of Tribulus terrestris L. as a perspective sample for study. We have provided an example of flavo-noids determination with high-performance liquid chromatography / MS at the Waters Acquility chromatographer with tandem quad-rupolar MS-detector TQD (Waters.

  2. Determination of Ultralow Level 129I/127I in Natural Samples by Separation of Microgram Carrier Free Iodine and Accelerator Mass Spectrometry Detection

    DEFF Research Database (Denmark)

    Hou, Xiaolin; Zhou, Weijian; Chen, Ning

    2010-01-01

    of 129I/127I, and a detection limit of this method for 129I is calculated to be 105 atoms. This will allow us to accurately determine 129I in prenuclear geological samples of low iodine concentration with 129I/127I of 10−12, such as loess, soil, coral, rock, sediment, and groundwater. Some samples......Separation of carrier free iodine from low iodine level samples and accurate measurement of ultralow level 129I in micrograms of iodine target are essential but a bottleneck in geological dating of terrestrial system and tracer research using naturally produced 129I. In this work, we present...... a carrier free method using coprecipitation of AgI with AgCl for preparing micrograms of iodine target, associated with combustion using a tube furnace for separating iodine from solid samples and anion exchange chromatography for preconcentrating iodine from a large volume of water. An accelerator mass...

  3. Open focused microwave-assisted sample preparation for rapid total and mercury species determination in environmental solid samples

    OpenAIRE

    Tseng, C. M.; Garraud, H.; Amouroux, D.; Donard, O. F. X.; de Diego, A.

    1998-01-01

    This paper describes rapid, simple microwave-assisted leaching/ digestion procedures for total and mercury species determination in sediment samples and biomaterials. An open focused microwave system allowed the sample preparation time to be dramatically reduced to only 24 min when a power of 40-80 W was applied. Quantitative leaching of methylmercury from sediments by HNO3 solution and complete dissolution of biomaterials by an alkaline solution, such as 25% TMAH solution, were obtained. Met...

  4. Distribution of the Determinant of the Sample Correlation Matrix: Monte Carlo Type One Error Rates.

    Science.gov (United States)

    Reddon, John R.; And Others

    1985-01-01

    Computer sampling from a multivariate normal spherical population was used to evaluate the type one error rates for a test of sphericity based on the distribution of the determinant of the sample correlation matrix. (Author/LMO)

  5. Terrestrial ecology

    International Nuclear Information System (INIS)

    Anon.

    1977-01-01

    The main effort of the Terrestrial Ecology Division has been redirected to a comprehensive study of the Espiritu Santo Drainage Basin located in northeastern Puerto Rico. The general objective are to provide baseline ecological data for future environmental assessment studies at the local and regional levels, and to provide through an ecosystem approach data for the development of management alternatives for the wise utilization of energy, water, and land resources. The interrelationships among climate, vegetation, soils, and man, and their combined influence upon the hydrologic cycle will be described and evaluated. Environmental management involves planning and decision making, and both require an adequate data base. At present, little is known about the interworkings of a complete, integrated system such as a drainage basin. A literature survey of the main research areas confirmed that, although many individual ecologically oriented studies have been carried out in a tropical environment, few if any provide the data base required for environmental management. In view of rapidly changing socio-economic conditions and natural resources limitations, management urgently requires data from these systems: physical (climatological), biological, and cultural. This integrated drainage basin study has been designed to provide such data. The scope of this program covers the hydrologic cycle as it is affected by the interactions of the physical, biological, and cultural systems

  6. Determination of mercury in biologycal samples by radiochemical neutron activation analysis

    International Nuclear Information System (INIS)

    Suc, N.V.

    1989-01-01

    The radiochemical neutron activation analysis was applied to determine contents of mercury in biological samples. Samples were digested in mixing of H 2 SO 4 and HNO 3 acid. After extraction of mercury by Ni-Ditiodietylphosphoric acid in carbontetrachloride, mercury was back extracted by 5% KI solution. Contents of mercury from five samples of fish was determined by this method. The accuracy of the method was checked by comparing it with NBS standard samples and results are good agreement

  7. Quantitative method of determining beryllium or a compound thereof in a sample

    Science.gov (United States)

    McCleskey, T. Mark; Ehler, Deborah S.; John, Kevin D.; Burrell, Anthony K.; Collis, Gavin E.; Minogue, Edel M.; Warner, Benjamin P.

    2010-08-24

    A method of determining beryllium or a beryllium compound thereof in a sample, includes providing a sample suspected of comprising beryllium or a compound thereof, extracting beryllium or a compound thereof from the sample by dissolving in a solution, adding a fluorescent indicator to the solution to thereby bind any beryllium or a compound thereof to the fluorescent indicator, and determining the presence or amount of any beryllium or a compound thereof in the sample by measuring fluorescence.

  8. Experimental-calculation technique for Ksub(IC) determination using the samples of decreased dimensions

    International Nuclear Information System (INIS)

    Vinokurov, V.A.; Dymshits, A.V.; Pirusskij, M.V.; Ovsyannikov, B.M.; Kononov, V.V.

    1981-01-01

    A possibility to decrease the size of samples, which is necessary for the reliable determination of fractUre toughness Ksub(1c), is established. The dependences of crack-resistance caracteristics on the sample dimensions are determined experimentally. The static bending tests are made using the 1251 model of ''Instron'' installation with a specially designed device. The samples of the 20KhNMF steel have been tested. It is shown that the Ksub(1c) value, determined for the samples with the largest netto cross section (50x100 rm), is considerably lower than Ksub(1c) values, determined for the samples with the decreased sizes. it is shown that the developed experimental-calculated method of Ksub(1c) determination can be practically used for the samples of the decreased sizes with the introduction of the corresponding amendment coefficient [ru

  9. Determination of potential radiation exposure via terrestrial food chains by the release of radioactive material from nuclear facilities

    International Nuclear Information System (INIS)

    Handge, P.; Meurin, G.

    1978-01-01

    The radiation exposure level caused by consumption of vegetable and animal products in the environment of nuclear power plants is determined to a large extent by the release of 90 Sr, 134 Cs, and 137 Cs. For long-lived nuclides, especially 90 Sr, transfer from the soil into vegetation makes the essential contribution to plant contamination after several years of power plant operation. The relevant transfer coefficients for the different plant species vary, depending on the soil properties, between 0.02 and 6.0 [pCi/kg fresh weigth of vegetation : pCi/kg dry weight of soil] for Sr and between 1.10 -3 and 0.2 [pCi/kg fresh weight of vegetation : pCi/kg dry weight of soil] for Cs. The sensitivity analysis shows that already a variation of the transfer coefficients for Sr from 0.5 up to 2.5 [pCi/kg fresh weight of vegetation : pCi/kg dry weight of soil] and for Cs from 3.10 -2 up to 2.10 -1 cause variations in the level of radiation exposure for individual exposure pathways by factors fo 2 to 4. Correspondingly higher values are to be expected by still larger transfer of Sr and Cs from the ground to vegetation. For transfer coefficients >- 2.5 [pCi/kg fresh weight of vegetation : pCi/kg dry weight of soil], however, removal of radioactive substances from the ground by the plants must not remain without consideration any longer. (orig./HP) [de

  10. Determination of rare earth elements in natural water samples – A review of sample separation, preconcentration and direct methodologies

    Energy Technology Data Exchange (ETDEWEB)

    Fisher, Andrew, E-mail: afisher@plymouth.ac.uk [School of Geography, Earth and Environmental Sciences, Plymouth University, Drake Circus, Plymouth, Devon, PL4 8AA (United Kingdom); Kara, Derya [Department of Chemistry, Art and Science Faculty, Balikesir University, 10100, Balikesir (Turkey)

    2016-09-07

    This review discusses and compares the methods given for the determination of rare earth elements (REE) in natural water samples, including sea, river, lake, tap, ground and waste waters as well as Antarctic ice. Since REE are at very low concentrations in natural waters, numerous different preconcentration methods have been proposed to enable their measurement. These include liquid liquid extraction, dispersive liquid-liquid micro-extraction and solidified floating drop micro-extraction. In addition to liquid-liquid extraction methods, solid phase extraction using commercial resins, resins made in-house, silica-based exchange materials and other solid media is also discussed. These and other techniques such as precipitation/co-precipitation and flotation are compared in terms of speed, preconcentration factors achieved, precision, accuracy and limits of detection (LOD). Some papers have discussed the direct determination of REE in these sample types. Some have used specialised sample introduction systems such as ultrasonic nebulization whereas others have used a standard sample introduction system coupled with inductively coupled plasma mass spectrometry (ICP-MS) detection. These direct methods have also been discussed and compared. - Highlights: • The determination of rare earth elements in waters is reviewed. • Assorted preconcentration techniques are discussed and evaluated. • Detection techniques include atomic spectrometry, potentiometry and spectrophotometry. • Special nebulisers and electrothermal vaporization approaches are reviewed.

  11. Correction for sample self-absorption in activity determination by gamma spectrometry

    International Nuclear Information System (INIS)

    Galloway, R.B.

    1991-01-01

    Gamma ray spectrometry is a convenient method of determining the activity of the radioactive components in environmental samples. Commonly samples vary in gamma absorption or differ in absorption from the calibration standards available, so that accurate correction for self-absorption in the sample is essential. A versatile correction procedure is described. (orig.)

  12. 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.

  13. Determination of selected metals in coal samples from Lafia-Obi and ...

    African Journals Online (AJOL)

    coal samples were determined using atomic absorption spectroscopy (AAS). All the samples have comparable chromium and copper contents, while iron, aluminum, magnesium and potassium content vary to some extent. Metals concentrations in both Lafia-Obi and Chikila coal samples are within the limits allowed by the ...

  14. Determination of rhenium in geologic samples of sandstone-type uranium deposit

    International Nuclear Information System (INIS)

    Li Yanan; Wang Xiuqin; Yin Jinshuang

    1997-01-01

    The thiourea colorimetry method suitable for the determination of samples with rhenium content higher than 5 μg/g is described. The method is characterized by many advantages: stability of analytical results, simplicity and cheapness of reagent, and wide range of analysed samples. The catalytic colorimetry is also applied to determine trace rhenium meeting the demand for comprehensive appraisal of prospecting and exploration, recovery and utilization of rhenium. This method can also be applied to analyse rhenium of other samples

  15. Specific determination of clinical and toxicological important substances in biological samples by LC-MS

    International Nuclear Information System (INIS)

    Mitulovic, G.

    2001-02-01

    This thesis of this dissertation is the specific determination of clinical and toxicological important substances in biological samples by LC-MS. Nicotine was determined in serum after application of nicotine plaster and nicotine nasal spray with HPLC-ESI-MS. Cotinine was determined direct in urine with HPLC-ESI-MS. Short time anesthetics were determined in blood and cytostatics were determined in liquor with HPLC-ESI-MS. (botek)

  16. 90Sr and 137Cs determination in milk and foodstuff samples in North and Middle Moravia

    International Nuclear Information System (INIS)

    Bartuskova, M.; Lusnak, J.; Rada, J.; Beckova, V.

    2008-01-01

    Activities of radionuclides Sr-90 and Cs-137 in milk and parts of foodstuff have been determined in National Radiation Protection Institute for many years. Sr-90 activity in those samples determinate branch Ostrava by radiochemical procedure - precipitation with oxalic acid and measuring with using gas-flow proportional detector. Gamma spectrometry with HPGe detector is using for 137 Cs determination. (authors)

  17. Single injection 51Cr EDTA plasma clearance determination in children using capillary blood samples

    International Nuclear Information System (INIS)

    Broechner-Mortensen, J.; Christoffersen, J.

    1977-01-01

    The reliability of a determination of the total 51 Cr EDTA plasma clearance (e) (and with it the glomerular filtration rate), by a simplified single injection method (injected dose: 4.5 μCi per kg b.w.) using capillary blood samples (0.2 ml), was investigated in twenty children. Clearance values determined from capillary blood samples did not differ significantly from those measured simultaneously from venous blood samples, the mean ratio+-SD being 1.02+-0.06(n = 10). The reproducibility (total day-to-day variation) of E determined from capillary blood samples was 6.7% in children with decreased renal function (n = 3) and 6.9% in children with normal renal function (n = 7). The present data indicate that the use of capillary blood samples is an accurate and very precise approach for determination of E in children. (Auth.)

  18. Laser fluorimetric determination of uranium in environmental samples from Nile Delta and adjacent regions

    International Nuclear Information System (INIS)

    Shawky, S.; Ibrahiem, N.; Farouk, A.; Ghods, A.

    1994-01-01

    Total uranium content was determined in soil and plant samples obtained from various areas in the Nile Delta. Samples taken from east and west of the delta, Suez canal cities and from the Alexandria region were analysed using laser fluorimetry (LF). Uranium was extracted from digested samples with methyl-isobutyl ketone and measured using a laser fluorimeter. The radium content of the same soil samples was determined using gamma spectroscopy. The uranium content of plant samples was determined using LF, since this technique has a detection limit lower than that of GS. Uranium content in the samples varied between 0.6-4.4 μg/g for soil and 0.032-0.17 μg/g for plant tissue. (author)

  19. An overview of sample preparation procedures for LC-MS multiclass antibiotic determination in environmental and food samples.

    Science.gov (United States)

    Moreno-Bondi, María Cruz; Marazuela, María Dolores; Herranz, Sonia; Rodriguez, Erika

    2009-10-01

    Antibiotics are a class of pharmaceuticals that are of great interest due to the large volumes of these substances that are consumed in both human and veterinary medicine, and due to their status as the agents responsible for bacterial resistance. They can be present in foodstuffs and in environmental samples as multicomponent chemical mixtures that exhibit a wide range of mechanisms of action. Moreover, they can be transformed into different metabolites by the action of microorganisms, as well as by other physical or chemical means, resulting in mixtures with higher ecotoxicities and risks to human health than those of the individual compounds. Therefore, there is growing interest in the availability of multiclass methods for the analysis of antimicrobial mixtures in environmental and food samples at very low concentrations. Liquid chromatography (LC) has become the technique of choice for multiclass analysis, especially when coupled to mass spectrometry (LC-MS) and tandem MS (LC-MS(2)). However, due to the complexity of the matrix, in most cases an extraction step for sample clean-up and preconcentration is required before analysis in order to achieve the required sensitivities. This paper reviews the most recent developments and applications of multiclass antimicrobial determination in environmental and food matrices, emphasizing the practical aspects of sample preparation for the simultaneous extraction of antimicrobials from the selected samples. Future trends in the application of LC-MS-based techniques to multiclass antibiotic analysis are also presented.

  20. 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)

  1. Amines as extracting agents for the quantitative determinations of actinides in biological samples

    International Nuclear Information System (INIS)

    Singh, N.P.

    1987-01-01

    The use of amines (primary, secondary and tertiary chains and quaternary ammonium salts) as extracting agents for the quantitative determination of actinides in biological samples is reviewed. Among the primary amines, only Primene JM-T is used to determine Pu in urine and bone. No one has investigated the possibility of using secondary amines to quantitatively extract actinides from biological samples. Among the tertiary amines, tri-n-octylamine, tri-iso-octylamine, tyricaprylamine (Alamine) and trilaurylamine (tridodecylamine) are used extensively to extract and separate the actinides from biological samples. Only one quaternary ammonium salt, methyltricapryl ammonium chloride (Aliquat-336), is used to extract Pu from biological samples. (author) 28 refs

  2. Passive Dosing to Determine the Speciation of Hydrophobic Organic Chemicals in Aqueous Samples

    DEFF Research Database (Denmark)

    Birch, Heidi; Gouliarmou, V.; Lützhøft, Hans-Christian Holten

    2010-01-01

    A new analytical approach to determine the speciation of hydrophobic organic analytes is presented. The freely dissolved concentration in a sample is controlled by passive dosing from silicone (poly(dimethylsiloxane)), and the total sample concentration at equilibrium is measured. The free fraction...... is determined as the ratio between measured concentrations in pure water and sample. C-14-labeled fluoranthene served as model analyte, and total sample concentrations were easily measured by liquid scintillation counting. The method was applied to surface water, stormwater runoff, and wastewater...... (SPME). This analytical approach combines simplicity with high precision, and it does not require any phase separation steps....

  3. Determination of Iron and Nickel in Geological Samples by Activation Analysis with Reactor Fast Neutrons

    International Nuclear Information System (INIS)

    El Abd, A.

    2009-01-01

    Threshold reactions induced by reactor fast neutrons are well recognized. The concentration of Fe and Ni were determined in nine geological samples by activation analysis with reactor fast neutrons using the threshold reactions 5 4F e( n,p) 54 Mn and 58 Ni ( n, p )'5 8 Co respectively. The fast neutron flux was determined using the reactions 92 Mo(n, 2n) 92 mNb and 95 Mo(n,p) 95 Nb. The determined concentration of Fe and Ni in the samples were checked by determining them in the GSJ JB-1 reference material using the same , ( p, n) reactions. There are a good agreement between the measured and recommended values. The concentrations of Fe were also determined by the ) , ( n, γ) capture reactions in the geological samples and the JB-1 reference material using the K θ - NAA method. There are good agreements between the determined concentrations from the ) , ( p, n) and the ( γ, n) reactions.

  4. Determination of uranium and thorium by neutron activation analysis applied to fossil samples dating

    International Nuclear Information System (INIS)

    Ticianelli, Regina B.; Figueiredo, Ana Maria Graciano; Zahn, Guilherme S.; Kinoshita, Angela; Baffa, Oswaldo

    2011-01-01

    Electron Spin Resonance (ESR) dating is based on the fact that ionizing radiation can create stable free radicals in insulating materials, like tooth enamel and bones. The concentration of these radicals - determined by ESR - is a function of the dose deposed in the sample along the years. The accumulated dose of radiation, called Archaeological Dose, is produced by the exposition to environmental radiation provided by U, Th, K and cosmic rays. If the environmental dose rate in the site where the fossil sample is found is known, it is possible to convert this dose into the age of the sample. The annual dose rate coming from the radioactive elements present in the soil and in the sample itself can be calculated by determining the U, Th and K concentration. Therefore, the determination of the dose rate depends on the concentration of these main radioactive elements. Neutron Activation Analysis has the sensitivity and the accuracy necessary to determine U, Th and K with this objective. Depending on the composition of the sample, the determination of U and Th can be improved irradiating the sample inside a Cd capsule, reducing the thermal neutron incidence on the sample and, therefore, diminishing the activation of possible interfering nuclides. In this study the optimal irradiation and counting conditions were established for U and Th determination in fossil teeth and soil. (author)

  5. The use of slurry sampling for the determination of manganese and copper in various samples by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Tokman, Nilgun

    2007-01-01

    Manganese and copper in multivitamin-mineral supplements and standard reference materials were determined by slurry sampling electrothermal atomic absorption spectrometry. Slurries were prepared in an aqueous solution containing Triton X-100. The effects of different parameters such as ratio of solid to liquid phase volume, total slurry volume and addition of Triton X-100 as a dispersant on the analytical results were investigated. The graphite furnace programs were optimized for slurry sampling depending on the analytes and their concentrations in the samples. The linear calibration method with aqueous standard solutions was used for the quantification. At optimum experimental conditions, R.S.D. values were below 5%. The analytes were determined in the limits of 95% confidence level with respect to certified values in coal and soil standard reference materials and to those found by wet-digestion in multivitamin-mineral supplements. Detection limits (3δ) for Mn and Cu were 0.10 μg L -1 and 1.82 μg L -1 for 10 μL coal standard reference material slurry, respectively

  6. [Pretreatment of Aluminum-Lithium Alloy Sample and Determination of Argentum and Lithium by Spectral Analysis].

    Science.gov (United States)

    Zhou, Hui; Tan, Qian; Gao, Ya-ling; Sang, Shi-hua; Chen, Wen

    2015-10-01

    Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES), Flame Atomic Absorption Spectrometry (FAAS) and Visible Spectrometry (VS) was applied for determination of Ag and Li in lithium-aluminium alloy standard sample and test sample, their respective advantages and disadvantages were compared, the excellent selectivity of ICP-OES was confirmed by analyses of certified standard sample. Three different sample digestion methods were compared and discussed in this study. It was found that the better accuracy would be obtained by digesting sample with chloroazotic acid while the content of Li was measured by FAAS, and it was better to digest sample with hydrochloric acid and hydrogen peroxide while determining Ag and Li by ICP-OES simultaneously and determining Ag by FAAS and VS. The interference of co-existing elements and elimination methods was detailedly discussed. Ammonium hydroxide was added to adjust the sample solution into alkalescent and Al, Ti, Zr was precipitated by forming hydroxide precipitation, Mg and Cu was formed complex precipitation with 8-hydroxyquinoline in this condition, then the interference from matrix element to determinate Ag by FAAS was eliminated. In addition, phosphate was used to precipitate Ti to eliminate its interference for determination of Li by FAAS. The same treatment of determination for Ag by FAAS was used to eliminate the interference of matrix element for determination of Ag by VS, the excess of nitrate was added into sample and heated to release Ag+ from silver chloride complex, and the color of 8-hydroxyquinoline was eliminated because of decomposed by heating. The accuracy of analysis result for standard sample was conspicuously improved which confirms the efficient of the method to eliminate interference in this study. The optimal digestion method and eliminate interference method was applied to lithium-aluminium alloy samples. The recovery of samples was from 100.39% to 103.01% by ICP-OES determination for Ag

  7. Rapid method to determine actinides and 89/90Sr in limestone and marble samples

    International Nuclear Information System (INIS)

    Maxwell, S.L.; Culligan, Brian; Hutchison, J.B.; Utsey, R.C.; Sudowe, Ralf; McAlister, D.R.

    2016-01-01

    A new method for the determination of actinides and radiostrontium in limestone and marble samples has been developed that utilizes a rapid sodium hydroxide fusion to digest the sample. Following rapid pre-concentration steps to remove sample matrix interferences, the actinides and 89 / 90 Sr are separated using extraction chromatographic resins and measured radiometrically. The advantages of sodium hydroxide fusion versus other fusion techniques will be discussed. This approach has a sample preparation time for limestone and marble samples of <4 h. (author)

  8. Improved sample treatment for the determination of insoluble soap in sewage sludge samples by liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Cantarero, Samuel; Zafra-Gómez, A; Ballesteros, O; Navalón, A; Vílchez, J L; Crovetto, G; Verge, C; de Ferrer, J A

    2010-09-15

    A new selective and sensitive method for the determination of insoluble fatty acid salts (soap) in sewage sludge samples is proposed. The method involves a clean up of sample with petroleum ether, the conversion of calcium and magnesium insoluble salts into soluble potassium salts, potassium salts extraction with methanol, and a derivatization procedure previous to the liquid chromatography with fluorescence detection (LC-FLD) analysis. Three different extraction techniques (Soxhlet, microwave-assisted extraction and ultrasounds) were compared and microwave-assisted extraction (MAE) was selected as appropriate for our purpose. This allowed to reduce the extraction time and solvent waste (50 mL of methanol in contrast with 250 mL for Soxhlet procedure). The absence of matrix effect was demonstrated with two standards (C(13:0) and C(17:0)) that are not commercials and neither of them has been detected in sewage sludge samples. Therefore, it was possible to evaluate the matrix effect since both standards have similar environmental behaviour (adsorption and precipitation) to commercial soaps (C(10:0)-C(18:0)). The method was successfully applied to samples from different sources and consequently, with different composition. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  9. Determination of natural alpha-emitting isotopes of uranium and thorium in environmental and geological samples

    International Nuclear Information System (INIS)

    Crespo, M.T.

    1996-01-01

    It is described the complete radiochemical procedure used for the determination of uranium and thorium isotopes in environmental and geological samples by alpha spectrometry. Source preparation methods, alpha-counting and spectral analysis are also included

  10. Blood oxygen saturation determined by transmission spectrophotometry of hemolyzed blood samples

    Science.gov (United States)

    Malik, W. M.

    1967-01-01

    Use of the Lambert-Beer Transmission Law determines blood oxygen saturation of hemolyzed blood samples. This simplified method is based on the difference in optical absorption properties of hemoglobin and oxyhemoglobin.

  11. Technical developments for accurate determination of amount of samples used for TOF measurements

    Directory of Open Access Journals (Sweden)

    Terada Kazushi

    2017-01-01

    Full Text Available Activity determination of 241,243Am samples has been performed with two separate methods of calorimetry and gamma-ray spectroscopy. Decay heat measurements of the samples were carried out by using a calorimeter, and activities of the samples were accurately determined with uncertainties less than 0.45%. The primary source of uncertainty in the calorimetric method is the accuracy of available half-life data. Gamma-ray detection efficiencies of a HPGe detector were determined with uncertainties of 1.5% by combining measured efficiencies and Monte Carlo simulation. Activities of the samples were determined with uncertainties less than 2.0% by gamma-ray spectroscopy and were concordant with those of the calorimetry.

  12. A pyrolysis/gas chromatographic method for the determination of hydrogen in solid samples

    Science.gov (United States)

    Carr, R. H.; Bustin, R.; Gibson, E. K.

    1987-01-01

    A method is described for the determination of hydrogen in solid samples. The sample is heated under vacuum after which the evolved gases are separated by gas chromatography with a helium ionization detector. The system is calibrated by injecting known amounts of hydrogen, as determined manometrically. The method, which is rapid and reliable, was checked for a variety of lunar soils; the limit of detection is about 10 ng of hydrogen.

  13. Simple Modification of Karl-Fischer Titration Method for Determination of Water Content in Colored Samples

    OpenAIRE

    Eva Tavčar; Erika Turk; Samo Kreft

    2012-01-01

    The most commonly used technique for water content determination is Karl-Fischer titration with electrometric detection, requiring specialized equipment. When appropriate equipment is not available, the method can be performed through visual detection of a titration endpoint, which does not enable an analysis of colored samples. Here, we developed a method with spectrophotometric detection of a titration endpoint, appropriate for moisture determination of colored samples. The reaction takes p...

  14. Determination of artificial and natural radionuclides and others trace elements in environmental samples form Antarctica

    International Nuclear Information System (INIS)

    Schuch, L.A.; Godoy, J.M.; Nordemann, D.J.R.

    1994-01-01

    The results of the radioactive elements concentrations, determined by gamma spectrometry and the others trace elements determined by neutron activation analysis of several environmental samples (soils, marine sediments, algae mosses and lichens) in Comandante Ferraz Antartica Station are presented. The high concentrations of Cs-137 were found in lichens and mosses samples and the soils and sediments showed concentrations of natural radionuclides. (C.G.C.). 8 refs, 1 fig, 3 tabs

  15. Determination of Magnesium in Needle Biopsy Samples of Muscle Tissue by Means of Neutron Activation Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Brune, D; Sjoeberg, H E

    1964-07-15

    Magnesium has been determined by means of neutron-activation analysis in needle biopsy samples of the order of magnitude 1 mg dry weight. The procedure applied was to extract the Mg-27 activity from irradiated muscle tissue with concentrated hydrochloric acid followed by a fast hydroxide precipitation and gamma-spectrometric measurements. The Mg activity was recovered in the muscle tissue samples to (97 {+-} 2) per cent. The sensitivity for the magnesium determination is estimated as 0.3 {mu}g.

  16. An analytical method for the determination of plutonium in autopsy samples

    International Nuclear Information System (INIS)

    Santori, G.

    1983-01-01

    A sensitive method for the determination of plutonium in autopsy samples is described. After a suitable chemical pretreatment of the samples the plutonium is separated by extraction chromatography with tri-n-octylphosphine oxide (TOPO) supported on microporus polyethylene. After electrodeposition of plutonium the activity is counted by alpha spectroscopy. The global yield was 75-80%. The reagent blank activity was such to allow the determination of some femtocuries of plutonium

  17. On-line determination of manganese in solid seafood samples by flame atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Yebra, M.C.; Moreno-Cid, A.

    2003-01-01

    Manganese is extracted on-line from solid seafood samples by a simple continuous ultrasound-assisted extraction system (CUES). This system is connected to an on-line manifold, which permits the flow-injection flame atomic absorption spectrometric determination of manganese. Optimisation of the continuous leaching procedure is performed by an experimental design. The proposed method allows the determination of manganese with a relative standard deviation of 0.9% for a sample containing 23.4 μg g -1 manganese (dry mass). The detection limit is 0.4 μg g -1 (dry mass) for 30 mg of sample and the sample throughput is ca. 60 samples per hour. Accurate results are obtained by measuring TORT-1 certified reference material. The procedure is finally applied to mussel, tuna, sardine and clams samples

  18. Terrestrial studies

    International Nuclear Information System (INIS)

    Anon.

    1980-01-01

    Tritium in the organic fraction of soil, separated as water by high temperature combustion, was 5 to 50 times higher in activity than water that was freeze-dried from the same samples. The 50-year dose commitment from ingestion of crops is not influenced significantly by the plutonium in the SRP environment. This plutonium is a result of more than 20 years of operating chemical separations facilities. Techniques were developed to detect as little as 0.02 pCi/m 2 of iodine-129 and 0.2 pg of technetium-99 in soil to evaluate environmental effects. A sensitive three-stage mass spectrometer was completed for use in environmental studies of transuranium elements. Results of monitoring particle size distribution of entrapped particles containing Pu-238, and Pu-239,240 are reported

  19. [Feasibility study for whole plant medicinal use of Tribulus terrestris].

    Science.gov (United States)

    Yang, Li; Wang, Chunyu; Han, Meiw; Yang, Limin

    2009-09-01

    The content differences of leaf, plant and fruit of Tribulus terrestris was compared to study the feasibility of whole plant medicinal use. The samples were collected in three typical habitats and six different production areas of T. terrestris. The main medicinal ingredients saponins and flavonoids were determined in root, stem, leaf and fruit during the harvest time. The two ingredients were abounded in leaf and more than 2.61 times as in other parts of the plant. The results showed that there were no differences between the whole plant and the fruit. It should pay more attentions on the collection, preservation and utilization of the leaf of T. terrestris in the harvesting and processing stage. The whole plant for medical use was feasibility based on the content of the ingredients.

  20. Determination of 90Sr in environmental samples by microwave assisted digestion - chromatographic separation

    International Nuclear Information System (INIS)

    Torres, J.M.; Llaurado, M.; Rauret, G.

    1998-01-01

    The stages involved in the determination of 90 Sr in environmental samples are: sample attack, radiochemical separation (of both 90 Sr and its progeny 90 Y) and measurement. For the determination of 90 Sr, the introduction of microwave-assisted digestion methods has improved acid attack by drastically decreasing both digestion time and the volume of acidic reagents. Recent studies describe many applications of microwave-assisted methods for the determination of inorganic and organometallic compounds in several matrices. We have recently studied the microwave-assisted digestion of soils for the 90 Sr determination. The presented work extends the application of microwaves for the 90 Sr determination to other environmental samples such as sediments, vegetation and milk. An open-focused microwave system, which accepts large samples intakes usually required for radioanalytical chemistry due to the low level content of radionuclides in environmental samples, was used. This system can handle up to 10 g of sample intake which, in many cases, is enough to have acceptable limits of detection. Different digestion procedures are optimised for each matrix studied, paying special attention to the microwave power, the time of digestion and the volume of acidic reagents. Once the sample is in solution a new separation procedure using a specific resin -Sr.Spec- is applied and the measurement is performed by liquid scintillation. The results obtained are compared with a previously optimised method based on liquid-liquid extraction of 90 Y and Cerenkov radiation measurement

  1. Determination of vanadium in steel and geological samples by its extraction and spectrophotometric determination using 2,3-dihydroxynaphthalene

    International Nuclear Information System (INIS)

    Mondal, R.K.; Tarafder, P.K.; Rathore, D.P.S.

    2013-01-01

    A new and simple method for extraction and spectrophotometric determination of vanadium has been described. Iron has been removed from the sample solution by its prior extraction with MIBK from concentrated HCl medium (∼6 M). Vanadium has been determined in the form of a colored complex with 2,3-dihydroxynaphthalene after its extraction into MIBK. The method is at least 5 fold more sensitive to BPHA method. The molar absorptivity of the complex at 530 nm being 1.5 x 10 4 Lmol -1 cm -1 . For samples having >5 fold excess concentration of TiO 2 , a prior separation of TiO 2 as its (Ti (OH) (HND) 3 ) complex is a must. The method has been successfully applied to different rock, soil and steel samples. (author)

  2. Burn-up determination of irradiated thoria samples by isotope dilution-thermal ionisation mass spectrometry

    International Nuclear Information System (INIS)

    Aggarwal, S.K.; Jaison, P.G.; Telmore, V.M.; Shah, R.V.; Sant, V.L.; Sasibhushan, K.; Parab, A.R.; Alamelu, D.

    2010-03-01

    Burn-up was determined experimentally using thermal ionization mass spectrometry for two samples from ThO 2 bundles irradiated in KAPS-2. This involved quantitative dissolution of the irradiated fuel samples followed by separation and determination of Th, U and a stable fission product burn-up monitor in the dissolved fuel solution. Stable fission product 148 Nd was used as a burn-up monitor for determining the number of fissions. Isotope Dilution-Thermal Ionisation Mass Spectrometry (ID-TIMS) using natural U, 229 Th and enriched 142 Nd as spikes was employed for the determination of U, Th and Nd, respectively. Atom % fission values of 1.25 ± 0.03 were obtained for both the samples. 232 U content in 233 U determined by alpha spectrometry was about 500 ppm and this was higher by a factor of 5 compared to the theoretically predicted value by ORIGEN-2 code. (author)

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

    International Nuclear Information System (INIS)

    Thakur, P.; Mulholland, G.P.

    2012-01-01

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

  4. Determination of natural uranium, thorium and radium isotopes in water and soil samples by alpha spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Hao, Le Cong; Tao, Chau Van; Thong, Luong Van; Linh, Duong Mong [University of Science Ho Chi Minh City (Viet Nam). Faculty of Physics and Engineering Physics; Dong, Nguyen Van [University of Science Ho Chi Minh City (Viet Nam). Faculty of Chemistry

    2011-08-15

    In this study, a simple procedure for the determination of natural uranium, thorium and radium isotopes in water and soil samples by alpha spectroscopy is described. This procedure allows a sequential extraction polonium, uranium, thorium and radium radionuclides from the same sample in two to three days. It was tested and validated with the analysis of certified reference materials from the IAEA. (orig.)

  5. Determination of heavy metals in groundwater samples - ICP-MS analysis and evaluation

    International Nuclear Information System (INIS)

    Leiterer, M.; Muench, U.

    1994-01-01

    An analytical programme which permits the direct, simultaneous determination of Al, As, Cd, Cr, Cu, Mn, Ni, Pb and Zn in groundwater samples was developed for ICP-MS. Spectral mass interferences, attributable to great differences in groundwater matrices, precision and accuracy have been discussed. The evaluation of analytical results was demonstrated for selected sampling points of the groundwater observation network of Thuringia. (orig.)

  6. 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...

  7. Application of neutron activation analysis to trace elements determinations in lung samples

    International Nuclear Information System (INIS)

    Rogero, S.O.

    1991-01-01

    The purpose of this work was to apply the instrumental neutron activation analysis method to determine trace elements in lung samples from smokers and non smokers. Samples of lung tissues and lymph nodes from pulmonary hilum analyzed were collected from autopsies by researchers from Faculdade de Medicina da USP. (author)

  8. Procedure for determination of alpha emitters in urine and dregs samples

    International Nuclear Information System (INIS)

    Serdeiro, Nelida H.

    2005-01-01

    The purpose of this work is to establish the procedure for the identification and quantification of emitting alpha radionuclides in urine and dregs samples. This procedure are applied to all laboratories of the countries of the Project ARCAL LXXVII that determinate alpha emitting radionuclides in biological samples for biological assessment [es

  9. Radiochemical separation of actinides for their determination in environmental samples and waste products

    Energy Technology Data Exchange (ETDEWEB)

    Gleisberg, B [Nuclear Engineering and Analytics Rossendorf, Inc. (VKTA), Dresden (Germany)

    1997-03-01

    The determination of low level activities of actinides in environmental samples and waste products makes high demands on radiochemical separation methods. Artificial and natural actinides were analyzed in samples form the surrounding areas of NPP and of uranium mines, incorporation samples, solutions containing radioactive fuel, solutions and solids resutling from the process, and in wastes. The activities are measured by {alpha}-spectrometry and {gamma}-spectrometry. (DG)

  10. Role of NAA in determination and characterisation of sampling behaviours of multiple elements in CRMs

    International Nuclear Information System (INIS)

    Tian Weizhi; Ni Bangfa; Wang Pingsheng; Nie Huiling

    2002-01-01

    Taking the advantage of high precision and accuracy of neutron activation analysis (NAA), sampling constants have been determined for multielements in several international and Chinese reference materials. The suggested technique may be used for finding elements in existing CRMs qualified for quality control (QC) of small size samples (several mg or less), and characterizing sampling behaviors of multielements in new CRMs specifically made for QC of microanalysis. (author)

  11. A method for determination of mass per unit area inhomogeneity of thin samples in XRF analysis

    International Nuclear Information System (INIS)

    Sitko, R.; Jurczyk, J.

    1999-01-01

    The authors have presented a simple method for the determination of possible inhomogeneity of thin samples in a wavedispersive XRF analysis after previous examination of intensity distribution of exciting radiation on sample's surface. Investigations were carried out using as an example microsamples of mono- and polycrystals. Samples were prepared by digesting an analysed material directly on the substrate. The obtained results have been presented in a graphical way. (author)

  12. Determination of the REE in environmental samples near a coal power station based on k0-standardized NAA with counting in a LEPD

    International Nuclear Information System (INIS)

    Freitas, M.C.; Gouveia, M.A.; Prudencio, M.I.; Cabral, J.M.P.; Corte, F. de

    1993-01-01

    The REE contents in lichens and plants determined by k 0 -standardized NAA with LEPD and HPGe are compared. Similar values were obtained for Sm, Eu, Tb and Yb and better values for Ce and Nd by using LEPD Besides, LEPD allows the determination of Gd, Tm and Lu. The study of REE concentrations in the neighbourhood of two coal power stations show that in the station under construction (C.T. Pego), the index of accumulation of each REE by the lichens and olive tree leaves is identical in two sampling loci where the soils have different REE concentrations; and in the station in operation (C.T. Sines), the REE contents in the soils is identical and the differences observed in the lichens and wild terrestrial plants are most probably due to the fly-ashes emission from the station. (author) 9 refs.; 4 figs.; 6 tabs

  13. Sampling theorem for geometric moment determination and its application to a laser beam position detector.

    Science.gov (United States)

    Loce, R P; Jodoin, R E

    1990-09-10

    Using the tools of Fourier analysis, a sampling requirement is derived that assures that sufficient information is contained within the samples of a distribution to calculate accurately geometric moments of that distribution. The derivation follows the standard textbook derivation of the Whittaker-Shannon sampling theorem, which is used for reconstruction, but further insight leads to a coarser minimum sampling interval for moment determination. The need for fewer samples to determine moments agrees with intuition since less information should be required to determine a characteristic of a distribution compared with that required to construct the distribution. A formula for calculation of the moments from these samples is also derived. A numerical analysis is performed to quantify the accuracy of the calculated first moment for practical nonideal sampling conditions. The theory is applied to a high speed laser beam position detector, which uses the normalized first moment to measure raster line positional accuracy in a laser printer. The effects of the laser irradiance profile, sampling aperture, number of samples acquired, quantization, and noise are taken into account.

  14. Evaluating the use of gel-based sub-sampling for assessing responses of terrestrial microarthropods (Collembola and Acari) to different slurry applications and organic matter contents

    NARCIS (Netherlands)

    Jagers op Akkerhuis, G.A.J.M.; Dimmers, W.J.; Vliet, van P.C.J.; Goedhart, P.W.; Martakis, G.F.P.; Goede, de R.G.M.

    2008-01-01

    Microarthropods show considerable small-scale spatial variation, which on statistical grounds demands the use of numerous samples per experimental unit to obtain a representative density estimate. To avoid the identification of all individuals in these samples a sub-sampling technique is desirable.

  15. Determination of the neutron activation profile of core drill samples by gamma-ray spectrometry.

    Science.gov (United States)

    Gurau, D; Boden, S; Sima, O; Stanga, D

    2018-04-01

    This paper provides guidance for determining the neutron activation profile of core drill samples taken from the biological shield of nuclear reactors using gamma spectrometry measurements. Thus, it provides guidance for selecting a model of the right form to fit data and using least squares methods for model fitting. The activity profiles of two core samples taken from the biological shield of a nuclear reactor were determined. The effective activation depth and the total activity of core samples along with their uncertainties were computed by Monte Carlo simulation. Copyright © 2017 Elsevier Ltd. All rights reserved.

  16. Determination of gold and silver in geological standard samples MGI by instrument neutron activation analysis

    International Nuclear Information System (INIS)

    Lu Huijiuan; Zhou; Yunlu

    1987-01-01

    Gold and silver in geological standard samples MGI were determined by instrument neutron activation analysis. The various interferences of nuclides were considered. Corrected factors of the geometry in different positions have been determined. Using the geological standard sample MGM and radiochemical separation neutron activation method as reference, the reliability of this method is proved. Gold content in samples is 0.4-0.009 g/t, silver content is 9-0.3 g/t. Standard deviation is less than 3.5%, the precision of the measurement is 4.8-11.6%

  17. Efficiency and attenuation correction factors determination in gamma spectrometric assay of bulk samples using self radiation

    International Nuclear Information System (INIS)

    Haddad, Kh.

    2009-02-01

    Gamma spectrometry forms the most important and capable tool for measuring radioactive materials. Determination of the efficiency and attenuation correction factors is the most tedious problem in the gamma spectrometric assay of bulk samples. A new experimental and easy method for these correction factors determination using self radiation was proposed in this work. An experimental study of the correlation between self attenuation correction factor and sample thickness and its practical application was also introduced. The work was performed on NORM and uranyl nitrate bulk sample. The results of proposed methods agreed with those of traditional ones.(author)

  18. Determination of rare earth elements in uranium bearing samples using Inductively Coupled Plasma Mass Spectrometry (ICPMS)

    International Nuclear Information System (INIS)

    Mishra, S.; Chaudhury, P.; Pradeepkumar, K.S.; Sahoo, S.K.

    2017-01-01

    In the present study a methodology has been described for determination of REEs without involving separation and the method is successfully applied for determination of REE concentration in uranium ore as well as in soil samples from a uranium mining site

  19. Speciation and Determination of Low Concentration of Iron in Beer Samples by Cloud Point Extraction

    Science.gov (United States)

    Khalafi, Lida; Doolittle, Pamela; Wright, John

    2018-01-01

    A laboratory experiment is described in which students determine the concentration and speciation of iron in beer samples using cloud point extraction and absorbance spectroscopy. The basis of determination is the complexation between iron and 2-(5-bromo-2- pyridylazo)-5-diethylaminophenol (5-Br-PADAP) as a colorimetric reagent in an aqueous…

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  1. Determination of blood cell subtype concentrations from frozen whole blood samples using TruCount beads.

    Science.gov (United States)

    Langenskiöld, Cecilia; Mellgren, Karin; Abrahamsson, Jonas; Bemark, Mats

    2016-06-24

    In many studies it would be advantageous if blood samples could be collected and analyzed using flow cytometry at a later stage. Ideally, sample collection should involve little hands-on time, allow for long-term storage, and minimally influence the samples. Here we establish a flow cytometry antibody panel that can be used to determine granulocytes, monocytes, and lymphocyte subset concentrations in fresh and frozen whole blood using TruCount technology. The panel can be used on fresh whole-blood samples as well as whole-blood samples that have been frozen after mixing with 10% DMSO. Concentrations in frozen and fresh sample is highly correlated both when frozen within 4 h and the day after collection (r ≥ 0.98), and the estimated concentration in frozen samples was between 91 and 94% of that in fresh samples for all cell types. Using this method whole-blood samples can be frozen using a simple preparation method, and stored long-term before accurate determination of cell concentration. This allows for standardized analysis of the samples at a reference laboratory in multi-center studies. © 2016 International Clinical Cytometry Society. © 2016 International Clinical Cytometry Society.

  2. A study on aluminum determination in environmental samples by Neutron Activation Analysis

    International Nuclear Information System (INIS)

    Noyori, Amanda

    2017-01-01

    Aluminum determinations are of great interest since this element is toxic to humans and it is widely distributed in the environment. Besides, the determinations of this element by conventional analytical methods present difficulties due to sample contamination during the analyses. Neutron activation analysis (NAA) for Al determination presents advantages of fast analyses and of high sensitivity. However, NAA of Al does present problems of P and Si nuclear reaction interferences. Aluminum is determined by measuring 28 Al, formed in the reaction 27 Al (n, γ) 28 Al, the same radioisotope formed in reactions 31 P (n, α) 28 Al and 28 Si (n, p) 28 Al. The purpose of this study was to determine Al in environmental samples by NAA correcting these interferences using correction factors, and determining P and Si concentrations in the samples. In this study, certified reference materials and biomonitor samples (tree barks and lichen) were analyzed. Experimental procedure consisted of irradiating an aliquot of the sample at the IEA-R1 nuclear research reactor together with Al standard, followed by gamma ray spectrometry. Phosphorus was determined by measuring beta radiation of 32 P using a Geiger-Müller counter. Silicon was determined by epithermal neutron activation analysis and measuring 29 Al formed in the reaction 29 Si (n, p) 29 Al. Results obtained in the determination of Al, P and Si in the certified reference materials showed good precision and accuracy with |Z-score| ≤ 2. Aluminum results in the biomonitor samples varied from to 253 to 15783 μg g -1 . In the case of P its concentrations varied from 283 to 1946 μg g -1 . Silicon determinations in biomonitors varied from 0.11 to 7.8 %. The interference contribution rates in the analyses of the biomonitor samples were of the order of 2.0 % and this contribution depends on the relation between concentrations of interfering elements and of Al in the sample. Detection limit values of Al in the biomonitor analyses

  3. Fluorimetric determination of uranium in certain refractory minerals, environmental samples and industrial waste materials

    International Nuclear Information System (INIS)

    Premadas, A.; Saravanakumar, G.

    2005-01-01

    A simple sample decomposition and laser fluorimetric determination of uranium at trace level is reported in certain refractory minerals, like ilmenite, rutile, zircon and monazite; environmental samples viz. soil and sediments; industrial waste materials, such as, coal fly ash and red mud. Ilmenite sample is decomposed by heating with ammonium fluoride. Rutile, zircon and monazite minerals are decomposed by fusion using a mixture of potassium bifluoride and sodium fluoride. Environmental and industrial waste materials are brought into solution by treating with a mixture of hydrofluoric and nitric acids. The laser induced fluorimetric determination of uranium is carried out directly in rutile, zircon and in monazite minerals and after separation in other samples. The determination limit was 1 μg x g -1 for ilmenite, soil, sediment, coal fly ash and red mud samples, and it is 5 μg x g -1 for rutile, zircon and monazite. The method is also developed for the optical fluorimetric determination of uranium (determination limit 10 μg x g -1 ) in ilmenite, rutile, zircon and monazite minerals. The methods are simple, accurate, and precise and they require small quantity of sample and can be applied for the routine analysis. (author)

  4. 210Pb and 210Po determination in environmental samples using liquid scintillation counting and alpha spectrometry

    International Nuclear Information System (INIS)

    Perez Sanchez, D.; Martin Sanchez, A.; Jurado Vargas, M.

    2003-01-01

    A simple radiochemical procedure has been developed to determine 210 Pb and 210 Po in environmental samples from the same matrix. Sediment samples are decomposed by leaching with mineral acids or by microwave digestion, while water samples are pre-concentrated. One part of the resulting solution, spiked with 209 Po, is used for 210 Po determination by spontaneous deposition onto nickel disks (a-spectrometry). The other part is assayed for 210 Pb, separating the Pb either by anion-exchange (sediment samples), or by solvent extraction (water samples). The 210 Pb source is finally prepared by precipitation as oxalate and the chemical recovery determined by gravimetry. The 210 Pb activity concentration is determined by liquid scintillation. A standard sediment sample supplied by IAEA and spiked water samples were analysed to check the procedure. The 210 Pb and 210 Po measurements agreed well with the certifications, deviations being less than 10%. The mean recoveries for Pb and Po were (70±12)% and (77±8)% for sediments, and (70±10)% and (81±7)% for waters, respectively. (author)

  5. Quantitative determination of minerals in Nevada Test Site samples by x-ray diffraction

    International Nuclear Information System (INIS)

    Pawloski, G.A.

    1983-07-01

    The external standard intensity ratio technique has been developed into a routine procedure for quantitatively determining mineralogic compositions of Nevada Test Site (NTS) samples by x-ray diffraction. This technique used ratios of x-ray intensity peaks from the same run which eliminates many possible errors. Constants have been determined for each of thirteen minerals commonly found in NTS samples - quartz, montmorillonite, illite, clinoptilolite, cristobalite, feldspars, calcite, dolomite, hornblende, kaolinite, muscovite, biotite, and amorphous glass. Ratios of the highest intensity peak of each mineral to be quantified in the sample and the highest intensity peak of quartz are used to calculate sample composition. The technique has been tested on samples with three to eleven components representative of geologic environments at NTS, and is accurate to 7.0 wt % of the total sample. The minimum amount of each of these minerals detectable by x-ray diffraction has also been determined. QUANTS is a computer code that calculates mineral contents and produces a report sheet. Constants for minerals in NTS samples other than those listed above can easily be determined, and added to QUANTS at any time

  6. Standardization of method to determine 241Pu in urine samples by liquid scintillation analyzer

    International Nuclear Information System (INIS)

    Raveendran, Nanda; Rao, D.D.; Yadav, J.R.; Baburajan, A.

    2015-01-01

    As a part of radiation protection programme, occupational workers of fuel reprocessing plant are checked for internal contamination by analyzing urine samples periodically. Urine samples are analyzed to determine 239+240 Pu and 238 Pu by using standard conventional method and are counted by alpha spectrometry. 241 Pu is also one of the contaminant present in the urine sample of radiation workers. It is a low beta emitter with E max 21 keV. A methodology for the determination of this nuclide was standardized by using radiochemical analysis followed by Liquid Scintillation Counting. The method was tested and found suitable for the determination of 241 Pu in urine sample for the assessment of Committed Effective Dose (CED). (author)

  7. Sample size determination for logistic regression on a logit-normal distribution.

    Science.gov (United States)

    Kim, Seongho; Heath, Elisabeth; Heilbrun, Lance

    2017-06-01

    Although the sample size for simple logistic regression can be readily determined using currently available methods, the sample size calculation for multiple logistic regression requires some additional information, such as the coefficient of determination ([Formula: see text]) of a covariate of interest with other covariates, which is often unavailable in practice. The response variable of logistic regression follows a logit-normal distribution which can be generated from a logistic transformation of a normal distribution. Using this property of logistic regression, we propose new methods of determining the sample size for simple and multiple logistic regressions using a normal transformation of outcome measures. Simulation studies and a motivating example show several advantages of the proposed methods over the existing methods: (i) no need for [Formula: see text] for multiple logistic regression, (ii) available interim or group-sequential designs, and (iii) much smaller required sample size.

  8. Matrix modifiers application during microimpurities determination in complex samples by electrothermal atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Bejzel', N.F.; Daaman, F.I.; Fuks-Pol', G.R.; Yudelevich, I.G.

    1993-01-01

    The review covers publications of primarily last 5 years and is devoted to the use of matrix modifiers (MM) for the determinations of trace impurities in complex samples by electrothermal atomic-absorption analysis. The role of MM in analytical process has been discussed as well as MM influence on all the elements of analytical system; factors, determining the effectiveness of MM action, the basis types of MM have been described. A great body of information is tabulated on the use of different MM for the determination of particular analysis in geological, medicobiological, technological, ecological samples and in pure materials and chemicals

  9. Matrix modification for determination of microimpurities in complex samples by electrothermal atomic-absorption spectrometry

    International Nuclear Information System (INIS)

    Bejzel', N.F.; Daaman, F.I.; Fuks-Pol', G.R.; Yudelevich, I.G.

    1993-01-01

    The review covers publications of primarily last 5 years and is devoted to the use of matrix modifiers (MM) for the determinations of trace impurities in complex samples by electrothermal atomic-absorption analysis. The role of MM in analytical process has been discussed as well as MM influence on all the elements of analytical system; factors, determining the effectiveness of MM action, the basis types of MM have been described. A great body of information is tabulated on the use of different MM for the determination of particular analysis in geological, medicobiological, technological, ecological samples and in pure materials and chemicals

  10. Preconcentration and determination of heavy metals in water, sediment and biological samples

    Directory of Open Access Journals (Sweden)

    Shirkhanloo Hamid

    2011-01-01

    Full Text Available In this study, a simple, sensitive and accurate column preconcentration method was developed for the determination of Cd, Cu and Pb ions in river water, urine and sediment samples by flame atomic absorption spectrometry. The procedure is based on the retention of the analytes on a mixed cellulose ester membrane (MCEM column from buffered sample solutions and then their elution from the column with nitric acid. Several parameters, such as pH of the sample solution, volume of the sample and eluent and flow rates of the sample were evaluated. The effects of diverse ions on the preconcentration were also investigated. The recoveries were >95 %. The developed method was applied to the determination of trace metal ions in river water, urine and sediment samples, with satisfactory results. The 3δ detection limits for Cu, Pb and Cd were found to be 2, 3 and 0.2 μg dm−3, respectively. The presented procedure was successfully applied for determination of the copper, lead and cadmium contents in real samples, i.e., river water and biological samples.

  11. Determination of uranium and thorium in rock samples from Harargaj Anticline by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Rahman, M.; Molla, N.I.; Sharif, A.K.M.; Basunia, S.; Islam, S.; Miah, R.U.; Hossain, S.M.; Chowdhury, M.I.; Bhuiyan, A.D.; Stegnar, P.

    1993-01-01

    Uranium and thorium were determined in geological materials such as radioactive rock samples collected from the Harargaj Anticline in Moulavi Bazar. The pure instrumental neutron activation analysis (INAA) technique was used in qualitative and quantitative analysis of the rock samples for U and Th. The samples were properly prepared together with their standards and simultaneously irradiated in a neutron flux of the order of 10 12 n*cm -2 *s -1 using the TRIGA MARK II research reactor facility at the AERE, Savar, Dhaka. After activation the samples were subjected to γ-ray spectrometry using a high purity germanium detection system. As a result of the analysis, U and Th could be determined. The data are consistent with the values reported by the ground radiometric survey group for some of the samples. (author) 7 refs.; 1 fig.; 2 tabs

  12. On the accuracy of protein determination in large biological samples by prompt gamma neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kasviki, K. [Institute of Nuclear Technology and Radiation Protection, NCSR ' Demokritos' , Aghia Paraskevi, Attikis 15310 (Greece); Medical Physics Laboratory, Medical School, University of Ioannina, Ioannina 45110 (Greece); Stamatelatos, I.E. [Institute of Nuclear Technology and Radiation Protection, NCSR ' Demokritos' , Aghia Paraskevi, Attikis 15310 (Greece)], E-mail: ion@ipta.demokritos.gr; Yannakopoulou, E. [Institute of Physical Chemistry, NCSR ' Demokritos' , Aghia Paraskevi, Attikis 15310 (Greece); Papadopoulou, P. [Institute of Technology of Agricultural Products, NAGREF, Lycovrissi, Attikis 14123 (Greece); Kalef-Ezra, J. [Medical Physics Laboratory, Medical School, University of Ioannina, Ioannina 45110 (Greece)

    2007-10-15

    A prompt gamma neutron activation analysis (PGNAA) facility has been developed for the determination of nitrogen and thus total protein in large volume biological samples or the whole body of small animals. In the present work, the accuracy of nitrogen determination by PGNAA in phantoms of known composition as well as in four raw ground meat samples of about 1 kg mass was examined. Dumas combustion and Kjeldahl techniques were also used for the assessment of nitrogen concentration in the meat samples. No statistically significant differences were found between the concentrations assessed by the three techniques. The results of this work demonstrate the applicability of PGNAA for the assessment of total protein in biological samples of 0.25-1.5 kg mass, such as a meat sample or the body of small animal even in vivo with an equivalent radiation dose of about 40 mSv.

  13. On the accuracy of protein determination in large biological samples by prompt gamma neutron activation analysis

    International Nuclear Information System (INIS)

    Kasviki, K.; Stamatelatos, I.E.; Yannakopoulou, E.; Papadopoulou, P.; Kalef-Ezra, J.

    2007-01-01

    A prompt gamma neutron activation analysis (PGNAA) facility has been developed for the determination of nitrogen and thus total protein in large volume biological samples or the whole body of small animals. In the present work, the accuracy of nitrogen determination by PGNAA in phantoms of known composition as well as in four raw ground meat samples of about 1 kg mass was examined. Dumas combustion and Kjeldahl techniques were also used for the assessment of nitrogen concentration in the meat samples. No statistically significant differences were found between the concentrations assessed by the three techniques. The results of this work demonstrate the applicability of PGNAA for the assessment of total protein in biological samples of 0.25-1.5 kg mass, such as a meat sample or the body of small animal even in vivo with an equivalent radiation dose of about 40 mSv

  14. A radiochemical procedure for the determination of Po-210 in environmental samples

    International Nuclear Information System (INIS)

    Godoy, J.M.; Schuettelkopf, H.

    1980-07-01

    A radiochemical procedure for the determination of Po-210 in environmental samples was developed. Soil, sediments, filter materials, plants, water and food samples can be analyzed for Po-210. Wet ashing is achieved with HNO 3 + H 2 O 2 or HCl + HNO 3 . To separate disturbing substances, a coprecipitation with Te is used for sample materials containing silica. Po-210 deposition from HCl solution on Ag platelets with other sample materials is possible directly. Deposited Po-210 is counted by α-spectrometry. For chemical yield determination Po-208 is added, yields range between 60% and 100%. A lower detection limit of about 0,002 pCi Po-210/sample is achievable. (orig./HP) [de

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

    DEFF Research Database (Denmark)

    Qiao, Jixin

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

  16. Flame Photometric Determination of Lithium Contents Down to 10{sup -3} ppm in Water Samples

    Energy Technology Data Exchange (ETDEWEB)

    Joensson, Guenther

    1963-04-15

    A flame photometric method has been developed for determination of submicro contents of lithium in water. The intensity of the emission from lithium increases about three times if 20 % of a mixture of acetone - amyl alcohol (4:1) is added to the sample. Interferences by stray light from sodium present is eliminated with a special absorption filter. Interferences from oxide bands of the alkaline earth metals are completely suppressed after adding aluminium to the sample. With the development of this routine method it is possible by flame photometry to directly determine 0.01 ppm lithium with an error of analysis less than 10 %. Furthermore the investigation shows that, after concentration of the sample by evaporation, contents down to 10{sup -3} ppm can be determined without any difficulty. One person can run up to 50 determinations per day.

  17. Intercomparison study of sampling methods for the determination of polychlorinated biphenyl (PCB) in seawater

    International Nuclear Information System (INIS)

    Schulz-Bull, D.E.

    1999-01-01

    The determination of organic pollutants in seawater is a serious problem, as their concentrations in the water column are typical in the fg - ng/L range. Available methods therefore includes extensive sampling and laboratory work. The development of simple sampling techniques for organochlorines (e.g. passive sampling with semipermeable membrane device (SPMD), mussel watch) is required. Three methods for the measurement of trace organochlorines in seawater were investigated: (1) the filtration (GF/F) and extraction (XAD-2 resin) of seawater with an in-situ pumping system, (2) biological-accumulation by mussels (mytilus edulis) and (3) passive sampling with SPMD

  18. Determination of mercury species in biological samples by inductively coupled plasma mass spectrometry combined with solvent extraction and ultrasonication

    International Nuclear Information System (INIS)

    Sun, J.; Li, Y.F.; Wang, J.X.; Chen, C.Y.; Li, B.; Gao, Y.X.; Chai, Z.F.

    2005-01-01

    Mercury (Hg) is a well-known toxic element. The toxic effects of Hg depend on its chemical forms. The most important chemical forms are elemental Hg (Hg 0 ), inorganic Hg (Hg 2+ ) and methylmercury (CH 3 Hg + ). In the biogeochemical cycle of Hg, these species may interchange in atmospheric, aquatic and terrestrial environments. Among them, methylmercury is considerably higher toxic than elemental mercury and inorganic mercury because it is recognized as one of major health hazards for human due to its teratogenic, immunotoxic, and neurotoxic effects. Therefore, determinations of not only total mercury, but also methylmercury content in biological samples is necessary. In large numbers of analytical methods, inductively coupled plasma mass spectrometry (ICP-MS) using conventional sample introduction with a peristaltic pump is widely used for the determination of trace metals in a wide variety of different sample matrices. ICP-MS can offer high sensitivity, low detection limit, reasonable accuracy and precision, and can easily be automated. However, mercury is considered as an element with analytical problems. One problem is well known in Hg analysis that the memory effect increases the blank counts and worsens the analytical performance of ICP-MS. The possibility of Hg losses during sample decomposition procedure due to its volatility is another important issue. Additionally, its high first ionization potential and numerous isotopes have limited its sensitivity in ICP-MS analysis. In order to solve the above questions, the present work was carried out to develop a method based on ICP-MS coupled with solvent extraction for determination of mercury species in biological samples. At first step, we investigated different solvent extraction methods including acid leaching, CuSO 4 extraction, alkaline-methanol extraction, and surfactant extraction with ultrasonication for methylmercury determination using the certified reference materials GBW07601 (Human Hair). Next, we

  19. Rapid determination of radium-224/226 in seawater sample by alpha spectrometry.

    Science.gov (United States)

    Song, Lijuan; Yang, Yonggang; Luo, Maoyi; Ma, Yan; Dai, Xiongxin

    2017-05-01

    A new radiochemical separation method has been developed for rapid determination of alpha-emitting radium isotopes in seawater samples. This method can be applied for the measurement of 226 Ra in seawater samples when 224 Ra is used as tracer for chemical recovery correction. Likewise, 226 Ra can also be added as tracer for the determination of 224 Ra in seawater sample. In the method, radium is first pre-concentrated with hydrous titanium oxide (HTiO) and is purified by combined anion/cation exchange column chromatographic separation. The radium in the eluate is then co-precipitated with HTiO, dissolved in 9 M H 2 SO 4 , and followed through a BaSO 4 micro-precipitation step to prepare a thin-layer counting source to determine the activities of 224 Ra/ 226 Ra by alpha spectrometry. Replicate spike and blank samples were measured to evaluate the performance of the procedure. The minimum detectable activity concentration was determined to be 0.5 mBq·L -1 for 226 Ra and 0.4 mBq·L -1 for 224 Ra in 1 L of seawater sample with a counting time of 48 h. The method is a promising candidate for rapid measurement for alpha-emitting Ra isotopes in a large population of environment water samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Fast and effective determination of strontium-90 in high volumes water samples

    International Nuclear Information System (INIS)

    Basarabova, B.; Dulanska, S.

    2014-01-01

    A simple and fast method was developed for determination of 90 Sr in high volumes of water samples from vicinity of nuclear power facilities. Samples were taken from the environment near Nuclear Power Plants in Jaslovske Bohunice and Mochovce in Slovakia. For determination of 90 Sr was used solid phase extraction using commercial sorbent Analig R Sr-01 from company IBC Advanced Technologies, Inc.. Determination of 90 Sr was performed with dilute solution of HNO 3 (1.5-2 M) and also tested in base medium with NaOH. For elution of 90 Sr was used eluent EDTA with pH in range 8-9. To achieve fast determination, automation was applied, which brings significant reduction of separation time. Concentration of water samples with evaporation was not necessary. Separation was performed immediately after filtration of analyzed samples. The aim of this study was development of less expensive, time unlimited and energy saving method for determination of 90 Sr in comparison with conventional methods. Separation time for fast-flow with volume of 10 dm 3 of water samples was 3.5 hours (flow-rate approximately 3.2 dm 3 / 1 hour). Radiochemical strontium yield was traced by using radionuclide 85 Sr. Samples were measured with HPGe detector (High-purity Germanium detector) at energy E φ = 514 keV. By using Analig R Sr-01 yields in range 72 - 96 % were achieved. Separation based on solid phase extraction using Analig R Sr-01 employing utilization of automation offers new, fast and effective method for determination of 90 Sr in water matrix. After ingrowth of yttrium samples were measured by Liquid Scintillation Spectrometer Packard Tricarb 2900 TR with software Quanta Smart. (authors)

  1. Determination of molybdenum and selenium in bioenvironmental samples using neutron activation analysis

    International Nuclear Information System (INIS)

    Abu-Samra, A.; Morris, J.S.; Koirtyohann, S.R.; Vogt, J.R.

    1974-01-01

    Because of the increasing interest as to their roles in biological systems, a procedure has been developed by which molybdenum and selenium can be determined at nanogram levels in these types of samples. Results from the analysis of orchard leaves and bovine liver are presented. The samples are packaged in pre-cleaned quartz vials prepared from GE-204 tubing. If both selenium and molybdenum are to be determined, the samples are irradiated for 40 or more hours at a thermal neutron flux of 8 x 10 13 n cm -2 sec -1 . After the samples have decayed for approximately 48 hours the vials are unpackaged, cleaned in aqua-regia, and broken. The irradiation period can be reduced to 24 hours if molybdenum is to be determined individually or if the selenium content is known to be 1 microgram or more. The sample is digested with carriers and the selenium is then distilled as a volatile selenium halide. Elemental selenium is precipitated by reduction with SO 2 produced through the protonation of the hydrogen sulfite ion and subsequent decomposition of the resulting sulfurous acid. The 401 keV summation peak of 75 Se is normally used for quantitative determination. The chemical yield is determined by drying and weighing the elemental selenium

  2. Comparison of biamperometric and voltammetric method for plutonium and uranium determination in FBTR fuel samples

    International Nuclear Information System (INIS)

    Jayachandran, Kavitha; Gupta, Ruma; Gamare, Jayashree; Kamat, J.V.; Aggarwal, S.K.

    2015-01-01

    Accurate and precise determination of Pu and U in reactor fuel materials is essential for the characterization of the fuel as well as for fissile material accounting. Biamperometric method has been in routine use for Pu and U determination in a variety of nuclear fuel materials in our laboratory for past 25 years. A new methodology based on differential pulse voltammetry at single walled carbon nanotube modified gold electrode has been developed by us for the simultaneous determination of Pu and U in fuel samples. In order to validate the status of the methodologies employed for Pu and U determination, comparison experiments were performed involving Pu and U determination in FBTR fuel samples. Results of these studies are reported in this paper. (author)

  3. Determination of some trace elements in biological samples using XRF and TXRF techniques

    International Nuclear Information System (INIS)

    Khuder, A.; Karjou, J.; Sawan, M. K.

    2006-07-01

    XRF and TXRF techniques were successfully used for the multi-element determination of trace elements in whole blood and human head hair samples. This was achieved by the direct analysis using XRF technique with different collimation units and by the optimized chemical procedures for TXRF analysis. Light element of S and P were preferably determined by XRF with primary x-ray excitation, while, elements of K, Ca, Fe, and Br were determined with a very good accuracy and precision using XRF with Cu- and Mo-secondary targets. The chemical procedure dependent on the preconcentration of trace elements by APDC was superiorly used for the determination of traces of Ni and Pb in the range of 1.0-1.7 μg/dl and 11-23 μg/dl, respectively, in whole blood samples by TXRF technique; determination of other elements as Cu and Zn was also achievable using this approach. Rb in whole blood samples was determined directly after the digestion of samples using PTFE-bomb for TXRF analysis. (author)

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

    International Nuclear Information System (INIS)

    Qiao, J.

    2011-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Qiao, J.

    2011-03-15

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

  6. 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

  7. Sampling

    CERN Document Server

    Thompson, Steven K

    2012-01-01

    Praise for the Second Edition "This book has never had a competitor. It is the only book that takes a broad approach to sampling . . . any good personal statistics library should include a copy of this book." —Technometrics "Well-written . . . an excellent book on an important subject. Highly recommended." —Choice "An ideal reference for scientific researchers and other professionals who use sampling." —Zentralblatt Math Features new developments in the field combined with all aspects of obtaining, interpreting, and using sample data Sampling provides an up-to-date treat

  8. Determination of lanthanides in fossil samples using laser induced breakdown spectroscopy

    International Nuclear Information System (INIS)

    Anzano, J.M.; Lasheras, R.J.; Canudo, I.; Laguna, M.

    2017-01-01

    As being a fast, simple and relatively non-destructive analytical technique Laser-induced breakdown spectroscopy (LIBS) has a large variety of applications including the analysis of paleontological samples. In this work LIBS is employed for the quantitative determination of lanthanides (Ce, Dy, Er, Eu, Gd, Ho, La, Lu, Nd, Sm, Tb, Tm and Yb) in vertebrate fossil samples comprising teeth, disarticulated complete or fragmented bones, eggshell fragments, and coprolites of dinosaurs, mammals and crocodiles. For emission line data, standard AnalaR grade salts of lanthanides were used. The major components: iron, calcium, magnesium, silicon and aluminum in the samples were also determined. The analytical information may be helpful in studying the samples for their age, formation environment and other paleontological properties. (author)

  9. An improved combustion apparatus for the determination of organically bound tritium in environmental samples

    International Nuclear Information System (INIS)

    Du, Lin; Shan, Jian; Ma, Yu-Hua; Wang, Ling; Qin, Lai-Lai; Pi, Li; Zeng, You-Shi; Xia, Zheng-Hai; Wang, Guang-Hua; Liu, Wei

    2016-01-01

    This paper reports an improved combustion apparatus for the determination of organically bound tritium in environmental samples. The performance of this apparatus including the recovery rate and reproducibility was investigated by combusting lettuce and pork samples. To determine the factors for the different recovery rates of lettuce and pork and investigate whether the samples were completely oxidized, the ashes and exhaust gases produced by the combustion were analyzed. The results indicate that the apparatus showed an excellent performance in the combustion of environmental samples. Thus, the improvements conducted in this study were effective. - Highlights: • Three major improvements were made to develop the combustion apparatus for OBT. • The recovery is higher and more stable than that of current equipment. • Little hydrogen was present in the ashes and exhaust after combustion.

  10. [Standard sample preparation method for quick determination of trace elements in plastic].

    Science.gov (United States)

    Yao, Wen-Qing; Zong, Rui-Long; Zhu, Yong-Fa

    2011-08-01

    Reference sample was prepared by masterbatch method, containing heavy metals with known concentration of electronic information products (plastic), the repeatability and precision were determined, and reference sample preparation procedures were established. X-Ray fluorescence spectroscopy (XRF) analysis method was used to determine the repeatability and uncertainty in the analysis of the sample of heavy metals and bromine element. The working curve and the metrical methods for the reference sample were carried out. The results showed that the use of the method in the 200-2000 mg x kg(-1) concentration range for Hg, Pb, Cr and Br elements, and in the 20-200 mg x kg(-1) range for Cd elements, exhibited a very good linear relationship, and the repeatability of analysis methods for six times is good. In testing the circuit board ICB288G and ICB288 from the Mitsubishi Heavy Industry Company, results agreed with the recommended values.

  11. Determination of pesticides and toxic potency of rainwater samples in western Greece.

    Science.gov (United States)

    Rouvalis, Angela; Karadima, Constantina; Zioris, Ioannis V; Sakkas, Vasilios A; Albanis, Triantafyllos; Iliopoulou-Georgudaki, Joan

    2009-03-01

    Rainwater samples from four municipalities located in Achaia Prefecture, Greece, were collected from March to September 2006. The toxic potency of pollutants present in 36 rainwater samples was tested using Daphnia pulex. The pesticide determination was conducted with GC-MS. Only phosphamidon was detected, which appeared in 52% and 13% of the rural and urban areas, respectively. The toxicity of rainwater was determined in 52% and 46.7% of the rural and urban area samples, respectively. Chemical analyses showed that in rural areas, the PO(4)(3-) ions had higher concentrations than in urban areas. On the other hand, the SO(4)(2-), NO(-)(3), and NO(-)(2) anions are more highly concentrated in urban areas. Correlation analysis proved that the toxicity of the rainwater samples is moderate, affected by the presence of the insecticide only in the rural areas. The results indicated that toxicity can be directly assessed via bioassays, even when unknown pollutants are present.

  12. Gridsampler – A Simulation Tool to Determine the Required Sample Size for Repertory Grid Studies

    Directory of Open Access Journals (Sweden)

    Mark Heckmann

    2017-01-01

    Full Text Available The repertory grid is a psychological data collection technique that is used to elicit qualitative data in the form of attributes as well as quantitative ratings. A common approach for evaluating multiple repertory grid data is sorting the elicited bipolar attributes (so called constructs into mutually exclusive categories by means of content analysis. An important question when planning this type of study is determining the sample size needed to a discover all attribute categories relevant to the field and b yield a predefined minimal number of attributes per category. For most applied researchers who collect multiple repertory grid data, programming a numeric simulation to answer these questions is not feasible. The gridsampler software facilitates determining the required sample size by providing a GUI for conducting the necessary numerical simulations. Researchers can supply a set of parameters suitable for the specific research situation, determine the required sample size, and easily explore the effects of changes in the parameter set.

  13. Radium 226 and uranium isotopes simultaneously determination in water samples using liquid scintillation counter

    International Nuclear Information System (INIS)

    Al-Masri, M.S.; Al-Akel, B.; Saaid, S.; Nashawati, A.

    2007-04-01

    In this work a method has been developed to determine simultaneously Radium 226 and Uranium isotopes in water samples by low back ground Liquid Scintillation Counter. Radium 226 was determined by its progeny Polonium 214 after one month of sample storage in order to achieve the equilibrium between Radium 226 and Polonium 214. Uranium isotopes were determined by subtracting Radium 226 activity from total alpha activity. The method detection limits were 0.049 Bq/L and 0.176 Bq/L for Radium 226 and Uranium isotopes respectively. The repeatability limits were ± 0.32 Bq/L and ± 0.9 Bq/L for Radium 226 and Uranium isotopes respectively. While relative errors were % 9.5 and %18.2 for Radium 226 and Uranium isotopes respectively. On the other hand, the report presented the results of different standard and natural samples.(author)

  14. Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Rosa, Mychelle M.L.; Maihara, Vera A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT. [Comissao Nacional de Energia Nuclear (LAPOC/CNEN-MG), Pocos de Caldas, MG (Brazil). Laboratorio de Pocos de Caldas

    2015-07-01

    The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ({sup 234}U, {sup 235}U and {sup 238}U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

  15. Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

    International Nuclear Information System (INIS)

    Rosa, Mychelle M.L.; Maihara, Vera A.; Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT.

    2015-01-01

    The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ( 234 U, 235 U and 238 U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

  16. Study of performance characteristics of a radiochemical method to determine uranium in biological samples

    International Nuclear Information System (INIS)

    Puga, Maria J.; Cerchietti, Maria L.R.; Prudenzo, J.E.; Arguelles, Maria G.

    2005-01-01

    In this paper is described a methodology to calculate detection limit (Ld), quantification level (Lq) and minimum detectable activity (MDA) in a radiochemical method for determination of uranium in urine samples. The concentration is measured by fluorimetry and alpha gross activity using liquid scintillation counting (LSC). The calculation of total propagated uncertainty on a spike sample is presented. Furthermore, the major sources of uncertainty and percentage contribution in both measurements are assessed. (author)

  17. Determination of carbon-14 environmental samples by mixing 14CO2 with a liquid scintillator

    International Nuclear Information System (INIS)

    Garcia Sanz, M.R.; Gomez, V.; Heras, M.C.; Beltran, M.A.

    1990-01-01

    A method for the determination of Carbon-14 ( 14 CO 2 ) in environmental samples has been developed. The method use the direct absorption of the carbon dioxide into Carbosorb, followed with incorporation of the mixture (Carbosorb-CO 2 ) to the liquid scintillator. The results obtained to apply this method and the benzene synthesis, usual in our laboratory, are discused and compared. The method of collection of atmospheric samples is also described. (Author)

  18. Quantitative determination of alpha-quartz in airborne dust samples by x-ray diffraction

    International Nuclear Information System (INIS)

    Bayon, A.; Roca, M.

    1982-01-01

    The quantitative determination by X-ray diffractometry of alpha-quartz In airborne respirable dust samples on silver membrane filters is considered. A cobalt anode X-ray tube Is employed. NiO is used as Internal standard In order to compensate for both the variations of specimen absorption and the effect due to the nonuniformity of the incident X-ray beam and to the incomplete homogeneity on the filters of samples and standards. (Author) 17 refs

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

    International Nuclear Information System (INIS)

    Zal U'yun Wan Mahmood

    2002-01-01

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

  20. Determination of Carbon-14 in environmental samples by mixing 14CO2 with a liquid scintillator

    International Nuclear Information System (INIS)

    Garcia, M. R.; Gomez, V.; Heras, M. C.; Beltran, M. A.

    1990-01-01

    A method for the determination of Carbon-14 (14CO2) in environmental samples has been developed. The method use the direct absorption of the carbon dioxide into Carbosorb, followed with incorporation of the mixture (Carbosorb-CO2) to the liquid scintillator. The results obtained to apply this method and the benzene synthesis, usual in our laboratory, are discussed and compared. The method of collection of atmospheric samples is also described. (Author) 10 refs

  1. Determination of alpha-dose rates and chronostratigraphical study of travertine samples

    International Nuclear Information System (INIS)

    Oufni, L.; University Moulay Ismail, Errachidia; Misdaq, M.A.; Boudad, L.; Kabiri, L.

    2001-01-01

    Uranium and thorium contents in different layers of stratigraphical sedimentary deposits have been evaluated by using LR-115 type II and CR-39 solid state nuclear track detectors (SSNTD). A method has been developed for determining the alpha-dose rates of the sedimentary travertine samples. Using the U/Th dating method, we succeeded in age dating carbonated level sampled in the sedimentary deposits. Correlation between the stratigraphy, alpha-dose rates and age has been investigated. (author)

  2. Quantitative determination of alpha-quartz in airbone dust samples by X-ray diffraction

    International Nuclear Information System (INIS)

    Bayon, A.; Roca, M.

    1982-01-01

    The quantitative determination by X-ray diffractometry of alpha-quartz in airbone respirable dust samples on silver membrane filters is considered. A cobalt anode X-ray tube is employec. NiO is used as internal standard in order to compensate for both the variations of specimen absorption and the effect due to the nonuniformity of the incident X-ray beam and to the incomplete homogeneity on the filters of samples and standards. (auth.) [es

  3. 210Pb and 210Po determination in environmental samples using liquid scintillation counting and alpha spectrometry

    International Nuclear Information System (INIS)

    Sanchez, D.P.; Sanchez, A.M.; Vargas, M.J.

    2002-01-01

    A simple radiochemical procedure has been developed to determine 210 Pb and 210 Po in environmental samples. After adding 209 Po tracer and Pb carrier, an aliquot of the sample is decomposed by microwave digestion or by evaporation with mineral acids (depending on the expected activity of the sample). Part of the leaching solution must be used for 210 Po determination, preparing a polonium source by spontaneous deposition onto a nickel disk. The quantitative recoveries are determined using a standard 209 Po tracer, and the activity concentration is determined by isotopic dilution alpha spectrometry. The remaining part of the leaching solution is used for 210 Pb determination by means of two alternative methods: lead can be retained from 1.5 M HCl by the DOWEX 1 X 8, Cl - form resin in a chromatographic column, and stripped with deionised water, or it can be separated by solvent extraction as a lead bromide complex with the organic compound ALIQUAT-336 in toluene (this second method is used preferably in water samples). The Pb source for measurement is prepared by precipitation as oxalate and the chemical recovery determined by gravimetry. The activity concentration of 210 Pb is calculated from the spectra measured with a liquid scintillation spectrometer. Several certified material samples supplied by IAEA were analysed to check the procedure. The measured values for 210 Pb and 210 Po were in good agreement with the certified values presenting deviations lower than 5%. Several environmental samples (river and well waters and also sediments) from zones impacted by Uranium mine exploitation were analysed using the described procedure. The mean yields of Pb and Po were (70 ± 10)% and (81 ± 7)% for waters and (70 ± 12)% and (77 ± 8)% for sediments. (author)

  4. Determination of minor-and trace elements in magnesite samples, by activation analysis

    International Nuclear Information System (INIS)

    Sepulveda Munita, C.J.A.

    1979-01-01

    A method employing activation analysis with thermal neutron was developed for the determination of minor and trace elements in magnesite samples from the states of Ceara and Bahia (Brazil). Ten samples were analyzed. A qualitative analysis of the samples indicated the presence of Mn, Fe, Sc, Ca, Cu, Co and some of the lanthanides. The experimental part includes a non-destructive analysis of manganese and analysis with chemical separation of the other elements, individually or in groups, after sample dissolution, The dissolutions were made with concentrated HCl and the further separations were carried out in 8 N HCl medium. Iron was separated by means of an extraction of HFeCl 4 with isopropyl ether. Scandium and calcium were determined by retention of scandium with di-(2-ehylhexyl) phosphoric acid (HDEHP). The activities of 46 Sc and 47 Sc (a 47 Ca descendant) were employed for the analysis of scandium and calcium in the sample. In the effluent of the kieselguhr column copper and cobalt were determined, after retention in an anionic resin of the CuCl - 3 and CoCl - 3 complexes. Finally, in the effluent of the resin, the lanthanide group was separated by oxalate precipitation. In the gamma-ray spectrum of this precipitate the elements europium, cerium, samarium and lanthanum were determined. A detailed study of the possible interferences in the neutron activation analysis of the elements analysed was also made. The precision and accuracy of the results obtained and the sensitivity of the method are discussed. (Author) [pt

  5. Determination of phosphorus in small amounts of protein samples by ICP-MS.

    Science.gov (United States)

    Becker, J Sabine; Boulyga, Sergei F; Pickhardt, Carola; Becker, J; Buddrus, Stefan; Przybylski, Michael

    2003-02-01

    Inductively coupled plasma mass spectrometry (ICP-MS) is used for phosphorus determination in protein samples. A small amount of solid protein sample (down to 1 micro g) or digest (1-10 micro L) protein solution was denatured in nitric acid and hydrogen peroxide by closed-microvessel microwave digestion. Phosphorus determination was performed with an optimized analytical method using a double-focusing sector field inductively coupled plasma mass spectrometer (ICP-SFMS) and quadrupole-based ICP-MS (ICP-QMS). For quality control of phosphorus determination a certified reference material (CRM), single cell proteins (BCR 273) with a high phosphorus content of 26.8+/-0.4 mg g(-1), was analyzed. For studies on phosphorus determination in proteins while reducing the sample amount as low as possible the homogeneity of CRM BCR 273 was investigated. Relative standard deviation and measurement accuracy in ICP-QMS was within 2%, 3.5%, 11% and 12% when using CRM BCR 273 sample weights of 40 mg, 5 mg, 1 mg and 0.3 mg, respectively. The lowest possible sample weight for an accurate phosphorus analysis in protein samples by ICP-MS is discussed. The analytical method developed was applied for the analysis of homogeneous protein samples in very low amounts [1-100 micro g of solid protein sample, e.g. beta-casein or down to 1 micro L of protein or digest in solution (e.g., tau protein)]. A further reduction of the diluted protein solution volume was achieved by the application of flow injection in ICP-SFMS, which is discussed with reference to real protein digests after protein separation using 2D gel electrophoresis.The detection limits for phosphorus in biological samples were determined by ICP-SFMS down to the ng g(-1) level. The present work discusses the figure of merit for the determination of phosphorus in a small amount of protein sample with ICP-SFMS in comparison to ICP-QMS.

  6. Evaluation of active sampling strategies for the determination of 1,3-butadiene in air

    Science.gov (United States)

    Vallecillos, Laura; Maceira, Alba; Marcé, Rosa Maria; Borrull, Francesc

    2018-03-01

    Two analytical methods for determining levels of 1,3-butadiene in urban and industrial atmospheres were evaluated in this study. Both methods are extensively used for determining the concentration of volatile organic compounds in the atmosphere and involve collecting samples by active adsorptive enrichment on solid sorbents. The first method uses activated charcoal as the sorbent and involves liquid desorption with carbon disulfide. The second involves the use of a multi-sorbent bed with two graphitised carbons and a carbon molecular sieve as the sorbent, with thermal desorption. Special attention was paid to the optimization of the sampling procedure through the study of sample volume, the stability of 1,3-butadiene once inside the sampling tube and the humidity effect. In the end, the thermal desorption method showed better repeatability and limits of detection and quantification for 1,3-butadiene than the liquid desorption method, which makes the thermal desorption method more suitable for analysing air samples from both industrial and urban atmospheres. However, sampling must be performed with a pre-tube filled with a drying agent to prevent the loss of the adsorption capacity of the solid adsorbent caused by water vapour. The thermal desorption method has successfully been applied to determine of 1,3-butadiene inside a 1,3-butadiene production plant and at three locations in the vicinity of the same plant.

  7. A rapid method for the determination on fluoride in geological samples

    International Nuclear Information System (INIS)

    Josephson, M.; Cook, E.B.T.; Dixon, K.

    1977-01-01

    An account is given of a rapid procedure for the determination by use of the specific-ion electrode of fluoride in geological samples. The sample is fused with sodium hydroxide in a nickel crucible in a muffle furnace. The melt is leached with water, a buffer solution of ammonium citrate is added, and the fluoride activity is measured with a specific-ion electrode. All operations are carried out in the crucible, making possible approximately 100 determinations a day. The precision of the method is approximately 10 per cent at a fluoride concentration of 500 p.p.m., which is acceptable for geological-survey work [af

  8. Bayesian sample size determination for cost-effectiveness studies with censored data.

    Directory of Open Access Journals (Sweden)

    Daniel P Beavers

    Full Text Available Cost-effectiveness models are commonly utilized to determine the combined clinical and economic impact of one treatment compared to another. However, most methods for sample size determination of cost-effectiveness studies assume fully observed costs and effectiveness outcomes, which presents challenges for survival-based studies in which censoring exists. We propose a Bayesian method for the design and analysis of cost-effectiveness data in which costs and effectiveness may be censored, and the sample size is approximated for both power and assurance. We explore two parametric models and demonstrate the flexibility of the approach to accommodate a variety of modifications to study assumptions.

  9. Determination of total alpha and beta activities on vegetable samples by LSC

    International Nuclear Information System (INIS)

    Nogueira, Regina Apolinaria; Santos, Eliane Eugenia dos; Bakker, Alexandre Pereira; Vavassori, Giullia

    2011-01-01

    Gross alpha and beta analyses are screening techniques used for environmental radioactivity monitoring. The present study proposes to determine the gross alpha and beta activities in vegetable samples by using LSC - liquid scintillation spectrometry. The procedure was applied to vegetable foods. After ashing vegetable samples in a muffle furnace, 100 mg of ash were added to gel mixture of scintillation cocktails, Water - Instagel - Ultima Gold AB (6:10:4) ml, in polyethylene vial. Am-241 standard solution and a KCl (K-40) solution were used to determine the counting configuration, alpha/beta efficiencies and spillover

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

    International Nuclear Information System (INIS)

    Gasco, C.; Alvarez Garcia, A.

    1988-01-01

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

  11. Quantitative HPLC determination of [99mTc]-pertechnetate in radiopharmaceuticals and biological samples: Pt. 1

    International Nuclear Information System (INIS)

    Tianze Zhou; Hirth, W.W.; Heineman, W.R.; Deutsch, Edward

    1988-01-01

    Techniques have been developed which allow HPLC (high performance liquid chromatography) to be used for the quantitative determination of [ 99m Tc]pertechnetate in radiopharmaceuticals and biological samples. An instrumental technique accounts for 99m Tc species which do not elute from the HPLC column, while a chemical technique obviates interferences caused by Sn(II). These two techniques are incorporated into an anion exchange HPLC procedure which is applied to the determination of [ 99m Tc]pertechnetate in 99m Tc-diphosphonate radiopharmaceuticals and biological samples. (author)

  12. Sensor-triggered sampling to determine instantaneous airborne vapor exposure concentrations.

    Science.gov (United States)

    Smith, Philip A; Simmons, Michael K; Toone, Phillip

    2018-06-01

    It is difficult to measure transient airborne exposure peaks by means of integrated sampling for organic chemical vapors, even with very short-duration sampling. Selection of an appropriate time to measure an exposure peak through integrated sampling is problematic, and short-duration time-weighted average (TWA) values obtained with integrated sampling are not likely to accurately determine actual peak concentrations attained when concentrations fluctuate rapidly. Laboratory analysis for integrated exposure samples is preferred from a certainty standpoint over results derived in the field from a sensor, as a sensor user typically must overcome specificity issues and a number of potential interfering factors to obtain similarly reliable data. However, sensors are currently needed to measure intra-exposure period concentration variations (i.e., exposure peaks). In this article, the digitized signal from a photoionization detector (PID) sensor triggered collection of whole-air samples when toluene or trichloroethylene vapors attained pre-determined levels in a laboratory atmosphere generation system. Analysis by gas chromatography-mass spectrometry of whole-air samples (with both 37 and 80% relative humidity) collected using the triggering mechanism with rapidly increasing vapor concentrations showed good agreement with the triggering set point values. Whole-air samples (80% relative humidity) in canisters demonstrated acceptable 17-day storage recoveries, and acceptable precision and bias were obtained. The ability to determine exceedance of a ceiling or peak exposure standard by laboratory analysis of an instantaneously collected sample, and to simultaneously provide a calibration point to verify the correct operation of a sensor was demonstrated. This latter detail may increase the confidence in reliability of sensor data obtained across an entire exposure period.

  13. Determination of Boron in soils and plants samples using spectrophotometric method

    International Nuclear Information System (INIS)

    Stas, J.; Hariri, Z.

    2011-10-01

    In this work, the concentration of boron in soil and plant samples was determined with UV-vis spectrophotometer by using azomethine-H as a complex reagent. The calibration curve for boron determination in the range of (0μ3 g.mL - 1) was constructed by plotting the measured absorption of the yellow azomethine-H-B complex at λmax = 412.6 nm against boron concentration in the aqueous phase. The detection limit, repeatability limit, intermediate precision, accuracy, and recovery coefficient of this method were calculated and found to be 0.021 μg.mL - 1, 0.335% , 0.81%, 2.93%, (98.4-101.5)% respectively. The influence of some foreign ions on the determination of boron were also investigated in detail, most of the studied ions, like iron, iodide, and calcium can be tolerated within the ranges of (20-35μg.mL-1), (3000-5000μg.mL - 1) , (15000-30000μg.mL - 1) respectively. This is due to the fact, that ascorbic acid and EDTA in the buffer masking reagent reaction system can be very effective in masking these ions. This method was found to be economic and suitable for boron determination in standard and local samples (soil, plant) and requires small amount of sample (1g). This method can also be applied for boron determination in water samples (drinking and industrial waste water).(author)

  14. Application of the neutron activation analysis method to the multielemental determination of food samples

    International Nuclear Information System (INIS)

    Maihara, V.A.

    1985-01-01

    The application of thermal neutron activation analysis method for determining elements presented at low concentration and level of traces in bread and dried milk samples, using non-destructive and chemical analyses, was studied. The non-destructive analyses were based on measurements of gamma spectrometry of samples and standards irradiated by thermal neutron flux on the order of 10 12 n cm -2 s -1 . The irradiation time varied from some minutes to 8 hours. The Na, Cl, Mn, Br, Fe, Zn, Rb, Sb, Cr and Sc elements in bread samples were determined. The Na, K, Cl, Ca, Mg, Br, Al, Zn, Rb, Sb and Cr elements in dried milk samples were determined. In destructive analysis, the 24 Na radioisotope was separeted by retention on hydrated antimony pentoxide column from 8N HCL after digestion of organic matter. The bread was dissolved in HNO 3 concentrated and 70% of HCLO 4 and the dried milk was dissolved in HNO 3 concentrated and H 2 O 2 . The 64 Cu, 69m Zn and 140 La radioisotopes determined. The concentrations obtained for dried milk were compared with data obtained by other authors from different contries. Basic considerations on detection limit related to its application on the technique used in this work, were done. The detection limits and trace elements using the Currie and Girardi methods were determined. The accuracy of results obtained for trace element detection limits is discussed. (Author) [pt

  15. Determination of radiocesium in environmental water samples using copper ferro(II)cyanide and sodium tetraphenylborate

    International Nuclear Information System (INIS)

    Popov, L.; Kuleff, I.; Djingova, R.

    2006-01-01

    A procedure for the radiochemical separation and radiochemical purification of radiocesium ( 134 Cs and 137 Cs) in bulk environmental water samples is proposed. Radiocesium was removed from the water by cation-exchange with copper ferro(II)cyanide and was purified by precipitation with sodium tetraphenylborate. The influence of the concentration of potassium in the water sample on the chemical yield was investigated. The validation of the proposed method was carried out by analyzing reference materials. The application of the method was demonstrated with the determination of the concentration of radiocesium in water samples from rivers around NPP 'Kozloduy', Bulgaria, Danube and Ogosta. (author)

  16. Uranium and thorium determination in water samples taken along River Kura

    International Nuclear Information System (INIS)

    Ahmadov, M.M.; Ibadov, N.A.; Safarova, K.S.; Humbatov, F.Y.; Suleymanov, B.A.

    2014-01-01

    Full text : In the present investigation, uranium and thorium concentration in rivers water of Azerbaijan has been measured using inductively coupled plasma mass spectrometry. The Agilent 7700x series ICP-MS applied for analysis of water samples. This method is based on direct introduction of samples, without any chemical pre-treatment, into an inductively coupled plasma plasma mass spectrometer. Uranium and thorium was determined at the mass mass numbers of 238 and 232 respectively using Bi-209 as internal standard. The main purpose of the study is to measure the level of uranium and thorium in water samples taken along river Kura

  17. Determination of low concentrations of uranium in granite samples by X-ray fluorescence

    International Nuclear Information System (INIS)

    Roca, M.; Diaz-Guerra, J.P.

    1981-01-01

    An x-ray fluorescence method for the determination of uranium in granite samples for concentrations ranging from 3 to 100 ppm U 3 O 8 has been developed. To this purpose a sample holder, specially designed, allowing the irradiation of sample surfaces 42.5 mm in diameter and a molybdenum tube operating with a power of 2700 W (90 kV, 30 mA) are used. The background influence and the spectral interferences from rubidium and strontium have been taken into account and specific correction coefficients have been computed. A Basic program facilitates the report of the analytical results. (author)

  18. Determination of selenium in food matrices by replicate sample neutron activation analysis

    International Nuclear Information System (INIS)

    Ventura, M.G.; Freitas, M.C.; Ventura, M.G.; Pacheco, A.M.G.

    2009-01-01

    The replicate sample instrumental neutron activation method was optimized and used for the determination of selenium in foodstuffs. The method was reliable, yielding accurate results. Lower detections limits were obtained after each successive irradiation. Different irradiation conditions were used depending on the type of sample. For samples with higher selenium contents (meat, fish, eggs), the measured selenium in the first replicate is in all cases larger than the detection limit, but a better accuracy was obtained with a larger number of replicates (2-3 replicates). For samples with extremely low selenium contents (vegetable samples), at least seven replicates were necessary to obtain a concentration value two times larger than the detection limit. (author)

  19. An analytical protocol for the determination of total mercury concentrations in solid peat samples

    DEFF Research Database (Denmark)

    Roos-Barraclough, F; Givelet, N; Martinez-Cortizas, A

    2002-01-01

    Traditional peat sample preparation methods such as drying at high temperatures and milling may be unsuitable for Hg concentration determination in peats due to the possible presence of volatile Hg species, which could be lost during drying. Here, the effects of sample preparation and natural.......12 and 8.52 ng kg(-1) h(-1), respectively). Fertilising the peat slightly increased Hg loss (3.08 ng kg(-1) h(-1) in NPK-fertilised peat compared to 0.28 ng kg(-1) h(-1) in unfertilised peat, when averaged over all temperatures used). Homogenising samples by grinding in a machine also caused a loss of Hg....... A comparison of two Hg profiles from an Arctic peat core, measured in frozen samples and in air-dried samples, revealed that no Hg losses occurred upon air-drying. A comparison of Hg concentrations in several plant species that make up peat, showed that some species (Pinus mugo, Sphagnum recurvum...

  20. Study of phosphors determination in biological samples; Estudo da determinacao de fosforo em amostras biologicas

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Rosangela Magda de

    1994-12-31

    In this paper, phosphors determination by neutron activation analysis in milk and bone samples was studied employing both instrumental and radiochemical separation methods. The analysis with radiochemistry separation consisted of the simultaneous irradiation of the samples and standards during 30 minutes, dissolution of the samples, hold back carrier, addition precipitation of phosphorus with ammonium phosphomolibdate (A.M.P.) and phosphorus-32 by counting by using Geiger-Mueller detector. The instrumental analysis consisted of the simultaneous irradiation of the samples and standards during 30 minutes, transfer of the samples into a counting planchet and measurement of the beta radiation emitted by phosphorus-32, after a suitable decay period. After the phosphorus analysis methods were established they were applied to both commercial milk and animal bone samples, and data obtained in the instrumental and radiochemical separation methods for each sample, were compared between themselves. In this work, it became possible to obtain analysis methods for phosphorus that can be applied independently of the sample quantity available, and the phosphorus content in the samples or interference that can be present in them. (author). 51 refs., 7 figs., 4 tabs.

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

    International Nuclear Information System (INIS)

    Johnson, D.; Beach, C.

    1990-01-01

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

  2. Determination of 226Ra by gamma spectrometry: study of packaging vial of sample for analysis

    International Nuclear Information System (INIS)

    Carneiro, Andre Cavalcanti

    2015-01-01

    Determination of radioactivity levels of 226 Ra by gamma spectrometry in a sample is based on measurements of 214 Pb and 214 Bi, daughters of 222 Rn. Because radon is a gas, it can leak from the sample vial or accumulate on the upper empty it. If the vial has any crack, there will be loss of gas, which will cause error in determining the 226 Ra concentration. One possible cause of cracks in the vials, that houses standards and samples, is the radiolysis action in the vial material, usually a polymer. As the demand 226 Ra analysis in different matrices (geological samples, food, plants, etc.) is increasing, it was decided to study some polymer vials available on the market, to verify the feasibility to be used when is applied the analysis method using gamma spectrometry. Four types of polymer vials have been studied. The radiation doses in walls of the vials caused by natural radionuclides present in the sample were simulated using gamma irradiation. Tests, such as compressive strength test and tightness, were applied to the irradiated and non-irradiated vials. First, to verify the effect of radiolysis on the vial material and also if there was 222 Rn diffusion in their walls. These preliminary results pointed out that the acrylic vials are the best option of packaging samples for analysis. This study should be repeated in a larger number of samples for a better evaluation. (author)

  3. Epiboron instrumental neutron activation analysis for the determination of iodine in various salt samples

    International Nuclear Information System (INIS)

    Nyarko, B.J.B.; Serfor-Armah, Y.; Osae, S.; Akaho, E.H.K.; Anim-Sampong, S.; Maakuu, B.T.

    2001-01-01

    Epiboron instrumental neutron activation analysis (EINAA) using flexible boron as thermal neutron filter, has been used to analyze several salt samples obtained from various markets in Ghana for iodine. The method involves the irradiation of samples in boron carbide-lined polyethylene vials at the outer irradiation site of the Ghana Research Reactor-1 (GHARR-1). The samples were then counted directly without any pre-treatment on a Canberra N-type HPGe detector. The qualitative and quantitative analyses were done using the 443 keV photopeak of 128 I. The precision and accuracy of the method have been evaluated and the detection limits of the various samples were calculated. The values of iodine determined in the iodized salt range between 10.0 and 210 ppm. For non-iodinated salts, iodine levels were below 500 ppb. The values obtained show great variations among the salt samples, sample collection time and from market to market. This results show that the method can be successfully applied in the determination of trace amount of iodine in salt samples without any chemical separation. (author)

  4. Using forbidden ordinal patterns to detect determinism in irregularly sampled time series.

    Science.gov (United States)

    Kulp, C W; Chobot, J M; Niskala, B J; Needhammer, C J

    2016-02-01

    It is known that when symbolizing a time series into ordinal patterns using the Bandt-Pompe (BP) methodology, there will be ordinal patterns called forbidden patterns that do not occur in a deterministic series. The existence of forbidden patterns can be used to identify deterministic dynamics. In this paper, the ability to use forbidden patterns to detect determinism in irregularly sampled time series is tested on data generated from a continuous model system. The study is done in three parts. First, the effects of sampling time on the number of forbidden patterns are studied on regularly sampled time series. The next two parts focus on two types of irregular-sampling, missing data and timing jitter. It is shown that forbidden patterns can be used to detect determinism in irregularly sampled time series for low degrees of sampling irregularity (as defined in the paper). In addition, comments are made about the appropriateness of using the BP methodology to symbolize irregularly sampled time series.

  5. Determination of drugs in biological fluids by direct injection of samples for liquid-chromatographic analysis.

    Science.gov (United States)

    Mullett, Wayne M

    2007-03-10

    The analysis of drugs in various biological fluids is an important criterion for the determination of the physiological performance of a drug. After sampling of the biological fluid, the next step in the analytical process is sample preparation. The complexity of biological fluids adds to the challenge of direct determination of the drug by chromatographic analysis, therefore demanding a sample preparation step that is often time-consuming, tedious, and frequently overlooked. However, direct on-line injection methods offer the advantage of reducing sample preparation steps and enabling effective pre-concentration and clean-up of biological fluids. These procedures can be automated and therefore reduce the requirements for handling potentially infectious biomaterial, improve reproducibility, and minimize sample manipulations and potential contamination. The objective of this review is to present an overview of the existing literature with emphasis on advances in automated sample preparation methods for liquid-chromatographic methods. More specifically, this review concentrates on the use of direct injection techniques, such as restricted-access materials, turbulent-flow chromatography and other automated on-line solid-phase extraction (SPE) procedures. It also includes short overviews of emerging automated extraction-phase technologies, such as molecularly imprinted polymers, in-tube solid-phase micro-extraction, and micro-extraction in a packed syringe for a more selective extraction of analytes from complex samples, providing further improvements in the analysis of biological materials. Lastly, the outlook for these methods and potential new applications for these technologies are briefly discussed.

  6. Spectrophotometric determination of mercury in water samples after preconcentration using dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Lemos, Valfredo Azevedo; dos Santos, Liz Oliveira; Silva, Eldevan dos Santos; Vieira, Emanuel Vitor dos Santos

    2012-01-01

    A simple method for the determination of mercury in water samples after preconcentration using dispersive liquid-liquid microextraction is described. The procedure is based on the extraction of mercury in the form of a complex and its subsequent determination by spectrophotometry. The complex is formed between Hg(II) and 2-(2-benzothiazolylazo)-p-cresol. The detection at 650 nm is performed directly in the metal-rich phase, which is spread on a triacetylcellulose membrane. The method eliminates the need to use a cuvet or large quantities of samples and reagents. The parameters that influence the preconcentration were studied, and the analytical characteristics were determined. The enrichment factor and the consumptive index for this method were 64 and 0.16 mL, respectively. The LOD (3.3 microg/L) and LOQ (11.1 microg/L) were also determined. The accuracy of the method was tested by the determination of mercury in certified reference materials BCR 397 (Human Hair) and SRM 2781 (Domestic Sludge). The method was applied to the determination of mercury in samples of drinking water, sea water, and river water.

  7. New method for simultaneous determination of 55Fe and 59Fe in blood serum samples

    International Nuclear Information System (INIS)

    Saukkonen, H.; Uhlenius, R.

    1978-01-01

    Routine methods for the measurement of 55 Fe and 59 Fe activities in biological samples are frequently required in metabolic studies of iron. A new simple method for the simultaneous determination of 59 Fe and 55 Fe concentration in 5 cm 3 samples of blood is described and carefully evaluated. Before the measurement of the activity, organic matter was eliminated by HNO 3 -HClO 4 wet ashing and iron was electroplated onto a copper plate. The accuracy of results was studied by assessing samples, which contained known amounts of radioactivity and determining the counts per nanocurie in each case. The accuracy of the results of 59 Fe and 55 Fe determinations was found to be about 5%. The method has been routinely used to determine iron resorption in patients using the double isotope method. The determination proved to be satisfactory and not too laborious. When performing the yield determination there is a way of detecting and correcting mistakes or incompleteness in different stages of the measurement, thus leading to a high degree of reliability. (T.G.)

  8. EDXRF applied to the chemical element determination of small invertebrate samples

    International Nuclear Information System (INIS)

    Magalhaes, Marcelo L.R.; Santos, Mariana L.O.; Cantinha, Rebeca S.; Souza, Thomas Marques de; Franca, Elvis J. de

    2015-01-01

    Energy Dispersion X-Ray Fluorescence - EDXRF is a fast analytical technique of easy operation, however demanding reliable analytical curves due to the intrinsic matrix dependence and interference during the analysis. By using biological materials of diverse matrices, multielemental analytical protocols can be implemented and a group of chemical elements could be determined in diverse biological matrices depending on the chemical element concentration. Particularly for invertebrates, EDXRF presents some advantages associated to the possibility of the analysis of small size samples, in which a collimator can be used that directing the incidence of X-rays to a small surface of the analyzed samples. In this work, EDXRF was applied to determine Cl, Fe, P, S and Zn in invertebrate samples using the collimator of 3 mm and 10 mm. For the assessment of the analytical protocol, the SRM 2976 Trace Elements in Mollusk produced and SRM 8415 Whole Egg Powder by the National Institute of Standards and Technology - NIST were also analyzed. After sampling by using pitfall traps, invertebrate were lyophilized, milled and transferred to polyethylene vials covered by XRF polyethylene. Analyses were performed at atmosphere lower than 30 Pa, varying voltage and electric current according to the chemical element to be analyzed. For comparison, Zn in the invertebrate material was also quantified by graphite furnace atomic absorption spectrometry after acid treatment (mixture of nitric acid and hydrogen peroxide) of samples have. Compared to the collimator of 10 mm, the SRM 2976 and SRM 8415 results obtained by the 3 mm collimator agreed well at the 95% confidence level since the E n Number were in the range of -1 and 1. Results from GFAAS were in accordance to the EDXRF values for composite samples. Therefore, determination of some chemical elements by EDXRF can be recommended for very small invertebrate samples (lower than 100 mg) with advantage of preserving the samples. (author)

  9. EDXRF applied to the chemical element determination of small invertebrate samples

    Energy Technology Data Exchange (ETDEWEB)

    Magalhaes, Marcelo L.R.; Santos, Mariana L.O.; Cantinha, Rebeca S.; Souza, Thomas Marques de; Franca, Elvis J. de, E-mail: marcelo_rlm@hotmail.com, E-mail: marianasantos_ufpe@hotmail.com, E-mail: rebecanuclear@gmail.com, E-mail: thomasmarques@live.com.pt, E-mail: ejfranca@cnen.gov.br [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil)

    2015-07-01

    Energy Dispersion X-Ray Fluorescence - EDXRF is a fast analytical technique of easy operation, however demanding reliable analytical curves due to the intrinsic matrix dependence and interference during the analysis. By using biological materials of diverse matrices, multielemental analytical protocols can be implemented and a group of chemical elements could be determined in diverse biological matrices depending on the chemical element concentration. Particularly for invertebrates, EDXRF presents some advantages associated to the possibility of the analysis of small size samples, in which a collimator can be used that directing the incidence of X-rays to a small surface of the analyzed samples. In this work, EDXRF was applied to determine Cl, Fe, P, S and Zn in invertebrate samples using the collimator of 3 mm and 10 mm. For the assessment of the analytical protocol, the SRM 2976 Trace Elements in Mollusk produced and SRM 8415 Whole Egg Powder by the National Institute of Standards and Technology - NIST were also analyzed. After sampling by using pitfall traps, invertebrate were lyophilized, milled and transferred to polyethylene vials covered by XRF polyethylene. Analyses were performed at atmosphere lower than 30 Pa, varying voltage and electric current according to the chemical element to be analyzed. For comparison, Zn in the invertebrate material was also quantified by graphite furnace atomic absorption spectrometry after acid treatment (mixture of nitric acid and hydrogen peroxide) of samples have. Compared to the collimator of 10 mm, the SRM 2976 and SRM 8415 results obtained by the 3 mm collimator agreed well at the 95% confidence level since the E{sub n} Number were in the range of -1 and 1. Results from GFAAS were in accordance to the EDXRF values for composite samples. Therefore, determination of some chemical elements by EDXRF can be recommended for very small invertebrate samples (lower than 100 mg) with advantage of preserving the samples. (author)

  10. Sampling problems and the determination of mercury in surface water, seawater, and air

    International Nuclear Information System (INIS)

    Das, H.A.; van der Sloot, H.A.

    1976-01-01

    Analysis of surface water for mercury comprises the determination of both ionic and organically bound mercury in solution and that of the total mercury content of the suspended matter. Eventually, metallic mercury has to be determined too. Requirements for the sampling procedure are given. A method for the routine determination of mercury in surface water and seawater was developed and applied to Dutch surface waters. The total sample volume is 2500 ml. About 500 ml is used for the determination of the content of suspended matter and the total amount of mercury in the water. The sample is filtered through a bed of previously purified active charcoal at a low flow-rate. The main portion ca. 2000 ml) passes a flow-through centrifuge to separate the solid fraction. One liter is used to separate ''inorganic'' mercury by reduction, volatilization in an airstream and adsorption on active charcoal. The other liter is led through a column of active charcoal to collect all mercury. The procedures were checked with 197 Hg radiotracer both as an ion and incorporated in organic compounds. The mercury is determined by thermal neutron activation, followed by volatilization in a tube furnace and adsorption on a fresh carbon bed. The limit of determination is approximately equal to 1 ng 1 -1 . The rate of desorption from and adsorption on suspended material has been measured as a function of a pH of the solution for Hg +2 and various other ions. It can be concluded that only the procedure mentioned above does not disturb the equilibrium. The separation of mercury from air is obtained by suction of 1 m 3 through a 0.22 μm filter and a charcoal bed. The determination is then performed as in the case of the water samples

  11. Determination of trace elements in fisheries samples by instrumental neutron and photon activation analysis

    International Nuclear Information System (INIS)

    Chattopadhyay, A.; Ellis, K.M.; Nimalasiri Desilva, K.

    1979-01-01

    An instrumental neutron activation analysis (INAA) method has been developed for the simultaneous determination of trace concentrations of up to 23 elements in fisheries samples. The INAA method consists of irradiations of wet and lyophilized cod muscle and liver samples for three different periods at a flux density of 5x10 11 n.cm -2 .s -1 and subsequent measurements after four different decay periods using high-resolution Ge(Li) gamma-ray spectrometry. Concentrations of several essential and toxic elements have been determined. Loss of certain elements during lyophilization has been studied. Elemental distribution in muscles and livers as a function of the age of fish has been investigated. Precision and accuracy of the INAA method have been evaluated by analysing replicate samples, National Bureau of Standards' bovine liver standard reference material, and an intercalibration fish flour sample provided by the International Council for the Exploration of the Sea. A few fish samples have also been analysed by an alternative method, namely instrumental photon activation analysis (IPAA). Elemental concentrations determined by both INAA and IPAA methods are reported here. (author)

  12. Determination of 129I in large soil samples after alkaline wet disintegration

    International Nuclear Information System (INIS)

    Bunzl, K.; Kracke, W.

    1992-01-01

    Large soil samples (up to 500 g) can conveniently be disintegrated by hydrogen peroxide in an utility tank under alkaline conditions to determine subsequently 129 I by neutron activation analysis. Interfering elements such as Br are removed already before neutron irradiation to reduce the radiation exposure of the personnel. The precision of the method is 129 I also by the combustion method. (orig.)

  13. Gas-chromatographic quantitative determination of argon in air samples, by elimination of oxigen

    International Nuclear Information System (INIS)

    Sofronie, E.

    1982-08-01

    A method of gas-chromatographic quantitative determination of argon in air samples, by elimination of oxygen, is presented. Experiments were carried out in a static system. Conditions for the application of the method in dynamic systems are specified. Sensibility of the method: 5 10 -4 cm 3 Ar per cm 3 of air. (author)

  14. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil); Pozebon, Dirce [Instituto de Quimica, Universidade Federal do Rio Grande do Sul, UFRGS, 91501-970 Porto Alegre, RS (Brazil)], E-mail: dircepoz@iq.ufrgs.br; Mello, Paola A.; Flores, Erico M.M. [Departamento de Quimica, Universidade Federal de Santa Maria, UFSM, 97105-900 Santa Maria, RS (Brazil)

    2007-10-17

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO{sub 3}){sub 2} was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 {mu}g g{sup -1} of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

  15. DETERMINATION OF CHLOROPHEONIS, NITROPHENOIS AND METHYLPHENOIS IN GROUND-WATER SAMPLES USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

    Science.gov (United States)

    A high performance liquid chromatography (HPLC) method was developed to quantitatively determine phenolic compounds and their isomers in aqueous samples. The HPLC method can analyze a mixture of 15 contaminants in the same analytical run with an analysis time of 25 minutes. The...

  16. DETERMINATION OF CHLOROPHENOLS, NITROPHENOLS, AND METHYLPHENOLS IN GROUND-WATER SAMPLES USING HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

    Science.gov (United States)

    A high performance liquid chromatography (HPLC) method was developed to quantitatively determine phenolic compounds and their isomers in aqueous samples. The HPLC method can analyze a mixture of 15 contaminants in the same analytical run with an analysis time of 25 minutes. The...

  17. Determination of Technetium-99 in Environmental Samples by Solvent Extraction at Controlled Valence

    DEFF Research Database (Denmark)

    Chen, Q.J.; Aarkrog, A.; Dahlgaard, H.

    1989-01-01

    Distribution coefficients of technetium and ruthenium are determined under different conditions with CCl4, cyclohexanone, and 5% tri-isooctylamine (TIOA)/xylene. A method for analyzing 99Tc in environmental samples has been developed by solvent extraction in which the valences of technetium...

  18. Determination of total alpha index in samples of see water by coprecipitation method

    International Nuclear Information System (INIS)

    Suarez-Navarro, J.A.; Pujol, L.; Pozuelo, M.; Pablo, A. de

    1998-01-01

    An environmental radiological monitoring network in the Spanish sea waters was set up by CEDEX in 1993. Water radioactivity is determined quarterly in eleven sampling points along the Spanish coast. The gross alpha activity is one of the parameters to be determined. The usual method for monitoring the gross alpha activity includes sample evaporation to dryness on a disk and counting using ZnS(Ag) scintillation detector. Nevertheless, the gross alpha activity determination in saline waters, such as sea waters, is troublesome, because mass attenuation is high and a very small of water is needed (0.2 ml). The coprecipitation method allows to analyze 500 ml water samples, so the detection limit is reduced and sensitivity is improved. In this work, the coprecipitation method was used to determine the gross alpha activity in the radiological network of the Spanish coast sea waters during 1996 and 1997. Gross alpha activity was very homogenous. It averaged 0.0844±0.0086 Bq.1''1 and ranged from 0.062 to 0.102 Bq.1''1. In collaboration with CIEMAT a set of samples was analyzed, they averaged 0.0689±0.0074 Bq.1''1 and ranged from 0.056 to 0.082 Bq.1''1. (Author) 5 refs

  19. Determination of the plutonium contamination level in biological samples by liquid scintillation

    International Nuclear Information System (INIS)

    Willemot, J.M.; Verry, M.; Lataillade, G.

    1989-01-01

    Usual radiochemical processes are unable to carry out without delay the very large number of analyses as required in plutonium toxicology studies. Liquid scintillation is the best method to quickly determine plutonium contamination levels in most various samples (bone, organs,...) [fr

  20. Evaluation of sample preparation methods and optimization of nickel determination in vegetable tissues

    Directory of Open Access Journals (Sweden)

    Rodrigo Fernando dos Santos Salazar

    2011-02-01

    Full Text Available Nickel, although essential to plants, may be toxic to plants and animals. It is mainly assimilated by food ingestion. However, information about the average levels of elements (including Ni in edible vegetables from different regions is still scarce in Brazil. The objectives of this study were to: (a evaluate and optimize a method for preparation of vegetable tissue samples for Ni determination; (b optimize the analytical procedures for determination by Flame Atomic Absorption Spectrometry (FAAS and by Electrothermal Atomic Absorption (ETAAS in vegetable samples and (c determine the Ni concentration in vegetables consumed in the cities of Lorena and Taubaté in the Vale do Paraíba, State of São Paulo, Brazil. By means of the analytical technique for determination by ETAAS or FAAS, the results were validated by the test of analyte addition and recovery. The most viable method tested for quantification of this element was HClO4-HNO3 wet digestion. All samples but carrot tissue collected in Lorena contained Ni levels above the permitted by the Brazilian Ministry of Health. The most disturbing results, requiring more detailed studies, were the Ni concentrations measured in carrot samples from Taubaté, where levels were five times higher than permitted by Brazilian regulations.

  1. Determination of trace elements in paints by direct sampling graphite furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Bentlin, Fabrina R.S.; Pozebon, Dirce; Mello, Paola A.; Flores, Erico M.M.

    2007-01-01

    A direct sampling graphite furnace atomic absorption spectrometric (DS-GFAAS) method for the determination of Cd, Pb, Cr, Ni, Co and Cu in paints has been developed. Serigraphy, acrylic and tattoo paints were analysed. Approaches like pyrolysis and atomization temperatures, modifiers and sample mass introduced in the atomizer were studied. Quantification was performed using calibration curves measured with aqueous standard solutions pipetted onto the platform. The sample mass introduced in the graphite tube ranged from 0.02 to 8.0 mg. Palladium was used as modifier for Cd, Pb and Cu, while Mg(NO 3 ) 2 was used for Co. For Ni determination, the graphite platform was covered with carbon powder. The characteristic masses of Cd, Pb, Cr, Ni, Co and Cu were 1.4, 22.5, 7.9, 11.0, 9.6 and 12.5 pg, while the limits of detection were 0.0004, 0.001, 0.03, 0.22, 0.11 and 0.05 μg g -1 of Cd, Pb, Cr, Ni, Co and Cu, respectively. The accuracy was determined by comparison of the results with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GFAAS), using liquid sampling of digests. For matrix characterization, major and minor elements (Al, Mg, Ba, Ca, Cr, Cu, Pb, Sr, Ti and Mg) were determined by inductively coupled plasma optical emission spectrometry (ICP OES)

  2. Determinants of salivary evening alpha-amylase in a large sample free of psychopathology

    NARCIS (Netherlands)

    Veen, Gerthe; Giltay, Erik J.; Vreeburg, Sophie A.; Licht, Carmilla M. M.; Cobbaert, Christa M.; Zitman, Frans G.; Penninx, Brenda W. J. H.

    Objective: Recently, salivary alpha-amylase (sAA) has been proposed as a suitable index for sympathetic activity and dysregulation of the autonomic nervous system (ANS). Although determinants of sAA have been described, they have not been studied within the same study with a large sample size

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

    International Nuclear Information System (INIS)

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

    1993-11-01

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

  4. A contact method of determination of thermophysical properties of rocks from core samples

    International Nuclear Information System (INIS)

    Gavril'ev, R.I.

    1995-01-01

    The zone of the action of thermal disturbances around a circular heat source on the surface of a semi-infinite body is estimated with the aim of using contact methods of determination of thermophysical properties of materials from core samples

  5. Analytical determination of traced elements in concrete samples used in nuclear reactors of the European Community

    International Nuclear Information System (INIS)

    May, S.; Piccot, D.

    1984-01-01

    In reactor dismantling residual radioacting of concrete used, especially in biological shield can brought problems for treatment and disposal. Radioactivity of concrete from reactors can be forecasted if element content is known. Elements producing long life radionuclides are: chlorine, calcium nickel, cobalt, niobium, europium and samarium. Neutron activation analysis is used for determination of these elements whithout chemical separation for Ca, Co, Eu and Sm and with radiochemical separation for Cl, Ni and Nb. A lot of elements, less interesting are also determined by gamma spectrometry after irradiation. It was possible to determine 29 elements in 21 concrete samples from different European Community reactors

  6. Determination of heavy metals in solid emission and immission samples using atomic absorption spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Fara, M.; Novak, F. [EGU Prague, PLC, Bichovice, Prague (Czechoslovakia)

    1995-12-01

    Both flame and electrothermal methods of atomic absorption spectroscopy (AAS) have been applied to the determination of Al, As, Be, Ca, Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, TI, Se, V and Zn in emission and emission (deposition) samples decomposed in open PTFE test-tubes by individual fuming-off hydrofluoric, perchloroic and nitric acid. An alternative hydride technique was also used for As and Se determination and Hg was determined using a self-contained AAS analyzer. A graphite platform proved good to overcome non-spectral interferences in AAS-ETA. Methods developed were verified by reference materials (inc. NBS 1633a).

  7. Atomic absorption determination of ultratrace tellurium in rocks utilizing high sensitivity sampling systems

    International Nuclear Information System (INIS)

    Beaty, R.D.

    1973-01-01

    The sampling boat and the graphite furnace were shown to possess the required sensitivity to detect tellurium at ultratrace levels, in a variety of sample types, by atomic absorption. In the sampling boat approach, tellurium in sample solutions is chemically separated and concentrated by extraction into methyl isobutyl ketone before measurement. For samples exhibiting extraction interferences or excessively high background absorption, a preliminary separation of tellurium by coprecipitation with selenium is described. Using this technique, tellurium can be quantitatively detected down to 5 nanograms and linear response is observed to 100 nanograms. Relative standard deviations of better than 7 percent are achieved for 50 nanograms of tellurium. For samples that have a tellurium content below the detection limits of the sampling boat, the graphite furnace is used for atomization. By this method, as little as 0.07 nanograms of tellurium can be detected, and a precision of 1 percent relative standard deviation is achievable at the 5 nanogram level. A routinely applicable procedure was developed for determining tellurium in rocks, using the graphite furnace, after a hydrofluoric acid decomposition of the sample. Using this procedure, tellurium data were obtained on 20 different rocks, and the significance of this new information is discussed. (Diss. Abstr. Int., B)

  8. Hydrogen determination using secondary processes of recoil proton interaction with sample material

    International Nuclear Information System (INIS)

    Muminov, V.A.; Khajdarov, R.A.; Navalikhin, L.V.; Pardaev, Eh.

    1980-01-01

    Possibilities of hydrogen content determination in different materials according to secondary processes of interaction of recoil protons(irradiation in the field of fast neutrons) with sample material resulting in the appearance of characteristic X-ray irradiation are studied. Excitated irradiation is recorded with a detector placed in the protective screen and located at a certain distance from the object analyzed and neutron source. The method is tested taking as an example analysis of bromine-containing samples (30% Br, 0.5% H) and tungsten dioxide. The determination limit of hydrogen content constitutes 0.05% at confidence coefficient of 0.9. Neutron flux constituted 10 3 neutrons/cm 2 xs, the time of measurement being 15-20 minutes, the distance from the sample to the detector being 12-15 cm [ru

  9. Determination of thorium and uranium isotopes in the mining lixiviation liquor samples

    Energy Technology Data Exchange (ETDEWEB)

    Reis Júnior, Aluísio de Souza; Monteiro, Roberto Pellacani Guedes, E-mail: reisas@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2017-07-01

    The alpha spectrometric analysis refers to determination of thorium and uranium isotopes in the mining lixiviation liquor samples. The analytical procedure involves sample preparation steps for rare earth elements, thorium and uranium separation using selective etching with hydrofluoric acid and further radiochemical separation of these using TRU chromatographic resins (Eichrom Industries Inc. USA) besides electroplating of the isolated radionuclides. An isotopic tracer is used to determine the overall chemical yield and to ensure traceability to a national standard. The results are compared to results obtained for the same samples by Becquerel laboratory. We improved the method looking for reproducibility and isotopes isolation as required by alpha spectrometry and the method showing effective in analysis of mining liquor. (author)

  10. Determination of thorium and uranium isotopes in the mining lixiviation liquor samples

    International Nuclear Information System (INIS)

    Reis Júnior, Aluísio de Souza; Monteiro, Roberto Pellacani Guedes

    2017-01-01

    The alpha spectrometric analysis refers to determination of thorium and uranium isotopes in the mining lixiviation liquor samples. The analytical procedure involves sample preparation steps for rare earth elements, thorium and uranium separation using selective etching with hydrofluoric acid and further radiochemical separation of these using TRU chromatographic resins (Eichrom Industries Inc. USA) besides electroplating of the isolated radionuclides. An isotopic tracer is used to determine the overall chemical yield and to ensure traceability to a national standard. The results are compared to results obtained for the same samples by Becquerel laboratory. We improved the method looking for reproducibility and isotopes isolation as required by alpha spectrometry and the method showing effective in analysis of mining liquor. (author)

  11. Determination of traces of lithium in biological, environmental and metal samples by neutron activation analysis

    International Nuclear Information System (INIS)

    Yang, J.Y.; Tseng, C.L.; Lo, J.M.; Yang, M.H.

    1985-01-01

    Lithium in environmental, biological and metal samples was determined by neutron activation analysis via the 6 Li(n,α)T and 16 O(T,n) 18 F reactions. The samples were converted to aqueous solutions either by dissolution or by digestion and their aliquots were irradiated in a nuclear reactor for 2 h. The irradiated sample solution, was placed in a ZrO 2 column on which the 18 F nuclide was adsorbed. Most of the coexisting nuclides 24 Na, 82 Br, 38 Cl, 64 Cu, etc. were separated by elution with pH 1proportional3 solution. The column was subjected to a Ge(Li) detector for γ-ray spectrometry. The lithium content in the sample was estimated from the 18 F activity obtained. The matrix effect can be eliminated by either strong dilution of the samples in aqueous medium or by the method of standard addition. Lithium can be determined with high precision and accuracy in sub-ppm samples. (orig.) [de

  12. HPLC/DAD determination of rosmarinic acid in Salvia officinalis: sample preparation optimization by factorial design

    International Nuclear Information System (INIS)

    Oliveira, Karina B. de; Oliveira, Bras H. de

    2013-01-01

    Sage (Salvia officinalis) contains high amounts of the biologically active rosmarinic acid (RA) and other polyphenolic compounds. RA is easily oxidized, and may undergo degradation during sample preparation for analysis. The objective of this work was to develop and validate an analytical procedure for determination of RA in sage, using factorial design of experiments for optimizing sample preparation. The statistically significant variables for improving RA extraction yield were determined initially and then used in the optimization step, using central composite design (CCD). The analytical method was then fully validated, and used for the analysis of commercial samples of sage. The optimized procedure involved extraction with aqueous methanol (40%) containing an antioxidant mixture (ascorbic acid and ethylenediaminetetraacetic acid (EDTA)), with sonication at 45 deg C for 20 min. The samples were then injected in a system containing a C 18 column, using methanol (A) and 0.1% phosphoric acid in water (B) in step gradient mode (45A:55B, 0-5 min; 80A:20B, 5-10 min) with flow rate of 1.0 mL min−1 and detection at 330 nm. Using this conditions, RA concentrations were 50% higher when compared to extractions without antioxidants (98.94 ± 1.07% recovery). Auto-oxidation of RA during sample extraction was prevented by the use of antioxidants resulting in more reliable analytical results. The method was then used for the analysis of commercial samples of sage. (author)

  13. Determination of Slake Durability Index (Sdi) Values on Different Shape of Laminated Marl Samples

    Science.gov (United States)

    Ankara, Hüseyin; Çiçek, Fatma; Talha Deniz, İsmail; Uçak, Emre; Yerel Kandemir, Süheyla

    2016-10-01

    The slake durability index (SDI) test is widely used to determine the disintegration characteristic of the weak and clay-bearing rocks in geo-engineering problems. However, due to the different shapes of sample pieces, such as, irregular shapes displayed mechanical breakages in the slaking process, the SDI test has some limitations that affect the index values. In addition, shape and surface roughness of laminated marl samples have a severe influence on the SDI. In this study, a new sample preparation method called Pasha Method was used to prepare spherical specimens from the laminated marl collected from Seyitomer collar (SLI). Moreover the SDI tests were performed on equal size and weight specimens: three sets with different shapes were used. The three different sets were prepared as the test samples which had sphere shape, parallel to the layers in irregular shape, and vertical to the layers in irregular shape. Index values were determined for the three different sets subjected to the SDI test for 4 cycles. The index values at the end of fourth cycle were found to be 98.43, 98.39 and 97.20 %, respectively. As seen, the index values of the sphere sample set were found to be higher than irregular sample sets.

  14. HPLC/DAD determination of rosmarinic acid in Salvia officinalis: sample preparation optimization by factorial design

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Karina B. de [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Farmacia; Oliveira, Bras H. de, E-mail: bho@ufpr.br [Universidade Federal do Parana (UFPR), Curitiba, PR (Brazil). Dept. de Quimica

    2013-01-15

    Sage (Salvia officinalis) contains high amounts of the biologically active rosmarinic acid (RA) and other polyphenolic compounds. RA is easily oxidized, and may undergo degradation during sample preparation for analysis. The objective of this work was to develop and validate an analytical procedure for determination of RA in sage, using factorial design of experiments for optimizing sample preparation. The statistically significant variables for improving RA extraction yield were determined initially and then used in the optimization step, using central composite design (CCD). The analytical method was then fully validated, and used for the analysis of commercial samples of sage. The optimized procedure involved extraction with aqueous methanol (40%) containing an antioxidant mixture (ascorbic acid and ethylenediaminetetraacetic acid (EDTA)), with sonication at 45 deg C for 20 min. The samples were then injected in a system containing a C{sub 18} column, using methanol (A) and 0.1% phosphoric acid in water (B) in step gradient mode (45A:55B, 0-5 min; 80A:20B, 5-10 min) with flow rate of 1.0 mL min-1 and detection at 330 nm. Using this conditions, RA concentrations were 50% higher when compared to extractions without antioxidants (98.94 {+-} 1.07% recovery). Auto-oxidation of RA during sample extraction was prevented by the use of antioxidants resulting in more reliable analytical results. The method was then used for the analysis of commercial samples of sage. (author)

  15. {sup 222}Rn determination in water and brine samples using liquid scintillation spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Thiago C.; Oliveira, Arno H., E-mail: oliveiratco2010@gmail.com [Universidade Federal de Minas Gerais (DEN/UFMG), Belo Horizonte (Brazil). Departamento de Engenharia Nuclear; Monteiro, Roberto P.G.; Moreira, Rubens M., E-mail: rpgm@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN-CNEN-MG), Belo Horizonte, MG (Brazil)

    2017-07-01

    Liquid scintillation spectrometry (LSC) is the most common technique used for {sup 222}Rn determination in environmental aqueous sample. In this study, the performance of water-miscible (Ultima Gold AB) and immiscible (Optiscint) liquid scintillation cocktails has been compared for different matrices. {sup 241}Am, {sup 90}Sr and {sup 226}Ra standard solutions were used for LSC calibration. {sup 214}Po region was defined as better for both cocktails. Counting efficiency of 76 % and optimum PSA level of 95 for Ultima Gold AB cocktail, and counting efficiency of 82 % and optimum PSA level of 85 for Optiscint cocktail were obtained. Both cocktails showed similar results when applied for {sup 222}Rn activity determination in water and brine samples. However the Optiscint is recommended due to its quenching resistance. Limit of detection of 0.08 and 0.06 Bq l{sup -1} were obtained for water samples using a sample:cocktail ratio of 10:12 mL for Ultima Gold AB and Optiscint cocktails, respectively. Limit of detection of 0.08 and 0.04 Bq l{sup -1} were obtained for brine samples using a sample:cocktail ratio of 8:12 mL for Ultima Gold AB and Optiscint cocktails, respectively. (author)

  16. 222Rn determination in water and brine samples using liquid scintillation spectrometry

    International Nuclear Information System (INIS)

    Oliveira, Thiago C.; Oliveira, Arno H.

    2017-01-01

    Liquid scintillation spectrometry (LSC) is the most common technique used for 222 Rn determination in environmental aqueous sample. In this study, the performance of water-miscible (Ultima Gold AB) and immiscible (Optiscint) liquid scintillation cocktails has been compared for different matrices. 241 Am, 90 Sr and 226 Ra standard solutions were used for LSC calibration. 214 Po region was defined as better for both cocktails. Counting efficiency of 76 % and optimum PSA level of 95 for Ultima Gold AB cocktail, and counting efficiency of 82 % and optimum PSA level of 85 for Optiscint cocktail were obtained. Both cocktails showed similar results when applied for 222 Rn activity determination in water and brine samples. However the Optiscint is recommended due to its quenching resistance. Limit of detection of 0.08 and 0.06 Bq l -1 were obtained for water samples using a sample:cocktail ratio of 10:12 mL for Ultima Gold AB and Optiscint cocktails, respectively. Limit of detection of 0.08 and 0.04 Bq l -1 were obtained for brine samples using a sample:cocktail ratio of 8:12 mL for Ultima Gold AB and Optiscint cocktails, respectively. (author)

  17. Development of an automated method for determination of thorium in soil samples and aerosols

    International Nuclear Information System (INIS)

    Stuart, J.E.; Robertson, R.

    1986-09-01

    Methodology for determining trace thorium levels in a variety of sample types was further developed. Thorium in filtered water samples is concentrated by ferric hydroxide precipitation followed by dissolution and co-precipitation with lanthanum fluoride. Aerosols on glass fibre, cellulose ester, or teflon filters and solid soil and sediment samples are acid digested. Subsequently thorium is concentrated by lanthanum fluoride co-precipitation. Chemical separation and measurement is then done on a Technicon AA11-C autoanalyzer, using solvent extraction into thenoyltrifuoroacetone in kerosene followed by back extraction into 2 N H NO 3 , and colourometric measurement of the thorium arsenazo III complex. Chemical yields are determined by the addition of thorium-234 tracer using gamma-ray spectrometry. The sensitivities of the methods for water, aerosol and solid samples are approximately 1.0 μg/L, 0.5 μg/g and 1.0 μg/g respectively. At thorium levels about ten times the detection limit, accuracy is estimated to be ± 10% for liquids and aerosols and ± 15% for solid samples, and precision ± 5% for all samples

  18. Precise simultaneous determination of zirconium and hafnium in silicate rocks, meteorites and lunar samples. [Neutron reactions

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, P A; Garg, A N; Ehmann, W D [Kentucky Univ., Lexington (USA). Dept. of Chemistry

    1977-01-01

    A precise, sensitive and rapid analytical technique has been developed for the simultaneous determination of Zr and Hf in natural silicate matrices. The technique is based on radiochemical neutron activation analysis and employs a rapid fusion dissolution of the sample and simultaneous precipitation of the Zr-Hf pair with p-hydroxybenzene arsenic acid in an acidic medium. The indicator radionuclides, /sup 95/Zr and /sup 181/Hf, are counted and the /sup 95/Zr activity is corrected for the contribution from U fission. The chemical yields of the radiochemical separation are based on Hf carrier. The yield is determined by reactivation of the processed samples and standards with a /sup 252/Cf isotopic neutron source and by counting the 18.6 sec half-life sup(179m)Hf. The RNAA procedure for Zr and Hf has been shown to be precise and accurate for natural silicate samples, based on replicate analyses of samples containing Zr in the range of 1 ..mu..g/g to over 600 ..mu..g/g. The procedure is relatively rapid with a total chemical processing time of approximately 3 hours. At least 4 samples are processed simultaneously. Ten additional elements (Fe, Cr, Co, Sc, Eu, La, Lu, Ce, Th and Tb) can be determined by direct Ge(Li) spectrometry (INAA) on the samples prior to dissolution for the RNAA determination of Zr and Hf. Corrections for the U fission contribution can be made on the basis of the known U content or from the INAA Th content, based on the relatively constant natural Th/U ratio.

  19. Spectrophotometric determination of trace and ultratrace levels of boron in silicon and chlorosilane samples

    International Nuclear Information System (INIS)

    Chen, J.S.; Lin, H.M.; Yang, M.H.

    1991-01-01

    Spectrophotometric methods for the determination of boron in the low μg/g and ng/g range in high-purity silicon and dichloro- and trichlorosilanes were investigated in detail. The procedures established involve dissolution of silicon samples and the hydrolyzed products of chlorosilane samples in hydrofluoric acid-containing reagents followed by evaporation of the silicon matrix as H 2 SiF 6 . The boron retained in the treated sample solution was then determined by a spectrophotometric method using carminic acid as a chromatic reagent. Special effort has been paid to the control of the analytical blank and reproducible determination of boron. The results indicate that addition of mannitol and proper control of the evaporation process are effective in preventing volatilization of boron during the evaporation of silicon matrix and can thus attain high recovery of boron and reproducible analysis. Through meticulous control of the analytical blank and experimental conditions, the limit of detection for boron determination with the established method can be as low as ng/g levels. Application of the methods to the determination of boron in various stages of purification of silicon and trichlorosilane as well as in borophosphosilicate film was conducted. (orig.)

  20. Establishing adequate conditions for mercury determination in environmental samples by INAA

    International Nuclear Information System (INIS)

    Perez, Caroline; Santos, Eliane C.; Saiki, Mitiko

    2017-01-01

    Mercury (Hg) is a toxic element released into the environment mainly by anthropic activities. Consequently, the improvement for Hg determination in environmental samples is of great interest. Instrumental Neutron Activation Analysis (INAA) is considered an adequate method to determine several elements. However, Hg determination by INAA is often hampered by its volatility, which causes losses. The aim of this study was to establish adequate irradiation conditions for Hg determination in environmental samples by INAA. The following parameters were evaluated: irradiation time, container for irradiation and spectral gamma ray interferences. For the study, aliquots of certified reference materials (CRMs) and tree bark samples were irradiated together with Hg synthetic standard at the IEA-R1 nuclear research reactor. Gamma ray activities of 1 97 Hg and 203 Hg were measured in a spectrometer coupled to a HGe detector. Results obtained indicated that polyethylene capsules or envelopes can be used as container for sample irradiation and the Hg impurities in these containers were negligible. Irradiation time of one hour was adequate for Hg determination and in long irradiations of 8 h problems of spectral interference of 198 Au and 75 Se were observed. In addition, Hg loss during the irradiation of 1 h and after irradiation was not observed. Quality control of Hg results, obtained in the CRMs analyses using one hour of irradiation, indicated good precision and accuracy with |Z score| < 2. The experimental conditions established in this study were applied to tree bark samples. Detection limits for Hg of these analyses were between 0.14 and 1.9 μg g -1 . (author)

  1. Establishing adequate conditions for mercury determination in environmental samples by INAA

    Energy Technology Data Exchange (ETDEWEB)

    Perez, Caroline; Santos, Eliane C.; Saiki, Mitiko, E-mail: caroline.perez@usp.br [Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP), São Paulo, SP (Brazil)

    2017-07-01

    Mercury (Hg) is a toxic element released into the environment mainly by anthropic activities. Consequently, the improvement for Hg determination in environmental samples is of great interest. Instrumental Neutron Activation Analysis (INAA) is considered an adequate method to determine several elements. However, Hg determination by INAA is often hampered by its volatility, which causes losses. The aim of this study was to establish adequate irradiation conditions for Hg determination in environmental samples by INAA. The following parameters were evaluated: irradiation time, container for irradiation and spectral gamma ray interferences. For the study, aliquots of certified reference materials (CRMs) and tree bark samples were irradiated together with Hg synthetic standard at the IEA-R1 nuclear research reactor. Gamma ray activities of 1{sup 97}Hg and {sup 203}Hg were measured in a spectrometer coupled to a HGe detector. Results obtained indicated that polyethylene capsules or envelopes can be used as container for sample irradiation and the Hg impurities in these containers were negligible. Irradiation time of one hour was adequate for Hg determination and in long irradiations of 8 h problems of spectral interference of {sup 198}Au and {sup 75}Se were observed. In addition, Hg loss during the irradiation of 1 h and after irradiation was not observed. Quality control of Hg results, obtained in the CRMs analyses using one hour of irradiation, indicated good precision and accuracy with |Z score| < 2. The experimental conditions established in this study were applied to tree bark samples. Detection limits for Hg of these analyses were between 0.14 and 1.9 μg g{sup -1}. (author)

  2. Trace determination of uranium and thorium in biological samples by radiochemical neutron activation analysis

    International Nuclear Information System (INIS)

    Benedik, Ljudmila; Repinc, Urska; Byrne, Anthony R.; Stegnar, Peter

    2002-01-01

    Radiochemical neutron activation analysis (RNAA) is an excellent method for determining uranium and thorium; it offers unique possibilities for their ultratrace analysis using selective radiochemical separations. Regarding the favourably sensitive nuclear characteristics of uranium and of thorium with respect to RNAA, but the different half-lives of their induced nuclides, two different approaches were used. In the first approach uranium and thorium were determined separately via 239 U, 239 Np and 233 Pa. In the second approach these elements were 239 239 233 determined simultaneously in a single sample using U and/or Np and Pa. Isolation of induced nuclides was based on separation by extraction and/or anion exchange chromatography. Chemical yields were measured in each sample aliquot using added 235 U, 238 Np and 231 Pa radioisotopic tracers. (author)

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

    International Nuclear Information System (INIS)

    Popov, L.

    2016-01-01

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

  4. Simple Modification of Karl-Fischer Titration Method for Determination of Water Content in Colored Samples

    Science.gov (United States)

    Tavčar, Eva; Turk, Erika; Kreft, Samo

    2012-01-01

    The most commonly used technique for water content determination is Karl-Fischer titration with electrometric detection, requiring specialized equipment. When appropriate equipment is not available, the method can be performed through visual detection of a titration endpoint, which does not enable an analysis of colored samples. Here, we developed a method with spectrophotometric detection of a titration endpoint, appropriate for moisture determination of colored samples. The reaction takes place in a sealed 4 ml cuvette. Detection is performed at 520 nm. Titration endpoint is determined from the graph of absorbance plotted against titration volume. The method has appropriate reproducibility (RSD = 4.3%), accuracy, and linearity (R 2 = 0.997). PMID:22567558

  5. Simple Modification of Karl-Fischer Titration Method for Determination of Water Content in Colored Samples

    Directory of Open Access Journals (Sweden)

    Eva Tavčar

    2012-01-01

    Full Text Available The most commonly used technique for water content determination is Karl-Fischer titration with electrometric detection, requiring specialized equipment. When appropriate equipment is not available, the method can be performed through visual detection of a titration endpoint, which does not enable an analysis of colored samples. Here, we developed a method with spectrophotometric detection of a titration endpoint, appropriate for moisture determination of colored samples. The reaction takes place in a sealed 4 ml cuvette. Detection is performed at 520 nm. Titration endpoint is determined from the graph of absorbance plotted against titration volume. The method has appropriate reproducibility (RSD=4.3%, accuracy, and linearity (2=0.997.

  6. Simple modification of karl-Fischer titration method for determination of water content in colored samples.

    Science.gov (United States)

    Tavčar, Eva; Turk, Erika; Kreft, Samo

    2012-01-01

    The most commonly used technique for water content determination is Karl-Fischer titration with electrometric detection, requiring specialized equipment. When appropriate equipment is not available, the method can be performed through visual detection of a titration endpoint, which does not enable an analysis of colored samples. Here, we developed a method with spectrophotometric detection of a titration endpoint, appropriate for moisture determination of colored samples. The reaction takes place in a sealed 4 ml cuvette. Detection is performed at 520 nm. Titration endpoint is determined from the graph of absorbance plotted against titration volume. The method has appropriate reproducibility (RSD = 4.3%), accuracy, and linearity (R(2) = 0.997).

  7. Non-Uniform Sampling and J-UNIO Automation for Efficient Protein NMR Structure Determination.

    Science.gov (United States)

    Didenko, Tatiana; Proudfoot, Andrew; Dutta, Samit Kumar; Serrano, Pedro; Wüthrich, Kurt

    2015-08-24

    High-resolution structure determination of small proteins in solution is one of the big assets of NMR spectroscopy in structural biology. Improvements in the efficiency of NMR structure determination by advances in NMR experiments and automation of data handling therefore attracts continued interest. Here, non-uniform sampling (NUS) of 3D heteronuclear-resolved [(1)H,(1)H]-NOESY data yielded two- to three-fold savings of instrument time for structure determinations of soluble proteins. With the 152-residue protein NP_372339.1 from Staphylococcus aureus and the 71-residue protein NP_346341.1 from Streptococcus pneumonia we show that high-quality structures can be obtained with NUS NMR data, which are equally well amenable to robust automated analysis as the corresponding uniformly sampled data. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Determination of 90Sr in environmental samples with resonance ionization spectroscopy in collinear geometry

    International Nuclear Information System (INIS)

    Zimmer, K.; Stenner, J.; Kluge, H.J.; Lantzsch, J.; Monz, L.; Otten, E.W.; Passler, G.; Schwalbach, R.; Schwarz, M.; Stevens, H.; Wendt, K.; Herrmann, G.; Niess, S.; Trautmann, N.; Walter, K.; Bushaw, B.A.

    1994-01-01

    A new, fast technique for trace analysis of the radioactive isotopes 89 Sr and 90 Sr in environmental samples has been developed. Conventional mass separation is combined with resonance ionization spectroscopy in collinear geometry, which provides high selectivity and sensitivity. In addition, a chemical separation procedure for sample preparation has been developed. The described technique was used to determine the 90 Sr content in ∼ 870 m 3 air samples collected near Munich during and shortly after the Chernobyl reactor accident in April 1986. The content of 90 Sr was measured to be 1.4 mBq per m 3 , corresponding to 1.6 x 10 9 atoms of 90 Sr per sample. This value is in good agreement with the results of radiochemical measurements. (orig.)

  9. Determination of [sup 90]Sr in environmental samples with resonance ionization spectroscopy in collinear geometry

    Energy Technology Data Exchange (ETDEWEB)

    Zimmer, K. (Inst. fuer Physik, Univ. Mainz (Germany)); Stenner, J. (Inst. fuer Physik, Univ. Mainz (Germany)); Kluge, H.J. (Inst. fuer Physik, Univ. Mainz (Germany)); Lantzsch, J. (Inst. fuer Physik, Univ. Mainz (Germany)); Monz, L. (Inst. fuer Physik, Univ. Mainz (Germany)); Otten, E.W. (Inst. fuer Physik, Univ. Mainz (Germany)); Passler, G. (Inst. fuer Physik, Univ. Mainz (Germany)); Schwalbach, R. (Inst. fuer Physik, Univ. Mainz (Germany)); Schwarz, M. (Inst. fuer Physik, Univ. Mainz (Germany)); Stevens, H. (Inst. fuer Physik, Univ. Mainz (Germany)); Wendt, K. (Inst. fuer Physik, Univ. Mainz (Germany)); Herrmann, G. (Inst. fuer Kernchemie, Univ. Mainz (Germany)); Niess, S. (Inst. fuer Kernchemie, Univ. Mainz (Germany)); Trautmann, N. (Inst. fuer Kernchemie, Univ. Mainz (Germany)); Walter, K. (Inst. fuer Kernchemie, Univ. Mainz (Germany)); Bushaw, B.A. (Pacific Northwest Lab., Richland, WA (United States))

    1994-08-01

    A new, fast technique for trace analysis of the radioactive isotopes [sup 89]Sr and [sup 90]Sr in environmental samples has been developed. Conventional mass separation is combined with resonance ionization spectroscopy in collinear geometry, which provides high selectivity and sensitivity. In addition, a chemical separation procedure for sample preparation has been developed. The described technique was used to determine the [sup 90]Sr content in [approx] 870 m[sup 3] air samples collected near Munich during and shortly after the Chernobyl reactor accident in April 1986. The content of [sup 90]Sr was measured to be 1.4 mBq per m[sup 3], corresponding to 1.6 x 10[sup 9] atoms of [sup 90]Sr per sample. This value is in good agreement with the results of radiochemical measurements. (orig.)

  10. Determination of short-lived trace elements in environmental samples by neutron activation analysis

    International Nuclear Information System (INIS)

    Wardani, S.; Sihombing, E.; Hamzah, A.; Rochidi; Hery, P.S.; Hartaman, S.; Iman, J.

    1998-01-01

    Concentration of a short-lived trace elements in environmental samples were determined by neutron activation analysis, a counting loss often occur due to the high counting rate. A Pile-Up Rejecter (PUR) electric circuit was installed in counting a short-lived trace elements by a γ-ray spectrometer in order to correct a counting loss. The samples were irradiated for 30∼60 seconds at neutron flux of 3.5 x 10 12 n.cm -2 .s -1 , then the samples cooled for 120 second and counted for 180 second using this system. The nuclides concentration in the varieties environmental samples have a difference analysis result, was more accurate and precise, which the measured result would be 30 % more higher by PUR system than the result would be counted using a conventional γ-ray spectrometry method

  11. Determination of Different Metals in Steel Waste Samples Using laser Induced Breakdown Spectroscopy

    Directory of Open Access Journals (Sweden)

    A. H. Bakry

    2007-12-01

    Full Text Available Elemental analysis of waste samples collected from steel products manufacturing plant (SPS located at industrial city of Jeddah, Saudi-Arabia has been carried out using Laser Induced Breakdown Spectroscopy (LIBS. The 1064 nm laser radiations from a Nd:YAG laser at an irradiance of 7.6  1010 W cm –2 were used. Atomic emission spectra of the elements present in the waste samples were recorded in the 200 – 620 nm region. Elements such as Fe, W, Ti, Al, Mg, Ca, S, Mn, and Na were detected in these samples. Quantitative determination of the elemental concentration was obtained for these metals against certified standard samples. Parametric dependences of LIBS signal intensity on incident laser energy and time delay between the laser pulse and data acquisition system were also carried out.

  12. Cadmium and lead determination by ICPMS: Method optimization and application in carabao milk samples

    Directory of Open Access Journals (Sweden)

    Riza A. Magbitang

    2012-06-01

    Full Text Available A method utilizing inductively coupled plasma mass spectrometry (ICPMS as the element-selective detector with microwave-assisted nitric acid digestion as the sample pre-treatment technique was developed for the simultaneous determination of cadmium (Cd and lead (Pb in milk samples. The estimated detection limits were 0.09ìg kg-1 and 0.33ìg kg-1 for Cd and Pb, respectively. The method was linear in the concentration range 0.01 to 500ìg kg-1with correlation coefficients of 0.999 for both analytes.The method was validated using certified reference material BCR 150 and the determined values for Cd and Pb were 18.24 ± 0.18 ìg kg-1 and 807.57 ± 7.07ìg kg-1, respectively. Further validation using another certified reference material, NIST 1643e, resulted in determined concentrations of 6.48 ± 0.10 ìg L-1 for Cd and 21.96 ± 0.87 ìg L-1 for Pb. These determined values agree well with the certified values in the reference materials.The method was applied to processed and raw carabao milk samples collected in Nueva Ecija, Philippines.The Cd levels determined in the samples were in the range 0.11 ± 0.07 to 5.17 ± 0.13 ìg kg-1 for the processed milk samples, and 0.11 ± 0.07 to 0.45 ± 0.09 ìg kg-1 for the raw milk samples. The concentrations of Pb were in the range 0.49 ± 0.21 to 5.82 ± 0.17 ìg kg-1 for the processed milk samples, and 0.72 ± 0.18 to 6.79 ± 0.20 ìg kg-1 for the raw milk samples.

  13. HPLC determination of betamethasone and prednisolone in urine samples using monolithic column

    International Nuclear Information System (INIS)

    Abro, K.; Memon, N.; Bhanger, M.I.

    2011-01-01

    A fast and reliable HPLC method is reported for the separation and quantification of betamethasone and prednisolone in urine samples using Chromolith at the rate of Performance RP-l8e (100 mm x 4.6 mm) column. The separation and detection was achieved using an isocratic mobile phase composed of methanol:water (44:56 v/v) at 2.0 mL/min and wavelength of 254 nm. After successful optimisation of method parameters, it was applied to the urine samples. Solid phase extraction technique was used to clean the sample before analysis. The developed method was validated for the system suitability, precision and accuracy. The limits of defection for the prednisolone and betamethasone are 0.11 ng and 0.075 ng/10 macro L injection, respectively allowing their determination in human urine samples. Recovery for spiked urine samples was in the range of 97-103 %. The method offers a valuable alternative to the methodologies currently employed for separation and quantification of prednisolone and betamethasone in urine samples. A fast and reliable HPLC method is reported for the separation and quantification of betamethasone and prednisolone in urine samples using Chromolith at the rate of Performance RP-l8e (100 mm x 4.6 mm) column. The separation and detection was achieved using an isocratic mobile phase composed of methanol:water (44:56 v/v) at 2.0 mL/min and wavelength of 254 nm. After successful optimisation of method parameters, it was applied to the urine samples. Solid phase extraction technique was used to clean the sample before analysis. The developed method was validated for the system suitability, precision and accuracy. The limits of defection for the prednisolone and betamethasone are 0.11 ng and 0.075 ng/10 macro L injection, respectively allowing their determination in human urine samples. Recovery for spiked urine samples was in the range of 97-103 %. The method offers a valuable alternative to the methodologies currently employed for separation and quantification

  14. Application of activation analysis for determination of some elements in cassiterite samples

    International Nuclear Information System (INIS)

    Armelin, Maria Jose Aguirre

    1978-01-01

    This work consists in the development of an analytical method using activation by thermal neutrons for the determination of some minor elements and traces present in cassiterite (tin ore). This method was then applied to determine these elements in samples of cassiterite from different regions of Brazil. An analysis was made of the mineralogy characteristic of cassiterite as well as of the minerals most commonly associated with it. Four main types of interference were found to occur in the analysis by activation of trace elements in samples of cassiterite. The method involves the analysis without chemical separation for the determination of some elements and the analysis with chemical separation for the determination of other elements. The steps involved in both types of analysis are described. In the analysis with chemical separation the matrix element (tin) is separated by distillation in an H 2 SO 4 -HBr medium, after fusion of the ore with Na 2 O 2 . Arsine and antimony are determined in the distilled, whereas some lanthanide elements and uranium are determined in the distillation residue by separating them as a group by precipitation with lanthanum fluoride. A discussion on the precision, accuracy and sensibility of the method is also included. (author)

  15. Determination of geostatistically representative sampling locations in Porsuk Dam Reservoir (Turkey)

    Science.gov (United States)

    Aksoy, A.; Yenilmez, F.; Duzgun, S.

    2013-12-01

    Several factors such as wind action, bathymetry and shape of a lake/reservoir, inflows, outflows, point and diffuse pollution sources result in spatial and temporal variations in water quality of lakes and reservoirs. The guides by the United Nations Environment Programme and the World Health Organization to design and implement water quality monitoring programs suggest that even a single monitoring station near the center or at the deepest part of a lake will be sufficient to observe long-term trends if there is good horizontal mixing. In stratified water bodies, several samples can be required. According to the guide of sampling and analysis under the Turkish Water Pollution Control Regulation, a minimum of five sampling locations should be employed to characterize the water quality in a reservoir or a lake. The European Union Water Framework Directive (2000/60/EC) states to select a sufficient number of monitoring sites to assess the magnitude and impact of point and diffuse sources and hydromorphological pressures in designing a monitoring program. Although existing regulations and guidelines include frameworks for the determination of sampling locations in surface waters, most of them do not specify a procedure in establishment of monitoring aims with representative sampling locations in lakes and reservoirs. In this study, geostatistical tools are used to determine the representative sampling locations in the Porsuk Dam Reservoir (PDR). Kernel density estimation and kriging were used in combination to select the representative sampling locations. Dissolved oxygen and specific conductivity were measured at 81 points. Sixteen of them were used for validation. In selection of the representative sampling locations, care was given to keep similar spatial structure in distributions of measured parameters. A procedure was proposed for that purpose. Results indicated that spatial structure was lost under 30 sampling points. This was as a result of varying water

  16. Determination of chromium, cobalt and nickel in tissue samples by radiochemical activation analysis

    International Nuclear Information System (INIS)

    Reisell, A.; Lakomaa, E.L.

    1983-03-01

    A radiochemical neutron activation analysis method for the determination of chromium, cobalt and nickel in tissue samples. A radiochemical neutron activation analysis method for the determination of chromium, cobalt and nickel has been developed. The destruction device used consisted of a combined wet-ashing-distillation and ion-exchange system. Six samples could be treated at the same time. The samples were wet-ashed with H*L2SO*L4-H*L2O*L2 mixture. Volatile elements were distilled as bromide compounds with HBr*H-. The distillation residue in 8M HCl was passed through hydrated antimony pentoxide (HAP) in order to remove disturbing *H2*H4Na-activity and through a Dowex 2 x 8 column so as to retain *H6*H0Co (formed from *H5*H8Ni). Chromium was elutriated from the column and precipitated as Cr(OH)*L3 for the removal of disturbing *H3*H2P-activity. The standards and samples were treated in a similar manner each so that the yield determination is not necessarily needed. The yields by tracer experiments were (43 +- 5) % for Cr, (93 +- 4) % for Co and (88 +- 14) % for Ni. The precision and accuracy of the method were studied by using reference materials of the National Bureau of Standards (NBS) and the International Atomic Energy Agency (IAEA)

  17. Porosity determination of alumina and boron carbide ceramic samples by gamma ray transmission

    International Nuclear Information System (INIS)

    Moreira, Anderson Camargo; Appoloni, Carlos Roberto

    2009-01-01

    The aim of this work is to apply the Gamma Ray Transmission (GRT), a non destructive technique, for structural characterization of ceramic samples. With this technique, the porosity of Alumina (Al 2 O 3 ) and Boron Carbide (B 4 C) ceramic samples, in tablet format, was determined. The equipment employed is constituted by a 241 Am gamma ray source (59.6 keV and 100mCi), a 2''x2'' diameter NaI (Tl) scintillation detector coupled to a standard gamma ray transmission electronic and a micrometric and automated table for sample movement. The porosity profile of the samples shows a homogeneous porosity distribution, within the spatial resolution of the employed transmission system. The mean porosity determined for Al 2 O 3 and B 4 C were 17.8±1.3% and 3.87±0.43%, respectively. A statistical treatment of these results was performed and showed that the mean porosity values determinate by the GRT are the same as those supplied by the manufacturer. (author)

  18. Determination of Sr-90 in milk samples from the study of statistical results

    Directory of Open Access Journals (Sweden)

    Otero-Pazos Alberto

    2017-01-01

    Full Text Available The determination of 90Sr in milk samples is the main objective of radiation monitoring laboratories because of its environmental importance. In this paper the concentration of activity of 39 milk samples was obtained through radiochemical separation based on selective retention of Sr in a cationic resin (Dowex 50WX8, 50-100 mesh and subsequent determination by a low-level proportional gas counter. The results were checked by performing the measurement of the Sr concentration by using the flame atomic absorption spectroscopy technique, to finally obtain the mass of 90Sr. From the data obtained a statistical treatment was performed using linear regressions. A reliable estimate of the mass of 90Sr was obtained based on the gravimetric technique, and secondly, the counts per minute of the third measurement in the 90Sr and 90Y equilibrium, without having to perform the analysis. These estimates have been verified with 19 milk samples, obtaining overlapping results. The novelty of the manuscript is the possibility of determining the concentration of 90Sr in milk samples, without the need to perform the third measurement in the equilibrium.

  19. Optimised method for the routine determination of Technetium-99 in environmental samples by liquid scintillation counting

    International Nuclear Information System (INIS)

    Wigley, F.; Warwick, P.E.; Croudace, I.W.; Caborn, J.; Sanchez, A.L.

    1999-01-01

    A method has been developed for the routine determination of 99 Tc in a range of environmental matrices using 99m Tc (t 1/2 =6.06 h) as an internal yield monitor. Samples are ignited stepwise to 550C and the 99 Tc is extracted from the ignited residue with 8 M nitric acid. Many contaminants are co-precipitated with Fe(OH) 3 and the Tc in the supernatant is pre-concentrated and further purified using anion exchange chromatography. Final separation of Tc from Ru is achieved by extraction of Tc into 5% tri-n-octylamine in xylene from 2 M sulphuric acid. The xylene fraction is mixed directly with a commercial liquid scintillant cocktail. The chemical yield is determined through the measurement of 99m Tc by gamma spectrometry and the 99 Tc activity is measured using liquid scintillation counting after a further two weeks to allow decay of the 99m Tc activity. Typical recoveries for this method are in the order 70-95%. The method has a detection limit of 1.7 Bq kg -1 based on a 2 h count time and a 10 g sample size. The chemical separation for 24 samples of sediment or marine biota can be completed by one analyst in a working week. A further week is required to allow the samples to decay before determination. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  20. Application of the neutron activation analysis method to the multielemental determination of food samples

    International Nuclear Information System (INIS)

    Maihara, V.A.

    1985-01-01

    The thermal neutron activation analysis method was applied to the determination of elements present at low concentrations and trace levels in samples of bread and milk powder using non-destructive analyses were based on gamma ray spectrometric measurements of samples and standards irradiated for periods which varied from some minutes to eight hours in a thermal neutron flux of about 10 12 n cm -2 s -1 . The concentrations obtained for milk powder were compared with the data obtained by other autors from different contries. For the bread, that comparison was not possible, because data about trace analysis in bread samples were not found. Besides, the results obtained for the various brands of bread and milk by means of non destructive and destructive analyses were compared using Student's t criterion. Some basic considerations about 'Detection Limit' were done, mainly in relation to its application in the technique used in the present work. The detection and determination limits of the trace elements analysed by destructive and non destructive techniques in bread and milk powder samples were determined using the Currie and Girardi methods. The precision of the analyses and the results obtained for the detection limits of the analysed trace elements are discussed. (Author) [pt

  1. Determination of lead in rice grains by solid sampling HR-CS GFAAS.

    Science.gov (United States)

    Gunduz, Sema; Akman, Suleyman

    2013-12-01

    A study was performed for the determination of lead in rice grains directly by solid sampling high resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GFAAS) without digesting sample. The effects of sample amount, pyrolysis/atomization temperatures on the determination of lead in rice were investigated and optimized using a certificated rice flour. The lead concentrations were determined applying 800 °C of pyrolysis and 1800 °C of atomization temperatures without modifier. LOD (N=10, 3σ) and characteristic mass were 2.3 μg kg(-1) and 8.1 pg, respectively. The certified lead value of a rice flour CRM was found in its uncertainity limits. The lead contents of various rice samples obtained from markets in Turkey were between 0.009 and 0.162 mg kg(-1) which are in acceptable range. The average lead concentrations in various rice grains taken from the same package were significantly different from each other. Copyright © 2013 Elsevier Ltd. All rights reserved.

  2. Characterizing Terrestrial Exoplanets

    Science.gov (United States)

    Meadows, V. S.; Lustig-Yaeger, J.; Lincowski, A.; Arney, G. N.; Robinson, T. D.; Schwieterman, E. W.; Deming, L. D.; Tovar, G.

    2017-11-01

    We will provide an overview of the measurements, techniques, and upcoming missions required to characterize terrestrial planet environments and evolution, and search for signs of habitability and life.

  3. Determination of acrolein, ethanol, volatile acidity, and copper in different samples of sugarcane spirits

    Directory of Open Access Journals (Sweden)

    José Masson

    2012-09-01

    Full Text Available Seventy-one samples of sugarcane spirits from small and average size stills produced in the northern and southern Minas Gerais (Brazil were analyzed for acrolein using HPLC (High Performance Liquid Chromatography. Ethanol and copper concentrations and volatile acidity were also determined according to methods established by the Ministry of Agriculture, Livestock and Supply (MAPA. A total of 9.85% of the samples tested showed levels of acrolein above the legal limits, while the copper concentrations of 21.00% of the samples and the volatile acidity of 8.85% of the samples were higher than the limits established by the Brazilian legislation. The concentration of acrolein varied from 0 to 21.97 mg.100 mL-1 of ethanol. However, no significant difference at 5% of significance was observed between the samples produced in the northern and southern Minas Gerais. The method used for determination of acrolein in sugarcane spirits involved the formation of a derivative with 2,4-dinitrophenylhydrazine (2,4-DNPH and subsequent analysis by HPLC.

  4. Determination of different contaminants in selective drinking water samples collected from Peshawar valley area

    International Nuclear Information System (INIS)

    Ihsanullah; Khan, M.; Khattak, T.N.; Sattar, A.

    1999-01-01

    Among the pollutants carried through sewage, industrial effluents, fertilizers, pesticides; heavy metals and various pathogenic bacteria are directly related to human/animal diseases. Samples of drinking water were collected from different locations, in the Peshawar area. Cadmium, lead and copper levels in these samples were determined by potentiometric stripping analysis (PSA). The data indicated wide variation in the concentration of these heavy metals. Variation in results is discussed on the basis of some possible sources of contamination. The concentration of cadmium and lead in all the samples was higher compared to the values given in the guideline of World Health Organization (WHO) for drinking water. Copper was below the detection limit in majority of the samples. The values of Cd, Pb and Cu were in the range of 0.023-2.75, 0.025-1.88 and 0-0.67 mg/1 respectively. Various physical quality indices (ph, electrical conductivity and total solids) and pathogenic bacteria (E. coli and total coliforms) were also determined in water samples. Most of the drinking waters was found contaminated with higher levels of Cd and Pb and pathogenic bacteria and hence, considered unfit for drinking purposes. (author)

  5. A very sensitive LSC procedure to determine Ni-63 in environmental samples, steel and concrete

    International Nuclear Information System (INIS)

    Scheuerer, C.; Schupfner, R.; Schuettelkopf, H.

    1995-01-01

    This procedure to determine Ni-63 contributes to a safe and economically reasonable decommissioning of nuclear power plants. Co-60, Fe-55 and Ni-63 are the most abundant long-lived radionuclides associated with contaminated piping, hardware and concrete for a period of several decades of years after shutdown. Samples are carefully ashed leached, or dissolved by suitable mixtures of acids. The analysis starts with the absorption Ni 2+ on the chelating resin CHELEX 100. The next purification steps include an anionic exchange column and a precipitation as Ni-dimethyl-glyoxime, which is extracted into chloroform. After reextraction with sulfuric acid the solution containing Ni 2+ is mixed with a scintillation cocktail and counted in an anticoincidence shielded LSC. The decontamination factors are determined for all important artificially and naturally occurring radionuclides ranging form above 10 4 to 10 9 . The chemical yield adopts a value of (95±5)%. Up to maximum sample amounts of 0.4 g steel, 5 g concrete and about 100 g of environmental samples the detection limits are about 5 mBq per sample or 12 mBq/g steel, 1 mBq/g concrete and 0.05 mBq/g environmental sample at a counting time of 1000 minutes. (author) 16 refs.; 2 figs.; 2 tabs

  6. The Determination of the Biochemical Properties of Some Monofloral Honey Samples Produced across Turkey

    Directory of Open Access Journals (Sweden)

    Aziz Gül

    2016-12-01

    Full Text Available This study was conducted in 2013 to determine the biochemical properties of 10 different monofloral honey types produced across Turkey. For the study, honey samples were obtained from beekeepers and the identity and relative percentage of dominant pollen types in samples was determined through microscopic analysis. Pollen analysis revealed that honey types chaste tree (Vitex agnus-castus and sunflower (Helianthus annuus contained high proportions of each respective pollen type. These proportions reached as high as 86%, while other honey types such as Anason had low Anasom pollen content, occurring at 45% in whole honey samples. Biochemical analysis revealed that the average honey sample quality characteristics were as followings: ash 0.37±0.04, electricity conductivity 0.79±0.07 mS/cm, moisture 19.15±0.09%, pH 3.97±0.02, acidity 29.07±0.39 meq/kg, hydroxymethylfurfural (HMF, 6.17±0.76 mg/kg, diastase 22.05±0.00, invert sugar 69.72±0.49% and sucrose 2.90±0.30%. These analyses confirmed that honey samples met standards outlined by the Turkish Food Codex Honey Standard, European Union Honey Standard and Codex Standards respectively.

  7. Microwave-assisted extraction and mild saponification for determination of organochlorine pesticides in oyster samples.

    Science.gov (United States)

    Carro, N; García, I; Ignacio, M-C; Llompart, M; Yebra, M-C; Mouteira, A

    2002-10-01

    A sample-preparation procedure (extraction and saponification) using microwave energy is proposed for determination of organochlorine pesticides in oyster samples. A Plackett-Burman factorial design has been used to optimize the microwave-assisted extraction and mild saponification on a freeze dried sample spiked with a mixture of aldrin, endrin, dieldrin, heptachlor, heptachorepoxide, isodrin, transnonachlor, p, p'-DDE, and p, p'-DDD. Six variables: solvent volume, extraction time, extraction temperature, amount of acetone (%) in the extractant solvent, amount of sample, and volume of NaOH solution were considered in the optimization process. The results show that the amount of sample is statistically significant for dieldrin, aldrin, p, p'-DDE, heptachlor, and transnonachlor and solvent volume for dieldrin, aldrin, and p, p'-DDE. The volume of NaOH solution is statistically significant for aldrin and p, p'-DDE only. Extraction temperature and extraction time seem to be the main factors determining the efficiency of extraction process for isodrin and p, p'-DDE, respectively. The optimized procedure was compared with conventional Soxhlet extraction.

  8. Method of separate determination of high-ohmic sample resistance and contact resistance

    Directory of Open Access Journals (Sweden)

    Vadim A. Golubiatnikov

    2015-09-01

    Full Text Available A method of separate determination of two-pole sample volume resistance and contact resistance is suggested. The method is applicable to high-ohmic semiconductor samples: semi-insulating gallium arsenide, detector cadmium-zinc telluride (CZT, etc. The method is based on near-contact region illumination by monochromatic radiation of variable intensity from light emitting diodes with quantum energies exceeding the band gap of the material. It is necessary to obtain sample photo-current dependence upon light emitting diode current and to find the linear portion of this dependence. Extrapolation of this linear portion to the Y-axis gives the cut-off current. As the bias voltage is known, it is easy to calculate sample volume resistance. Then, using dark current value, one can determine the total contact resistance. The method was tested for n-type semi-insulating GaAs. The contact resistance value was shown to be approximately equal to the sample volume resistance. Thus, the influence of contacts must be taken into account when electrophysical data are analyzed.

  9. System to determine present elements in oily samples; Sistema para determinar elementos presentes en muestras oleosas

    Energy Technology Data Exchange (ETDEWEB)

    Mendoza G, Y

    2004-11-01

    In the Chemistry Department of the National Institute of Nuclear Investigations of Mexico, dedicated to analyze samples of oleaginous material and of another origin, to determine the elements of the periodic table present in the samples, through the Neutron activation analysis technique (NAA). This technique has been developed to determine majority elements in any solid, aqueous, industrial and environmental sample, which consists basically on to irradiate a sample with neutrons coming from the TRIGA Mark III reactor and to carry out the analysis to obtain those gamma spectra that it emits, for finally to process the information, the quantification of the analysis it is carried out in a manual way, which requires to carry out a great quantity of calculations. The main objective of this project is the development of a software that allows to carry out the quantitative analysis of the NAA for the multielemental determination of samples in an automatic way. To fulfill the objective of this project it has been divided in four chapters: In the first chapter it is shortly presented the history on radioactivity and basic concepts that will allow us penetrate better to this work. In the second chapter the NAA is explained which is used in the sample analysis, the description of the process to be carried out, its are mentioned the characteristics of the used devices and an example of the process is illustrated. In the third chapter it is described the development of the algorithm and the selection of the programming language. The fourth chapter it is shown the structure of the system, the general form of operation, the execution of processes and the obtention of results. Later on the launched results are presented in the development of the present project. (Author)

  10. New developments in the extraction and determination of parabens in cosmetics and environmental samples. A review

    International Nuclear Information System (INIS)

    Ocaña-González, Juan Antonio; Villar-Navarro, Mercedes; Ramos-Payán, María; Fernández-Torres, Rut; Bello-López, Miguel Angel

    2015-01-01

    Highlights: • The analysis of parabens in cosmetics and environmental samples is reviewed. • Literature in this field from 1980 to 2003 is briefly discussed. • Determination and extraction methods in the last decade are discussed in-depth. - Abstract: Parabens are a family of synthetic esters of p-hydroxibenzoic acid widely used as preservatives in cosmetics and health-care products, among other daily-use commodities. Recently, their potential endocrine disrupting effects have raised concerns about their safety and their potential effects as emerging pollutants, leading to the regulation of the presence of parabens in commercial products by national and trans-national organizations. Also, this has led to an interest in developing sensible and reliable methods for their determination in environmental samples, cosmetics and health-care products. This paper is a comprehensive up-to-date review of the literature concerning the determination of parabens in environmental samples and cosmetic and health-care products. A brief revision of the literature concerning the traditional determination of parabens (1980–2003) is included, followed by an in-depth revision of the recent developments in both measurement and extraction methods for parabens in the last years (2003–2013). Finally, possible future perspectives in this field are proposed

  11. Multielemental determination in Citrus spp bee honey samples by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Favaro, D.I.T.; Vasconcellos, M.B.A.; Pamplona, B.

    1990-07-01

    Recently interest has grown in the determination of the concentration of inorganic chemical elements in honey bee samples, due its utilization as indicator of environmental pollution in several countries of Europe. In the present work, a method was developed to determine some essential and potentially inorganic elements in honey bee samples by intrumental neutrons activation analysis followed by high resolution gamma ray spectrometry. The honey samples were neutron irradiated during differents times at the nuclear research reactor IEA-Rl of the IPEN-CNEN/SP. The elements Na, Cl, K, Mg and Mn were determined using irradiations of 30 minutes under a thermal neutron flux of 10 12 n.cm -2 .s -1 . With 16 hours of irradiation under a flux of 10 13 n.cm -2 .s -1 and different cooling times, the elements Br, Ca, Au, Sb, Cs, Rb, Zn, Sc, Fe, Co and La were determined. The concentration of the analyzed elements ranged from ng/g to mg/g. In the future, different kinds of bee honey will be analyzed and the characteristic chemical composition of each one will be established. Based on these elemental concentration data, the relationship between the mineral composition of bee honey and its geographical origin can be studied. (author) [pt

  12. New developments in the extraction and determination of parabens in cosmetics and environmental samples. A review

    Energy Technology Data Exchange (ETDEWEB)

    Ocaña-González, Juan Antonio; Villar-Navarro, Mercedes [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain); Ramos-Payán, María [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain); Department of Analytical Chemistry, Lineberguer Cancer Center, The University of North Carolina at Chapel Hill, NC (United States); Fernández-Torres, Rut [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain); Research Centre of Health and Environment (CYSMA), University of Huelva (Spain); Bello-López, Miguel Angel, E-mail: mabello@us.es [Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Sevilla, c/Prof. García González, s/n. 41012 Seville (Spain)

    2015-02-09

    Highlights: • The analysis of parabens in cosmetics and environmental samples is reviewed. • Literature in this field from 1980 to 2003 is briefly discussed. • Determination and extraction methods in the last decade are discussed in-depth. - Abstract: Parabens are a family of synthetic esters of p-hydroxibenzoic acid widely used as preservatives in cosmetics and health-care products, among other daily-use commodities. Recently, their potential endocrine disrupting effects have raised concerns about their safety and their potential effects as emerging pollutants, leading to the regulation of the presence of parabens in commercial products by national and trans-national organizations. Also, this has led to an interest in developing sensible and reliable methods for their determination in environmental samples, cosmetics and health-care products. This paper is a comprehensive up-to-date review of the literature concerning the determination of parabens in environmental samples and cosmetic and health-care products. A brief revision of the literature concerning the traditional determination of parabens (1980–2003) is included, followed by an in-depth revision of the recent developments in both measurement and extraction methods for parabens in the last years (2003–2013). Finally, possible future perspectives in this field are proposed.

  13. 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)

  14. Radiometric sampling of bucked copper-nickel ores for determining chemical composition

    International Nuclear Information System (INIS)

    Komlev, V.N.; Eliseev, G.I.

    1978-01-01

    Presented are the results and the technique of experimental-methodical works on radiometric sampling of bucked copper-nickel ores for determining chemical composition with their selection and analysis by the neutron-gamma method and by the gamma-gamma method. The error is estimated according to the chosen conditions of sampling. It is found that the gamma-gamma method being more rapid but less accurate is applied for rapid control of ore current, whereas the neutron-gamma method is applied for quality control of ores extracted

  15. Determination of phosphorus in biological samples by thermal neutron activation followed by β--counting

    International Nuclear Information System (INIS)

    Weginwar, R.G.; Samudralwar, D.L.; Garg, A.N.

    1989-01-01

    Phosphorus was determined using the β - emitter 32 P by instrumental neutron activation analysis (INAA) in several NBS and IAEA standards, and in samples of biological origin such as human and animal blood, cancerous tissue, edible plant leaves, diets, milk samples, etc. The method involves thermal neutron irradiation (for 2-10 h in a reactor) followed by β - counting on an end-window gas flow proportional counter using aluminium filter. The results are within ±10% of the certified values in most cases. (author) 29 refs.; 3 tabs

  16. Phosphorus determination in bone samples by activation analysis using fast neutrons

    International Nuclear Information System (INIS)

    Madi Filho, T.; Cunha, I.I.L.

    1992-01-01

    In this report, the phosphorus determination in animal bone samples was made by means of the irradiation of samples using 14 MeV neutron generator (Van de Graaff accelerator). Induced radiation in irradiated material was measured using a NaI(Tl) detector. The method was tested in a IAEA certified standard, being obtained the values of 15,48% and 15,75%. The content of phosphorus was obtained by using two different calculating methods. Based on the experiments performed it was possible to establish a method of phosphorus analysis in bone using the Van de Graaff accelerator. (author)

  17. 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.

  18. Determining the number of samples required for decisions concerning remedial actions at hazardous waste sites

    International Nuclear Information System (INIS)

    Skiles, J.L.; Redfearn, A.; White, R.K.

    1991-01-01

    An important consideration for every risk analyst is how many field samples should be taken so that scientifically defensible decisions concerning the need for remediation of a hazardous waste site can be made. Since any plausible remedial action alternative must, at a minimum, satisfy the condition of protectiveness of human and environmental health, we propose a risk-based approach for determining the number of samples to take during remedial investigations rather than using more traditional approaches such as considering background levels of contamination or federal or state cleanup standards

  19. An XRF method for the determination of gold and silver in carbon samples from CIP plants

    International Nuclear Information System (INIS)

    Baumgartner, F.C.; Jackson, B.E.; Van Zyl, C.

    1985-01-01

    The improvement in the recovery of gold, utilizing the carbon-in-pulp (CIP) and carbon-in-leach (CIL) processes, are major developments which have taken place in the South African gold Mining industry in recent years. In addition to gold, many other elements are either adsorbed onto or physically trapped by the carbon granules during the CIP and CIL processes. X-ray fluorescence, a technique which offers the possibility of a minimum of sample preparation, is used to determine gold and silver in carbon samples from CIP plants

  20. Adsorptive stripping voltammetric determination of trace amounts of lead in environmental water samples with complicated matrix

    Directory of Open Access Journals (Sweden)

    Grabarczyk M.

    2013-04-01

    Full Text Available A sensitive, simple and fast adsorptive stripping voltammetric procedure for trace determination of lead in environmental water samples has been developed. The method is based on adsorptive accumulation of the Pb(II-cupferron complex onto a hanging mercury drop electrode, followed by the reduction of the adsorbed species by a voltammetric scan using differential pulse modulation. The interference from surface active substances was eliminated by adsorption of interferents onto an Amberlite XAD-16 resin. Optimumconditions for removing the surfactants by mixing the analysed sample with resin were evaluated. The accuracy of the method was tested by analyzing certified reference material (SPS-WW1 Waste Water.

  1. Application of neutron activation analysis to trace element determinations in lung samples

    International Nuclear Information System (INIS)

    Rocero, Sizue Ota

    1992-01-01

    The purpose of this work was to apply the instrumental neutron activation analysis method to determine trace elements in lung samples from smokers and non smokers. Samples of lung tissues and lymph nodes from pulmonary hilum analyzed were collected from autopsies by researchers from the Medicine College of the University of Sao Paulo, SP, Brazil. Adequate conditions for preparation and analysis of samples were previously established. The preparation of samples consisted of homogenization, lyophilization and sterilization in 60 Co source. The samples and standards were irradiated in the IEA-R1 reactor under thermal neutron flux of 3.7 x 10 11 n.cm -2 .s -1 for 30 min to determine Cl, K, Mn and Na and for 16 h under flux of 10 19 n.cm -2 .s -1 for the determination of Au, Br, Ce, Co, Cr, Cs, Eu, Fe, Hf, La, Rb, Sb, Sc, Se, Th and Zn. The counting were carried out with a hiperpure (ge) detector connected to a 4096 channels analyzer and a microcomputer. the results obtained for lung sample analyses indicated a good reproducibility of the method for most of the elements determined with relative standard deviations lower than 10.5%. The accuracy of the method was evaluated by analyzing reference materials such as IAEA Animal Muscle H-4, NIST Bovine Liver 1577a, IUPAC Bowen's Kale and NIES Vehicle Exhaust Particulates. The results obtained from these analyzes agreed with the values of the literature for several elements with relative errors less than 20%. Less precise and accurate results were obtained for elements with concentrations at the Mup/Kg levels. Elemental concentrations obtained in the lung tissue analyses were within the range of reference values for normal subjects presented in the literature, except for the Cl concentrations for non smokers, Hf in both groups and Sb for the smokers. By comparing results obtained for lung samples from smokers and non smokers, the concentrations of Ce, Cr and Sb were higher in lungs from smokers and the others elements were

  2. Solid-phase extraction and determination of trace elements in environmental samples using naphthalene adsorbent

    International Nuclear Information System (INIS)

    Pourreza, N.

    2004-01-01

    Naphthalene co-precipitated with quaternary ammonium salt such as tetraoctyl ammonium bromide and methyltrioctyl ammonium chloride have been used as adsorbent for solid phase extraction of metal ions such as Hg, Cd and Fe. The metal ions are retained on the adsorbent in a column as their complexes with suitable ligands and eluted by an eluent before instrumental measurements. The optimization of the procedures for solid phase extraction and consequent determination of trace elements and application to environmental samples especially water samples will be discussed. (author)

  3. Determination of elements in industrial waste sample and TENORM using XRF Technique in Nuclear Malaysia

    International Nuclear Information System (INIS)

    Paulus, W.; Sarimah Mahat; Meor Yusoff Meor Sulaiman

    2011-01-01

    Industrial waste such as aluminium dross and TENORM waste, oil sludge has been used as sample in this research. Determination of main elements by using X-Ray Fluorescence (XRF) in Material Technology Group, Malaysian Nuclear Agency. Results shows that main elements in these samples, aluminium and silicon, respectively. Thereby, this research shows that XRF can be considered as one of the techniques that can be used in waste characterization and furthermore, it can help researchers and engineer in the research related to waste treatment especially radioactive waste. (author)

  4. Determination of Na, Cl, Ca, Mg, Mn and K in milk samples by activation analysis

    International Nuclear Information System (INIS)

    Kira, Carmen S.; Maihara, Vera A.

    2000-01-01

    In the present work cow milk samples distributed for Sao Paulo government institutions, by means of the 'Viva leite' programme, have been monitored. The concentrations of Ca, Cl, K, Mg, Mn and Na were determined in five milk samples and in three different kinds of commercial powder milk, by instrumental neutron activation. For quality control, the reference materials NIST whole milk powder and non fat milk powder were analysed. The results obtained are in the range of the concentrations mentioned in the literature for these elements. (author)

  5. Determination of burial dose in incompletely bleached fluvial samples using single grains of quartz

    DEFF Research Database (Denmark)

    Thomsen, Kristina Jørkov; Murray, A.S.; Bøtter-Jensen, Lars

    2007-01-01

    We determine the burial dose in three known-age incompletely bleached fluvial samples using single grains of quartz. Estimation of burial dose in incompletely bleached samples requires that the characteristics of the well-bleached part of the distribution are known in order to distinguish between...... well-bleached and poorly bleached grains. It is especially important to investigate if the uncertainties assigned to individual estimates of dose adequately describe the observed variability in well-bleached dose distributions. We investigate this by quantifying the overdispersion in laboratory-bleached...

  6. Determining mutant spectra of three RNA viral samples using ultra-deep sequencing

    Energy Technology Data Exchange (ETDEWEB)

    Chen, H

    2012-06-06

    RNA viruses have extremely high mutation rates that enable the virus to adapt to new host environments and even jump from one species to another. As part of a viral transmission study, three viral samples collected from naturally infected animals were sequenced using Illumina paired-end technology at ultra-deep coverage. In order to determine the mutant spectra within the viral quasispecies, it is critical to understand the sequencing error rates and control for false positive calls of viral variants (point mutantations). I will estimate the sequencing error rate from two control sequences and characterize the mutant spectra in the natural samples with this error rate.

  7. 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)

  8. Trace aluminium determination and sampling problems of archeological bone employing destructive neutron activation analysis

    International Nuclear Information System (INIS)

    Blotcky, A.J.; Rack, E.P.; Recker, R.R.; Leffler, J.A.; Teitelbaum, S.

    1978-01-01

    A destructive neutron activation analysis procedure was developed for determining trace aluminium content in bone. The method is based on a carefully planned sample preparation, irradiation at a neutron flux for 3.1x10 11 nxcm -2 xs -1 for 5 minutes, and chemical separation based on ion exchange. It was found that bone samples soaked in aluminium containing soil gave highly elevated aluminium values as a result of the aluminium adsorption into the bone matrix. The maximum aluminium content values for prehistoric bones are larger than those of modern bones and comparable to aluminium levels present in bone from renal patients. (T.G.)

  9. Generalized procedures for determining inspection sample sizes (related to quantitative measurements). Vol. 1: Detailed explanations

    International Nuclear Information System (INIS)

    Jaech, J.L.; Lemaire, R.J.

    1986-11-01

    Generalized procedures have been developed to determine sample sizes in connection with the planning of inspection activities. These procedures are based on different measurement methods. They are applied mainly to Bulk Handling Facilities and Physical Inventory Verifications. The present report attempts (i) to assign to appropriate statistical testers (viz. testers for gross, partial and small defects) the measurement methods to be used, and (ii) to associate the measurement uncertainties with the sample sizes required for verification. Working papers are also provided to assist in the application of the procedures. This volume contains the detailed explanations concerning the above mentioned procedures

  10. Accurate determination of rates from non-uniformly sampled relaxation data

    Energy Technology Data Exchange (ETDEWEB)

    Stetz, Matthew A.; Wand, A. Joshua, E-mail: wand@upenn.edu [University of Pennsylvania Perelman School of Medicine, Johnson Research Foundation and Department of Biochemistry and Biophysics (United States)

    2016-08-15

    The application of non-uniform sampling (NUS) to relaxation experiments traditionally used to characterize the fast internal motion of proteins is quantitatively examined. Experimentally acquired Poisson-gap sampled data reconstructed with iterative soft thresholding are compared to regular sequentially sampled (RSS) data. Using ubiquitin as a model system, it is shown that 25 % sampling is sufficient for the determination of quantitatively accurate relaxation rates. When the sampling density is fixed at 25 %, the accuracy of rates is shown to increase sharply with the total number of sampled points until eventually converging near the inherent reproducibility of the experiment. Perhaps contrary to some expectations, it is found that accurate peak height reconstruction is not required for the determination of accurate rates. Instead, inaccuracies in rates arise from inconsistencies in reconstruction across the relaxation series that primarily manifest as a non-linearity in the recovered peak height. This indicates that the performance of an NUS relaxation experiment cannot be predicted from comparison of peak heights using a single RSS reference spectrum. The generality of these findings was assessed using three alternative reconstruction algorithms, eight different relaxation measurements, and three additional proteins that exhibit varying degrees of spectral complexity. From these data, it is revealed that non-linearity in peak height reconstruction across the relaxation series is strongly correlated with errors in NUS-derived relaxation rates. Importantly, it is shown that this correlation can be exploited to reliably predict the performance of an NUS-relaxation experiment by using three or more RSS reference planes from the relaxation series. The RSS reference time points can also serve to provide estimates of the uncertainty of the sampled intensity, which for a typical relaxation times series incurs no penalty in total acquisition time.

  11. Determination of Hf, Sc and Y in geological samples together with the rare-earth elements

    International Nuclear Information System (INIS)

    Lihareva, N.; Delaloye, M.

    1997-01-01

    A method is described for the determination of Hf, Sc and Y simultaneously with the REE in geological materials. An earlier method for REE separation from major elements was studied with the aim to apply it also to the determination of Hf, Sc and Y. Sample decomposition was carried out by melting with LiBO 2 . The method involves separation and concentration stages, using the cation-exchange resin DOWEX AG 50W-X8. Matrix elements were eluted with 2 mol/l HCl, whereas 6 mol/l HNO 3 with oxalic acid and 8 mol/l HNO 3 were used to elute the elements to be determined. Some of the matrix elements could not be completely removed. This effect as well as the recovery rates of the determined elements were investigated. The measurements were performed by ICP-AES. Spectral interferences were also tested. (orig.). With 1 tab

  12. Determination of Mn, Fe, Ni, Cu, Zn and Pb contents in samples in samples of apple trees by radionuclide X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Bumbalova, A.; Havranek, E.; Harangozo, M.

    1982-01-01

    The applicability of the radionuclide X-ray fluorescence analysis (RXFA) for qualitative and quantitative evaluation of environmental plant samples is discussed and examples of determination of Mn, Fe, Ni, Cu, Zn, Pb in samples of apple trees are given. The instrumentation, the standard and sample preparation are also presented. (author)

  13. Determination of self shielding factors and gamma attenuation effects for tree ring samples

    International Nuclear Information System (INIS)

    Dagistan Sahin; Kenan Uenlue

    2012-01-01

    Determination of tree ring chemistry using Neutron Activation Analysis (NAA) is part of an ongoing research between Penn State University (PSU) and Cornell University, The Malcolm and Carolyn Wiener Laboratory for Aegean and Near Eastern Dendrochronology. Tree-ring chemistry yields valuable data for environmental event signatures. These signatures are a complex function of elemental concentration. To be certain about concentration of signature elements, it is necessary to perform the measurements and corrections with the lowest error and maximum accuracy possible. Accurate and precise values of energy dependent neutron flux at dry irradiation tubes and detector efficiency for tree ring sample are calculated for Penn State Breazeale Reactor (PSBR). For the calculation of energy dependent and self shielding corrected neutron flux, detailed model of the TRIGA Mark III reactor at PSU with updated fuel compositions was prepared using the MCNP utility for reactor evolution (MURE) libraries. Dry irradiation tube, sample holder and sample were also included in the model. The thermal flux self-shielding correction factors due to the sample holder and sample for were calculated and verified with previously published values. The Geant-4 model of the gamma spectroscopy system, developed at Radiation Science and Engineering Center (RSEC), was improved and absolute detector efficiency for tree-ring samples was calculated. (author)

  14. Method validation to determine total alpha beta emitters in water samples using LSC

    International Nuclear Information System (INIS)

    Al-Masri, M. S.; Nashawati, A.; Al-akel, B.; Saaid, S.

    2006-06-01

    In this work a method was validated to determine gross alpha and beta emitters in water samples using liquid scintillation counter. 200 ml of water from each sample were evaporated to 20 ml and 8 ml of them were mixed with 12 ml of the suitable cocktail to be measured by liquid scintillation counter Wallac Winspectral 1414. The lower detection limit by this method (LDL) was 0.33 DPM for total alpha emitters and 1.3 DPM for total beta emitters. and the reproducibility limit was (± 2.32 DPM) and (±1.41 DPM) for total alpha and beta emitters respectively, and the repeatability limit was (±2.19 DPM) and (±1.11 DPM) for total alpha and beta emitters respectively. The method is easy and fast because of the simple preparation steps and the large number of samples that can be measured at the same time. In addition, many real samples and standard samples were analyzed by the method and showed accurate results so it was concluded that the method can be used with various water samples. (author)

  15. Determination of phosphorus in wheat grass samples by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Kulkarni, S.D.; Rajurkar, N.S.; Acharya, R.; Nair, A.G.C.; Reddy, A.V.R.

    2005-01-01

    An instrumental neutron activation analysis (INAA) method using β-counting was used to determine phosphorus in wheat grass; grown in three different conditions. The phosphorus concentration was found to be in the range of 950-23000 mg/g in the samples grown in different conditions. The accuracy of the method was evaluated by determining phosphorus in three reference materials and the % deviations were within 10%. Reliability of the method was checked by following the half-life of the 32 P. (author)

  16. Combined method for the fast determination of pure beta emitting radioisotopes in food samples

    International Nuclear Information System (INIS)

    Kabai, Eva; Savkin, Birgit; Mehlsam, Isabell; Poppitz-Spuhler, Angela

    2017-01-01

    Fast radioanalytical methods are essential for a rapid response of decision makers. A fast method for the simultaneous determination of the pure beta emitting radionuclides 89 Sr/ 90 Sr and 99 Tc in food samples was developed. It includes the precipitation of fat and proteins with trichloroacetic acid for milk and dairy products and microwave digestion for other food products, followed by an anion exchange step to separate strontium from technetium. The purification steps for strontium and technetium are done using Sr-resin and TEVA-resin, respectively. Typical chemical yields are around 70 % for both radionuclides. The whole determination takes only around 20 h. (author)

  17. Reimiep 87. An interlaboratory U-235 enrichment determination by gamma measurement on solid UF6 sample

    International Nuclear Information System (INIS)

    Aparo, M.; Cresti, P.

    1988-01-01

    Gamma spectroscopy technique, based on the measurement of U 235 186 KeV flux, is now currently used for the determination of Uranium enrichment in different material of nuclear fuel cycle, namely: Uranium metallic, UO 2 pellets, UF 6 liquid or solid. The present paper describes the use of such a technique and the obtained results in determining the U 235 /U atomic isotopic abundance on a certified UF 6 solid sample. The measurements have been carried out in the frame work of the partecipation to the ''UF 6 Interlaboratory Measurements Evaluation Programme'' organized by CBNM/Geel with the support of the ESARDA (European Safeguards Research and Development Association)

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

    Directory of Open Access Journals (Sweden)

    Zoraida Sosa-Ferrera

    2013-01-01

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

  19. A novel speciation alternative for the determination of inorganic arsenic in marine samples

    DEFF Research Database (Denmark)

    Rasmussen, Rie Romme; Hedegaard, Rikke Susanne Vingborg; Herbst, M. Birgitte Koch

    collected in the official EU food control today are reported as total arsenic. High Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) is a useful but expensive tool for metal speciation analysis. Our novel, simple and inexpensive method for determination...... exchange SPE. The procedure include first pre-condition of the column, then loading of the buffered samples (pH 5.0-7.5), washing with 0.5 M acetic acid and finally elution of the sample from the column by 0.5 M HCl. The concentration of arsenic is determined by HG-AAS using external standards. The method......Arsenic (As) is bioaccumulated from seawater to concentrations in the mg/kg range in marine animals. More than 50 naturally-occurring arsenic containing species, both inorganic and organic forms, have been identified in marine animals. The organic forms are mainly considered to be non...

  20. The application of extraction chromatography to the determination of radionuclides in biological and environmental samples

    International Nuclear Information System (INIS)

    Testa, C.; Delle Site, A.

    1976-01-01

    The paper describe the application of extraction chromatography to the determination of several alpha and beta emitters in biological and environmental samples. Both column extraction chromatography and batch extraction process have been used to isolate the radionuclides from the samples. The effect of several parameters (extractant concentration, support granulometry, stirring time, temperature, presence of a complexing agent) on the extraction and elution has been examined. The application of redox extraction chromatography is also described. A very simple and rapid determination of the activity retained on the column can be obtained by transferring the slurry to a counting vial and by adding the scintillation liquid for a direct detection of the α or β emission. The counting efficiencies obtained with this technique are compared with those obtained with ion exchange resins. The organic polymers used for the extraction chromatography give about 100% counting efficiency. The conventional ion exchange resin cannot be used to this purpose because of their strong light absorption. (T.G.)

  1. Cloud point extraction, preconcentration and spectrophotometric determination of nickel in water samples using dimethylglyoxime

    Directory of Open Access Journals (Sweden)

    Morteza Bahram

    2013-01-01

    Full Text Available A new and simple method for the preconcentration and spectrophotometric determination of trace amounts of nickel was developed by cloud point extraction (CPE. In the proposed work, dimethylglyoxime (DMG was used as the chelating agent and Triton X-114 was selected as a non-ionic surfactant for CPE. The parameters affecting the cloud point extraction including the pH of sample solution, concentration of the chelating agent and surfactant, equilibration temperature and time were optimized. Under the optimum conditions, the calibration graph was linear in the range of 10-150 ng mL-1 with a detection limit of 4 ng mL-1. The relative standard deviation for 9 replicates of 100 ng mL-1 Ni(II was 1.04%. The interference effect of some anions and cations was studied. The method was applied to the determination of Ni(II in water samples with satisfactory results.

  2. Extraction chromatographic separation of iron from complex liquid samples and the determination of 55Fe

    International Nuclear Information System (INIS)

    Grahek, Z.; Rozmaric Macefat, M.

    2006-01-01

    Iron separation is described from liquid samples with a high concentration of ions that enables simple determination of 55 Fe. One of the described methods consists of iron precipitation from a large volume seawater by sodium hydroxide and/or ammonium carbonate and separation from other elements (Ca, Sr, Cu, Mg, etc.) on a TRU column with 4M HCl or 8M HNO 3 . In the other procedure iron is separated directly from a mixture of seawater samples and HCl on a TRU column. In both methods, the iron recovery is almost 100%. After separation, 55 Fe is determined by counting with a liquid scintillation counter. The binding of Fe and Zn on TEVA, U/TEVA and TRU resins from seawater solutions of HCl and HNO 3 depends on the type of the resin, concentration of acid and other ions. Iron and zinc can be separated from seawater on a U/TEVA column with 2M HCl. (author)

  3. 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.

  4. Gridsampler – A Simulation Tool to Determine the Required Sample Size for Repertory Grid Studies

    OpenAIRE

    Heckmann, Mark; Burk, Lukas

    2017-01-01

    The repertory grid is a psychological data collection technique that is used to elicit qualitative data in the form of attributes as well as quantitative ratings. A common approach for evaluating multiple repertory grid data is sorting the elicited bipolar attributes (so called constructs) into mutually exclusive categories by means of content analysis. An important question when planning this type of study is determining the sample size needed to a) discover all attribute categories relevant...

  5. Determination of the boron content in polyethylene samples using the reactor Orphée

    CERN Document Server

    Gunsing, F; Aberle, O

    2017-01-01

    The boron content of two unknown types of polyethylene has been determined relative to a known reference type. Samples of polyethylene, including a known boron-less one, were irradiated with thermal neutrons at the reactor Orphée at Saclay in France. Prompt gamma rays were measured with a CeBr$_3$ detector and the intensity of the 478~keV line from $^{10}${B}(n,$\\alpha_1\\gamma$)$^{7}{Li*} was extracted.

  6. Socioeconomic Determinants of Bullying in the Workplace: A National Representative Sample in Japan

    OpenAIRE

    Tsuno, Kanami; Kawakami, Norito; Tsutsumi, Akizumi; Shimazu, Akihito; Inoue, Akiomi; Odagiri, Yuko; Yoshikawa, Toru; Haratani, Takashi; Shimomitsu, Teruichi; Kawachi, Ichiro

    2015-01-01

    Bullying in the workplace is an increasingly recognized threat to employee health. We sought to test three hypotheses related to the determinants of workplace bullying: power distance at work; safety climate; and frustration related to perceived social inequality. A questionnaire survey was administered to a nationally representative community-based sample of 5,000 residents in Japan aged 20-60 years. The questionnaire included questions about employment, occupation, company size, education, ...

  7. Investigation of applicability of extrapolation method for sample field determination in single-yoke measuring setup

    Czech Academy of Sciences Publication Activity Database

    Stupakov, Oleksandr

    2006-01-01

    Roč. 307, - (2006), s. 279-287 ISSN 0304-8853 R&D Projects: GA AV ČR(CZ) 1QS100100508 Institutional research plan: CEZ:AV0Z10100520 Keywords : magnetic measurement * open magnetic sample * surface field determination * single-yoke setup * magnetic non-destructive testing Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.212, year: 2006

  8. Determination of uranium in urine samples for workers in the phosphoric acid purification using fluorimetry technique

    International Nuclear Information System (INIS)

    Kharita, M. H.; Sakhita, Kh.; Aldalal, Z.

    2003-10-01

    There is probability of exposure to uranium for workers in the phosphoric acid purification (internal exposure) by inhalation, and the deposition of this uranium in organs and tissues, and the consequence excreation out of the body by perspiration or urine. This study focuses on the determination of uranium in urine samples of workers. All results seem to be under the detection limit of the method, therefore no routine monitoring is required. (author)

  9. The determination of chromium in water samples by neutron activation analysis after preconcentration on activated carbon

    International Nuclear Information System (INIS)

    Sloot, H.A. van der

    1977-01-01

    A method is presented for the determination of chromium in sea- and fresh water. Chromium is concentrated on activated carbon from a neutral solution after a previous reduction of chromate with sodium sulfite at pH 1.5. The adsorption conditions, acidity, concentrations, amount of carbon, stirring-time, sample-volume, salinity, the influence of storage on the ratio of tervalent to hexavalent chromium, were investigated. The final determination of the total chromium content is performed by instrumental neutron-activation analysis. By preconcentration on activated carbon, a differentiation between tervalent and hexavalent chromium is possible. A separate determination of both species is not yet feasible due to the high carbon blank and to the necessity of measuring the adsorption percentage on carbon. The lower limit of determination, which depends on the value of the carbon blank, is 0.05 μg Cr/l with a precision of 20%. The determination is hampered by the considerable blank from the carbon. The use of activated carbon prepared from recrystallized sugar will probably improve the lower limit of determination and possibly allow the determination of chromate. (T.G.)

  10. Determination of chromium in water samples by neutron activation analysis after preconcentration on activated carbon

    Energy Technology Data Exchange (ETDEWEB)

    van der Sloot, H A [Stichting Reactor Centrum Nederland, Petten

    1977-01-01

    A method is presented for the determination of chromium in sea- and fresh water. Chromium is concentrated on activated carbon from a neutral solution after a previous reduction of chromate with sodium sulfite at pH 1.5. The adsorption conditions, acidity, concentrations, amount of carbon, stirring-time, sample-volume, salinity, the influence of storage on the ratio of tervalent to hexavalent chromium, were investigated. The final determination of the total chromium content is performed by instrumental neutron-activation analysis. By preconcentration on activated carbon, a differentiation between tervalent and hexavalent chromium is possible. A separate determination of both species is not yet feasible due to the high carbon blank and to the necessity of measuring the adsorption percentage on carbon. The lower limit of determination, which depends on the value of the carbon blank, is 0.05 ..mu..g Cr/l with a precision of 20%. The determination is hampered by the considerable blank from the carbon. The use of activated carbon prepared from recrystallized sugar will probably improve the lower limit of determination and possibly allow the determination of chromate.

  11. 51Cr-EDTA plasma clearance in severe renal failure determined by one plasma sample

    DEFF Research Database (Denmark)

    Kamper, A L; Nielsen, S L

    1989-01-01

    Two hundred and thirty-four measurements of standard 51Cr-EDTA plasma clearance were made in 50 patients with severe chronic renal failure. Based on these data two calculation methods were attempted using one plasma sample drawn 24 h after injection of 51Cr-EDTA. One of the methods used the 'one...... at zero-time was derived from injected dose and body surface area. This method might provide values 1.5 ml/min below or 0.8 ml/min above the established method of 51Cr-EDTA plasma clearance, which would be acceptable for clinical purposes. It is concluded that exact plasma clearance of 51Cr-EDTA in severe...... renal dysfunction (estimated clearance values below 21 ml/min) may be determined with adequate precision by one plasma sample drawn at 24 h after injection of the tracer without sampling at 5 h. This appears to be a very practical simplification....

  12. 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)

  13. Determination of 137Cs activities in soil samples from east and south Marmara region, Turkey

    International Nuclear Information System (INIS)

    Kilic, Oe.; Belivermis, M.; Cotuk, Y.; Coskun, M.; Cayir, A.; Kuecer, R.

    2006-01-01

    Activity concentrations of 1 37Cs, 4 0K and physico-chemical parameters of soil samples collected from 99 sampling stations in the east and south of Marmara Region of Turkey were determined. The study region was divided into 20 x 20 km grids and soil samples collected randomly in each square from 0-5 cm surface layer. Activities were measured by means of multichannel gamma analyser provided with high purity germanium detector. Relations among 1 37Cs concentrations and physico-chemical parameters of soils and climatic factors of the region were evaluated. Arc View GIS version 3.1 was used mapping of study area. Distribution of radionuclide concentrations in the region illustrated with contour maps using Surfer 8.0 for Windows. The range of activity concentrations of 1 37Cs and 4 0K were measured to be 0.92-153.72 and 69.24-1085.57 Bq/kg respectively

  14. Determination of 36Cl in environmental samples collected in the JCO by AMS

    International Nuclear Information System (INIS)

    Seki, R.; Tsukuba Univ., Ibaraki; Arai, D.; Nagashima, Y.; Takahashi, T.; Matsuhiro, T.; Imanaka, T.

    2003-01-01

    Long-lived chlorine, 36 Cl (T 1/2 = 301,000 y) in environmental samples has been measured by the AMS system installed in Tandem Accelerator Center, University of Tsukuba. A tri-carbon-molecular 12 C 3 - pilot beam method is used to stabilize the terminal voltage of the tandem. A small amount of pure carbon graphite is well mixed into a AgCl target material for creating Cl - and 12 C 3 - in the ion source. A 36 S isobaric interference in the system is eliminated to determine 36 Cl in environmental samples by chemical procedure. Some samples containing chlorine such as soil, chemical reagents and table salt have been collected in the JCO criticality accident site and analyzed to detect neutron-induced 36 Cl. The experimental result has been compared with a theoretical calculation. (author)

  15. Evaluation of metal ions in rice samples: extraction and direct determination by ICP OES

    International Nuclear Information System (INIS)

    Oliveira, Andrea; Cadore, Solange; Baccan, Nivaldo

    2012-01-01

    A method for extraction of metal ions present in rice samples using ammoniacal EDTA solution, pH = 10, as extractor agent is proposed under the following optimized conditions: 0.20 g of rice sample and 5.00 mL of ammoniacal EDTA (ethylenediaminetetraacetic acid) solution, with 5 min of ultrasound exposure time. Using robust ICP OES (inductively coupled plasma atomic emission spectrometry) conditions, direct analysis of the extraction solution was allowed, and the recovery values obtained were above 90% for most of the studied elements (P, K, Mg, Ca, Zn, Mn, Cu and Mo) with RSD -1 (Mn) - 48.68 mg kg -1 (K), showing adequate detectability for the determination of the analytes. The analysis of different samples indicated that Brazilian 'integral' rice contains higher contents of the constituents studied, followed by 'parboiled' rice, and the 'agulhinha' rice a long and thin grain type. (author)

  16. Determination of uranium in clinical and environmental samples by FIAS-ICPMS

    International Nuclear Information System (INIS)

    Karpas, Z.; Lorber, A.; Halicz, L.; Gavrieli, I.

    1998-01-01

    Uranium may enter the human body through ingestion or inhalation. Ingestion of uranium compounds through the diet, mainly drinking water, is a common occurrence, as these compounds are present in the biosphere. Inhalation of uranium-containing particles is mainly an occupational safety problem, but may also take place in areas where uranium compounds are abundant. The uranium concentration in urine samples may serve as an indication of the total uranium body content. A method based on flow injection and inductively coupled plasma mass spectrometry (FIAS-ICPMS) was found to be most suitable for determination of uranium in clinical samples (urine and serum), environmental samples (seawater, wells and carbonate rocks) and in liquids consumed by humans (drinking water and commercial beverages). Some examples of the application of the FIAS-ICPMS method are reviewed and presented here

  17. Quantitative surface topography determination by Nomarski reflection microscopy. 2: Microscope modification, calibration, and planar sample experiments

    International Nuclear Information System (INIS)

    Hartman, J.S.; Gordon, R.L.; Lessor, D.L.

    1980-01-01

    The application of reflective Nomarski differential interference contrast microscopy for the determination of quantitative sample topography data is presented. The discussion includes a review of key theoretical results presented previously plus the experimental implementation of the concepts using a commercial Momarski microscope. The experimental work included the modification and characterization of a commercial microscope to allow its use for obtaining quantitative sample topography data. System usage for the measurement of slopes on flat planar samples is also discussed. The discussion has been designed to provide the theoretical basis, a physical insight, and a cookbook procedure for implementation to allow these results to be of value to both those interested in the microscope theory and its practical usage in the metallography laboratory

  18. Determination of the self-attenuation correction factor for environmental samples analysis in gamma spectrometry

    International Nuclear Information System (INIS)

    Santos, Talita O.; Rocha, Zildete; Knupp, Eliana A.N.; Kastner, Geraldo F.; Oliveira, Arno H. de; Oliveira, Arno H. de

    2015-01-01

    Gamma spectrometry technique has been used in order to obtain the activity concentrations of natural and artificial radionuclides in environmental samples of different origins, compositions and densities. These samples characteristics may influence the calibration condition by the self-attenuation effect. The sample density has been considered the most important factor. For reliable results, it is necessary to determine self-attenuation correction factor which has been subject of great interest due to its effect on activity concentration. In this context, the aim of this work is to show the calibration process considering the correction by self-attenuation in the evaluation of the concentration of each radionuclide to a gamma HPGEe detector spectrometry system. (author)

  19. Sampling and analysis plan for the 116-C-5 retention basins characteristic dangerous waste determination

    International Nuclear Information System (INIS)

    Bauer, R.G.; Dunks, K.L.

    1996-03-01

    Cooling water flow from the rear face of the 100-B and 100-C reactors was diverted to large retention basins prior to discharge to the Columbia River. These retention basins delayed the release of the reactor coolant for decay of the short-lived activation products and for thermal cooling. Some of the activation products were deposited in sludge that settled in the basins and discharge lines. In addition, some contamination was deposited in soil around the basins and associated piping. The sampling objective of this project is to determine if regulated levels of leachable lead are present in the abrasive materials used to decontaminate the retention basin tank walls, in the material between the tank base plate and the concrete foundation, and in the soils immediately surrounding the perimeter of the retention basins. Sampling details, including sampling locations, frequencies, and analytical requirements, are discussed. Also described is the quality assurance plan for this project

  20. [Determination of buprofezin, methamidophos, acephate, and triazophos residues in Chinese tea samples by gas chromatography].

    Science.gov (United States)

    Zhang, Shuiba; Yi, Jun; Ye, Jianglei; Zheng, Wenhui; Cai, Xueqin; Gong, Zhenbin

    2004-03-01

    A method has been developed for the simultaneous determination of buprofezin, methamidophos, acephate and triazophos residues in Chinese tea samples. The pesticide residues were extracted from tea samples with a mixture of ethyl acetate and n-hexane (50:50, v/v) at 45 degrees C. The extracts were subsequently treated with a column packed with 40 mg of active carbon by gradient elution with ethyl acetate and n-hexane. Buprofenzin and the three organophosphorus pesticides were analyzed by gas chromatography using a DB-210 capillary column and a nitrogen-phosphorus detector. The recoveries for spiked standards were 73.4%-96.9%. The relative standard deviations were all within 4.63%. The limits of quantitation (3sigma) in the tea samples were about 7.0-12.0 microg/kg.

  1. A faster sample preparation method for determination of polonium-210 in fish

    International Nuclear Information System (INIS)

    Sadi, B.B.; Jing Chen; Kochermin, Vera; Godwin Tung; Sorina Chiorean

    2016-01-01

    In order to facilitate Health Canada’s study on background radiation levels in country foods, an in-house radio-analytical method has been developed for determination of polonium-210 ( 210 Po) in fish samples. The method was validated by measurement of 210 Po in a certified reference material. It was also evaluated by comparing 210 Po concentrations in a number of fish samples by another method. The in-house method offers faster sample dissolution using an automated digestion system compared to currently used wet-ashing on a hot plate. It also utilizes pre-packed Sr-resin® cartridges for rapid and reproducible separation of 210 Po versus time-consuming manually packed Sr-resin® columns. (author)

  2. Determination of the refractive index of n+- and p-type porous Si samples

    International Nuclear Information System (INIS)

    Setzu, S.; Romestain, R.; Chamard, V.

    2004-01-01

    Photochemical etching of porous Si layers has been shown to be able to create micrometer or submicrometer-scale lateral gratings very promising for photonic applications. However, the reduced size of this lateral periodicity hinders standard measurements of refractive index variations. Therefore accurate characterizations of such gratings are usually difficult. In this paper we address this problem by reproducing on a larger scale (millimeter) the micrometer scale light-induced refractive index variations associated to the lateral periodicity. Using this procedure we perform standard X-ray and optical reflectivity measurements on our samples. One can then proceed to the determination of light-induced variations of porosity and refractive index. We present results for p-type samples, where the photo-dissolution can only be realized after the formation of the porous layer, as well as for n + -type samples, where light action can only be effective during the formation of the porous layer

  3. The determination of precious metals in geological samples by ICP - Mass Spectrometry

    International Nuclear Information System (INIS)

    Denoyer, E.; Ediger, R.; Hager, J.

    1989-01-01

    ICP - mass spectrometry with laser sampling has been used to determine gold directly in solid fire assay beads. A small portion of the lead bead is vaporized by Nd: YAG laser, and the resulting particulate material is passed by a flow of argon an ICP-mass spectrometer for quantitation of the gold content. Calibration with known geological materials gives linear calibration curves, and detection limits for gols are estimated to be 0.07 micrograms/gram in the original ore sample. The repeatability of the method is similar to that expected for traditional fire assay methods, and the analysis time for the solid lead bead is less than five minutes per sample. (author) [pt

  4. 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

  5. Intercomparison of methods for determining 90Sr and 137Cs in plant samples

    International Nuclear Information System (INIS)

    Sha Lianmao; Zhao Min; Tian Guizhi

    1986-01-01

    The results of intercomparison of methods for determining 90 Sr and 137 Cs in plant samples are reported. Nine laboratories participated in the intercomparison. The samples used in intercomparison were reed and tea powders. The analytical results of 90 Sr in reed and 137 Cs in tea from different laboratories show good comparability and follow the normal-distribution. Some results reported of 137 Cs in reed are apparently lower than others. The results of 90 Sr in tea from different laboratories have poor comparability. The results obtained by HDEHP rapid extraction chromatograph appear to be too high, and it's cause is discussed. The 95% confidence intervals of content of 90 Sr and 137 Cs in reed and tea samples are given

  6. Determination of Th and REE in columbite - tantalite samples by ICP-OES

    International Nuclear Information System (INIS)

    Hanuman, V.V.; Khorge, C.R.; Radhamai, R.; Nair, Sajitha; Srivastava, P.K.

    2007-01-01

    A simple method of decomposition and separation of Th and REE in columbite- tantalite is developed for determination by ICP- OES. The sample is decomposed with hydrofluoric and hydrochloric acid in presence of little sulphuric acid to avoid drying on water bath. Th and rare earths are separated as fluoride together with undecomposed sample. The residue is fused with a 1: 1 mixture of sodium di hydrogen orthophosphate and sodium pyrophosphate. The melt is dissolved in water for measurement. Nitric acid is found unsuitable due to loss in Ce in some of the samples. Matrix elements (more than 97.5) are removed in single step by both the treatments. The free cassiterite present in samples is not attacked during acid digestion. However, the same is easily decomposed in fusion. U (IV) is also precipitated along with Th and REE when hydrochloric acid is used. As expected uranium is lost when nitric acid is used. The results are compared with existing well-established procedure involving peroxide fusion for decomposition; hydroxide and fluoride precipitation separation. Both the methods yielded comparable result. The method is simple, comparatively rapid and suitable for routine application for determination of REE , Th and U(IV) content. The RSD of the method was found to be in the range of 1- 1.5% for various elements. (author)

  7. 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)

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

    Science.gov (United States)

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

    2017-04-15

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

  9. Solid phase extraction for determination of 90Sr in water sample

    International Nuclear Information System (INIS)

    Ometakova, J.

    2009-01-01

    We studied the use of an extraction chromatography for determination of 90 Sr in samples of contaminated water. The aim of the thesis was to compare selected products from the point of view of the strontium yields and time needed. Three commercial products: 3M Empore Strontium Rad Disk, AnaLig, Sr-Resin and two classical methods: liquid-liquid extraction with tributylphosphate and carbonate co-precipitation (to eliminate interferers) were used for separation of 90 Sr. The water sample was used in radiochemical analysis for determination volume activity of 90 Sr. A radiochemical strontium yield was traced by using radionuclide 85 Sr. Samples were counted over a two week period to monitor the ingrowth of 90 Y on TRI CARB LSC counter. Samples were measured using an HPGe detector to find out 85 Sr recoveries at 514 keV line and they were counted directly by Cherenkov counting after the growth of 90 Y using TriCarb LSC counter after a two- week period (author)

  10. Preliminary study on element mass fraction determination on catfish samples from Paraguay

    International Nuclear Information System (INIS)

    Moreira, Edson G.; Catharino, Marilia G.M.; Vasconcellos, Marina B.A.; Frutos, Sixto A.; Insaurralde, Mario S.

    2013-01-01

    South American catfish (Pseudoplatystoma), commonly known in Spanish as atigrado or surubi and in Portuguese as surubim or pintado is a large fish that typically reaches 1 m long and weighs 60 kg to 80 kg and may be found at the basins of the Amazon, the Sao Francisco and de la Plata rivers, usually in riverbeds and deep wells. Being a much appreciated fish for human consumption, it is quite sought after by fishermen who have been contributing to the reduction of the stocks. This fact attracted the attention of the Paraguayan authorities to the point of imposing restrictions to free fishing and commercialization. This study aims to assist the conservation efforts towards this fish by investigating its exposure to possible pollutants. Preliminary results on element determination on six samples of catfish from Paraguayan rivers are presented. Cs, Co, Fe, Se and Zn were determined by applying an Instrumental Neutron Activation Analysis method. While these element levels were lower than the legislation for human consumption, the elements As, Cr e La were not detected in the samples as they are below the detection limit of the method employed. Atomic Absorption Spectrometry was used to investigate the presence of Cd, Hg and Pb in the samples. Hg was detected in the samples while Cd and Pb were below the detection limit of the method. (author)

  11. Development of a fast capillary electrophoresis method for determination of carbohydrates in honey samples.

    Science.gov (United States)

    Rizelio, Viviane Maria; Tenfen, Laura; da Silveira, Roberta; Gonzaga, Luciano Valdemiro; Costa, Ana Carolina Oliveira; Fett, Roseane

    2012-05-15

    In this study, the determination of fructose, glucose and sucrose by capillary electrophoresis (CE) was investigated. The tendency of the analyte to undergo electromigration dispersion and the buffer capacity were evaluated using the Peakmaster(®) software and considered in the optimization of the background electrolyte, which was composed of 20 mmol L(-1) sorbic acid, 0.2 mmol L(-1) CTAB and 40 mmol L(-1) NaOH at pH 12.2. Under optimal CE conditions, the separation of the substances investigated was achieved in less than 2 min. The detection limits for the three analytes were in the range of 0.022 and 0.029 g L(-1) and precision measurements within 0.62-4.69% were achieved. The proposed methodology was applied in the quantitative analysis by direct injection of in honey samples to determine the main sugars presents. The samples were previously dissolved in deionized water and filtered with no other sample treatment. The mean values for fructose, glucose and sucrose were in the ranges of 33.65-45.46 g 100g(-1), 24.63-35.06 g 100g(-1) and <0.22-1.32 g 100g(-1), respectively. The good analytical performance of the method makes it suitable for implementation in food laboratories for the routine analysis of honey samples. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Comparison of two sample preparation procedures for HPLC determination of ochratoxin A

    Directory of Open Access Journals (Sweden)

    Vuković Gorica L.

    2009-01-01

    Full Text Available In preparation of samples for chromatographic determination of ochratoxin A, two types of columns were used for sample cleanup (SPE and immunoaffinity columns. The first method consisted of liquid-liquid extraction with a mixture of chloroform and phosphoric acid, followed by ion-exchange cleanup on Waters Oasis MAX columns. The sec­ond method consisted of extraction with a mixture of water and methanol, followed by LCTech OtaCLEAN immunoaf­finity column cleanup. Recoveries of the methods were determined at three levels in three repetitions for maize flour, and they were 84% (%RSD = 19.2 for the first method of sample preparation and 101% (%RSD = 2.2 for the second method. Values of LOQ for OTA were 0.25 and 1.00 μg/kg for the IAC and SPE clean-up procedures, respectively. Both methods comply with present regulations, but the MAX sample clean-up procedure should be used as an alternative, since the immunoaffinity column clean-up procedure is characterized by better reproducibility, accuracy, and efficiency.

  13. Preliminary study on element mass fraction determination on catfish samples from Paraguay

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Edson G.; Catharino, Marilia G.M.; Vasconcellos, Marina B.A., E-mail: emoreira@ipen.br, E-mail: mbvascon@ipen.br, E-mail: mariliasemmler@uol.com.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Frutos, Sixto A.; Insaurralde, Mario S., E-mail: tony8013@hotmail.com, E-mail: insaurraldemar9@hotmail.com [Universidad Nacional de Asuncion (FCV/UNA), San Lorenzo (Paraguay). Facultad de Ciencias Veterinarias. Departamento de Pesca y Acuicultura

    2013-07-01

    South American catfish (Pseudoplatystoma), commonly known in Spanish as atigrado or surubi and in Portuguese as surubim or pintado is a large fish that typically reaches 1 m long and weighs 60 kg to 80 kg and may be found at the basins of the Amazon, the Sao Francisco and de la Plata rivers, usually in riverbeds and deep wells. Being a much appreciated fish for human consumption, it is quite sought after by fishermen who have been contributing to the reduction of the stocks. This fact attracted the attention of the Paraguayan authorities to the point of imposing restrictions to free fishing and commercialization. This study aims to assist the conservation efforts towards this fish by investigating its exposure to possible pollutants. Preliminary results on element determination on six samples of catfish from Paraguayan rivers are presented. Cs, Co, Fe, Se and Zn were determined by applying an Instrumental Neutron Activation Analysis method. While these element levels were lower than the legislation for human consumption, the elements As, Cr e La were not detected in the samples as they are below the detection limit of the method employed. Atomic Absorption Spectrometry was used to investigate the presence of Cd, Hg and Pb in the samples. Hg was detected in the samples while Cd and Pb were below the detection limit of the method. (author)

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  15. Test of methods for retrospective activity size distribution determination from filter samples

    International Nuclear Information System (INIS)

    Meisenberg, Oliver; Tschiersch, Jochen

    2015-01-01

    Determining the activity size distribution of radioactive aerosol particles requires sophisticated and heavy equipment, which makes measurements at large number of sites difficult and expensive. Therefore three methods for a retrospective determination of size distributions from aerosol filter samples in the laboratory were tested for their applicability. Extraction into a carrier liquid with subsequent nebulisation showed size distributions with a slight but correctable bias towards larger diameters compared with the original size distribution. Yields in the order of magnitude of 1% could be achieved. Sonication-assisted extraction into a carrier liquid caused a coagulation mode to appear in the size distribution. Sonication-assisted extraction into the air did not show acceptable results due to small yields. The method of extraction into a carrier liquid without sonication was applied to aerosol samples from Chernobyl in order to calculate inhalation dose coefficients for 137 Cs based on the individual size distribution. The effective dose coefficient is about half of that calculated with a default reference size distribution. - Highlights: • Activity size distributions can be recovered after aerosol sampling on filters. • Extraction into a carrier liquid and subsequent nebulisation is appropriate. • This facilitates the determination of activity size distributions for individuals. • Size distributions from this method can be used for individual dose coefficients. • Dose coefficients were calculated for the workers at the new Chernobyl shelter

  16. Sample pretreatment for the determination of metal impurities in silicon wafer

    International Nuclear Information System (INIS)

    Chung, H. Y.; Kim, Y. H.; Yoo, H. D.; Lee, S. H.

    1999-01-01

    The analytical results obtained by microwave digestion and acid digestion methods for sample pretreatment to determine metal impurities in silicon wafer by inductively coupled plasma--mass spectrometry(ICP-MS) were compared. In order to decompose the silicon wafer, a mixed solution of HNO 3 and HF was added to the sample and the metal elements were determined after removing the silicon matrix by evaporating silicon in the form of Si-F. The recovery percentages of Ni, Cr and Fe were found to be 95∼106% for both microwave digestion and acid digestion methods. The recovery percentage of Cu obtained by the acid digestion method was higher than that obtained by the microwave digestion method. For Zn, however, the microwave digestion method gave better result than the acid digestion method. Fe was added to a silicon wafer using a spin coater. The concentration of Fe in this sample was determined by ICP-MS, and the same results were obtained in the two pretreatment methods

  17. Fluorine determination in diet samples using cyclic NAA and PIGE analysis

    International Nuclear Information System (INIS)

    Farooqi, A.S.; Arshed, W.; Akanle, O.A.; Spyrou, N.M.

    1991-01-01

    Fluorine is an important trace element for life and human well-being. Food, in general, provides about 40% of the fluorine intake in the human body. In order to measure fluorine levels in human diet samples, Instrumental Neutron Activation Analysis (INAA) and Proton Induced Gamma-Ray Emission (PIGE) analysis were used. Thermal and epithermal cyclic NAA methods were applied, employing the 19 F(n,γ) 20 F and 19 F(n,p) 19 O nuclear reactions for the determination of fluorine, respectively. Corrections were made for the sodium matrix interference caused by the 23 Na(n,α) 20 F threshold reaction in the case of thermal cyclic NAA and for the oxygen interference via 18 O(n,γ) 19 O reaction when using the epithermal cyclic NAA method. The fluorine contents of diet samples were also determined by PIGE analysis making use of the resonance reaction 19 F(p,αγ) 16 O at 872 KeV. Thermal cyclic NAA was found to be most suitable for the determination of low concentrations of fluorine in the diet samples, with a detection limit of less than 10 μg/g

  18. An overview of the main foodstuff sample preparation technologies for tetracycline residue determination.

    Science.gov (United States)

    Pérez-Rodríguez, Michael; Pellerano, Roberto Gerardo; Pezza, Leonardo; Pezza, Helena Redigolo

    2018-05-15

    Tetracyclines are widely used for both the treatment and prevention of diseases in animals as well as for the promotion of rapid animal growth and weight gain. This practice may result in trace amounts of these drugs in products of animal origin, such as milk and eggs, posing serious risks to human health. The presence of tetracycline residues in foods can lead to the transmission of antibiotic-resistant pathogenic bacteria through the food chain. In order to ensure food safety and avoid exposure to these substances, national and international regulatory agencies have established tolerance levels for authorized veterinary drugs, including tetracycline antimicrobials. In view of that, numerous sensitive and specific methods have been developed for the quantification of these compounds in different food matrices. One will note, however, that the determination of trace residues in foods such as milk and eggs often requires extensive sample extraction and preparation prior to conducting instrumental analysis. Sample pretreatment is usually the most complicated step in the analytical process and covers both cleaning and pre-concentration. Optimal sample preparation can reduce analysis time and sources of error, enhance sensitivity, apart from enabling unequivocal identification, confirmation and quantification of target analytes. The development and implementation of more environmentally friendly analytical procedures, which involve the use of less hazardous solvents and smaller sample sizes compared to traditional methods, is a rapidly increasing trend in analytical chemistry. This review seeks to provide an updated overview of the main trends in sample preparation for the determination of tetracycline residues in foodstuffs. The applicability of several extraction and clean-up techniques employed in the analysis of foodstuffs, especially milk and egg samples, is also thoroughly discussed. Copyright © 2018 Elsevier B.V. All rights reserved.

  19. Sample preparation of waste water to determine metallic contaminants by X-ray fluorescence spectroscopy

    International Nuclear Information System (INIS)

    Gonzalez Olivos, Javier.

    1987-01-01

    Trace X-ray fluorescence spectroscopy analysis in liquid samples is preceded by sample preparation, which usually consists in the precipitation of the metallic ions and concentration over a thin cellulose filter. The samples preparation of waste water by this method is not efficient, due to the great amount of organic and insoluble matter that they contain. The purpose of this work was to determine the optimal value of pH in order to adsorbe all the insoluble matter contained in a waste water sample in the activated charcoal, so that the metallic ions could be precipitated and concentrated on a thin filter and determinated by X-ray fluorescence spectroscopy. A survey about the adsorption of some ions in activated charcoal in function of the pH was made for the following: Cr 3+ , Fe 3+ , Ni 2+ , Cu 2+ , Zn 2+ , Se 2+ , Hg 2+ , and Pb 2+ . It was observed that at pH 0, the ions are not adsorbed, but Cu 2+ and Zn 2+ are adsorbed in small amount; at pH 14, the ions are adsorbed, excluding Se, which is not adsorbed at any value of pH. If a waste water sample is treated at pH 0 with activated charcoal to adsorbe the organic and insoluble matter, most of the metallic ions are not adsorbed by the activated charcoal and could be precipitated with APDC (ammonium 1-pirrolidine dithio carbamate salt) and concentrated on a thin filter. The analysis of the metallic ions contained on the filter and those adsorbed in the activated charcoal by X-ray fluorescence spectroscopy, gave the total amount of the ions in the sample. (author)

  20. V. Terrestrial vertebrates

    Science.gov (United States)

    Dean Pearson; Deborah Finch

    2011-01-01

    Within the Interior West, terrestrial vertebrates do not represent a large number of invasive species relative to invasive weeds, aquatic vertebrates, and invertebrates. However, several invasive terrestrial vertebrate species do cause substantial economic and ecological damage in the U.S. and in this region (Pimental 2000, 2007; Bergman and others 2002; Finch and...

  1. Determination of 210Pb e 210Po in marine samples and aerosols

    International Nuclear Information System (INIS)

    Saito, Roberto Tatsuya

    1996-01-01

    In this work the methodologies for 210 Pb e 210 Po analyses in marine samples, such as fish, seaweed, sediment, and aerosol samples are presented. The 210 Pb levels in the samples were obtained by both 210 Bi and 210 Po ingrowth. The 210 Pb analysis via 210 Bi presents the following steps: 210 Pb leaching from samples with 8 M nitric acid and hydrogen peroxide; lead sulphate precipitation; conversion to carbonate; dissolution; lead sulphate precipitation; gravimetric analysis of lead; waiting of time to reach radioactive equilibrium and 210 Bi beta counting by employing a Geiger-Mueller detector with a low background radiation. The 210 Pb analysis via 210 Po presents the following steps: 210 Pb and 210 Po leaching from samples with 8 M nitric acid and hydrogen peroxide; nitric acid elimination by heating and hydrochloric acid addition; spontaneous deposition onto silver disc and alpha counting of polonium in silicon surface-barrier detector. In order to determine 210 Pb activity, the solution was percolated in the Dowex AG 1-X 8 anion exchange resin; preconditioned with 8 M nitric acid; the lead was eluted by 8 M hydrochloric acid; the solution was gently evaporated to dryness and diluted with 0.5 N hydrochloric acid. After 3-6 months a second 210 Po spontaneous deposition onto silver disc was carried out. The methodology for 210 Pb analysis via 210 Bi showed lead recoveries from 63 to 100%. In the method via 210 Po the polonium recoveries were varied from 39 to 63% under manual agitation, and from 60 to 100% under mechanical agitation. The radiochemical methods for 210 Po and 210 Pb analyses were applied in reference samples from International Atomic Energy Agency (IAEA) and the results obtained showed the good precision and accuracy of the established methods. The analysis of marine sediment samples of Antarctica presented 210 Pb and Po levels from 8 to 60 Bq.kg -1 , and fish samples from Sao Paulo Coast presented 210 Po levels from 0.5 to 5.3 Bq.kg -1 . These

  2. A general method to determine sampling windows for nonlinear mixed effects models with an application to population pharmacokinetic studies.

    Science.gov (United States)

    Foo, Lee Kien; McGree, James; Duffull, Stephen

    2012-01-01

    Optimal design methods have been proposed to determine the best sampling times when sparse blood sampling is required in clinical pharmacokinetic studies. However, the optimal blood sampling time points may not be feasible in clinical practice. Sampling windows, a time interval for blood sample collection, have been proposed to provide flexibility in blood sampling times while preserving efficient parameter estimation. Because of the complexity of the population pharmacokinetic models, which are generally nonlinear mixed effects models, there is no analytical solution available to determine sampling windows. We propose a method for determination of sampling windows based on MCMC sampling techniques. The proposed method attains a stationary distribution rapidly and provides time-sensitive windows around the optimal design points. The proposed method is applicable to determine sampling windows for any nonlinear mixed effects model although our work focuses on an application to population pharmacokinetic models. Copyright © 2012 John Wiley & Sons, Ltd.

  3. Determination of Ra-226, Ra-228 and K-40 specific activities in samples of mineral fertilizer marketed in the Rio de Janeiro City

    International Nuclear Information System (INIS)

    Garcez, R. W. D.; Marques L, J.; Da Silva, A. X.

    2017-10-01

    The use a fertilizers ia a common practice in agriculture and several samples have radionuclides in their composition, this content is natural but some samples may have high concentrations of these radionuclides and this represent a potential radiological risk for plants, animals and water. Therefore the radiometric analyses these compounds is important and the main aim of this paper is to determine the specific concentration of K-40, Ra-226 and Ra-228 in fertilizer samples available in market of Rio de Janeiro city and discussing the impacts to agricultural soils caused by this practice. The analyzed fertilizer samples are of four types: nitrogen, potash, phosphate and NPK, they were analyzed using gamma spectroscopy with a Hp-Ge detector and with the LabSOCS software for the calculation of the efficiency curve. The specific activities of Ra-226 ranged from 1.48 Bq/kg to 597 Bq/kg, Ra-228 ranged from 2.66 Bq/kg to 832 Bq/kg and K-40 ranged from 16 Bq/kg to 13941 Bq/kg. All samples, except two nitrogen fertilizer samples, presented the absorbed dose rate in air at 1 m above the ground level higher than the estimated average global terrestrial radiation of 51 n Gy/h and the phosphate fertilizer samples presented the highest average absorbed dose rate of 532.5 n Gy/h, which indicates a greater potential of environmental contamination. But considering a dilution (1:1000) g of fertilizer in soil was found an average increase of 0.36 μSv/y at the annual outdoor effective dose while the annual average for the soil is of 63 μSv/y, so the risk to human health is minimum. (Author)

  4. Determination of biomass burning tracers in air samples by GC/MS

    Directory of Open Access Journals (Sweden)

    Janoszka Katarzyna

    2018-01-01

    Full Text Available Levoglucosan (LG as a main cellulose burning product at 300°C is a biomass burning tracer. LG characterize by relatively high molar mass and it is sorbed by particulate matter. In the study of air pollution monitoring LG is mainly analyzed in particulate matter, PM1 and PM2,5. The tracer create relatively high O-H…O bond and weaker C-H…O bond. Due to the hydrogen bond, LG dissolves very well in water. Analytical procedure of LG determination include: extraction, derivatization and analysis by gas chromatography coupled with mass spectrometry detector. In water samples levoglucosan is determined by liquid chromatography. The paper presents a methodology for particulate matter samples determination their analysis by gas chromatography coupled with a mass spectrometry detector. Determination of LG content in particulate matter was performed according to an analytical method based on simultaneous pyridine extraction and derivatization using N,O-bis (trimethylsilyl trifluoroacetamide and trimethylchlorosilane mixture (BSTFA: TMCS, 99: 1.

  5. Sensitive spectrophotometric methods for determination of some organophosphorus pesticides in vegetable samples

    Directory of Open Access Journals (Sweden)

    MAGDA A. AKL

    2010-03-01

    Full Text Available Three rapid, simple, reproducible and sensitive spectrophotometric methods (A, B and C are described for the determination of two organophosphorus pesticides, (malathion and dimethoate in formulations and vegetable samples. The methods A and B involve the addition of an excess of Ce4+ into sulphuric acid medium and the determination of the unreacted oxidant by decreasing the red color of chromotrope 2R (C2R at a suitable lmax = 528 nm for method A, or a decrease in the orange pink color of rhodamine 6G (Rh6G at a suitable lmax = = 525 nm. The method C is based on the oxidation of malathion or dimethoate with the slight excess of N-bromosuccinimide (NBS and the determination of unreacted oxidant by reacting it with amaranth dye (AM in hydrochloric acid medium at a suitable lmax = 520 nm. A regression analysis of Beer-Lambert plots showed a good correlation in the concentration range of 0.1-4.2 μg mL−1. The apparent molar absorptivity, Sandell sensitivity, the detection and quantification limits were calculated. For more accurate analysis, Ringbom optimum concentration ranges are 0.25-4.0 μg mL−1. The developed methods were successfully applied to the determination of malathion, and dimethoate in their formulations and environmental vegetable samples.

  6. Determination of biomass burning tracers in air samples by GC/MS

    Science.gov (United States)

    Janoszka, Katarzyna

    2018-01-01

    Levoglucosan (LG) as a main cellulose burning product at 300°C is a biomass burning tracer. LG characterize by relatively high molar mass and it is sorbed by particulate matter. In the study of air pollution monitoring LG is mainly analyzed in particulate matter, PM1 and PM2,5. The tracer create relatively high O-H…O bond and weaker C-H…O bond. Due to the hydrogen bond, LG dissolves very well in water. Analytical procedure of LG determination include: extraction, derivatization and analysis by gas chromatography coupled with mass spectrometry detector. In water samples levoglucosan is determined by liquid chromatography. The paper presents a methodology for particulate matter samples determination their analysis by gas chromatography coupled with a mass spectrometry detector. Determination of LG content in particulate matter was performed according to an analytical method based on simultaneous pyridine extraction and derivatization using N,O-bis (trimethylsilyl) trifluoroacetamide and trimethylchlorosilane mixture (BSTFA: TMCS, 99: 1).

  7. Determination of air-loop volume and radon partition coefficient for measuring radon in water sample.

    Science.gov (United States)

    Lee, Kil Yong; Burnett, William C

    A simple method for the direct determination of the air-loop volume in a RAD7 system as well as the radon partition coefficient was developed allowing for an accurate measurement of the radon activity in any type of water. The air-loop volume may be measured directly using an external radon source and an empty bottle with a precisely measured volume. The partition coefficient and activity of radon in the water sample may then be determined via the RAD7 using the determined air-loop volume. Activity ratios instead of absolute activities were used to measure the air-loop volume and the radon partition coefficient. In order to verify this approach, we measured the radon partition coefficient in deionized water in the temperature range of 10-30 °C and compared the values to those calculated from the well-known Weigel equation. The results were within 5 % variance throughout the temperature range. We also applied the approach for measurement of the radon partition coefficient in synthetic saline water (0-75 ppt salinity) as well as tap water. The radon activity of the tap water sample was determined by this method as well as the standard RAD-H 2 O and BigBottle RAD-H 2 O. The results have shown good agreement between this method and the standard methods.

  8. Determination of air-loop volume and radon partition coefficient for measuring radon in water sample

    International Nuclear Information System (INIS)

    Kil Yong Lee; Burnett, W.C.

    2013-01-01

    A simple method for the direct determination of the air-loop volume in a RAD7 system as well as the radon partition coefficient was developed allowing for an accurate measurement of the radon activity in any type of water. The air-loop volume may be measured directly using an external radon source and an empty bottle with a precisely measured volume. The partition coefficient and activity of radon in the water sample may then be determined via the RAD7 using the determined air-loop volume. Activity ratios instead of absolute activities were used to measure the air-loop volume and the radon partition coefficient. In order to verify this approach, we measured the radon partition coefficient in deionized water in the temperature range of 10-30 deg C and compared the values to those calculated from the well-known Weigel equation. The results were within 5 % variance throughout the temperature range. We also applied the approach for measurement of the radon partition coefficient in synthetic saline water (0-75 ppt salinity) as well as tap water. The radon activity of the tap water sample was determined by this method as well as the standard RAD-H 2 O and BigBottle RAD-H 2 O. The results have shown good agreement between this method and the standard methods. (author)

  9. Determination of the uranium concentration in water samples by the technique of fission track recording

    International Nuclear Information System (INIS)

    Geraldo, L.P.

    1979-01-01

    The technique of fission track register was developed for the determination of micrograms of uranium. The Makrofol KG, a synthetic plastic made by Bayer, was used as the detector and the wet method was utilized. The detector calibration curve allows the determination of the uranium concentration in a sample within an interval from 8.0 to 0.4μgU/L, the total error ranging from 3.3% to 29.0% respectively. The method was used in the determination of the uranium content in various water samples, obtained from various sources like rivers, sea etc. in the state of Sao Paulo, Brazil. Results were compared with those obtained by other authors using different methods. The average concentration found in sea waters (3.27 +- 9.12μgU/l) by this method is compatible with the international average accepted value of 3.3μgU/l, irrespective of site and depth. The determination of the uranium content by fission track counting has proved to be very convenient. (Author) [pt

  10. 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

  11. Analysis of volatile organic compounds in compost samples: A potential tool to determine appropriate composting time.

    Science.gov (United States)

    Zhu, Fengxiang; Pan, Zaifa; Hong, Chunlai; Wang, Weiping; Chen, Xiaoyang; Xue, Zhiyong; Yao, Yanlai

    2016-12-01

    Changes in volatile organic compound contents in compost samples during pig manure composting were studied using a headspace, solid-phase micro-extraction method (HS-SPME) followed by gas chromatography with mass spectrometric detection (GC/MS). Parameters affecting the SPME procedure were optimized as follows: the coating was carbon molecular sieve/polydimethylsiloxane (CAR/PDMS) fiber, the temperature was 60°C and the time was 30min. Under these conditions, 87 compounds were identified from 17 composting samples. Most of the volatile components could only be detected before day 22. However, benzenes, alkanes and alkenes increased and eventually stabilized after day 22. Phenol and acid substances, which are important factors for compost quality, were almost undetectable on day 39 in natural compost (NC) samples and on day 13 in maggot-treated compost (MC) samples. Our results indicate that the approach can be effectively used to determine the composting times by analysis of volatile substances in compost samples. An appropriate composting time not only ensures the quality of compost and reduces the loss of composting material but also reduces the generation of hazardous substances. The appropriate composting times for MC and NC were approximately 22days and 40days, respectively, during the summer in Zhejiang. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    1993-01-01

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

  13. Determination of low level of plutonium and uranium isotopes in safeguard swipe sample

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Myung Ho; Park, Jong Ho; Oh, Seong Yong; Lee, Chang Heon; Ahn, Hong Ju; Song, Kyu Seok [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2011-10-15

    For the determination of radionuclides, the separation techniques based on the principles of anion exchange, liquid-liquid extraction or column extraction chromatography are frequently used in nuclear analytical applications. Recently, a novel extraction chromatographic resin has been developed by Horwitz and co-workers, which are capable of selective extraction of the actinides. General separation of plutonium and uranium with extraction chromatographic techniques are focused on the environmental or radioactive waste samples. Also, the chemical yields for Pu and U isotopes with extraction chromatographic method sometimes are variable. For effective extraction of Pu isotopes in the very level of plutonium sample with UTEVA resin, the valence adjustment of Pu isotopes in the sample solution requires due to unstability in the oxidation state of Pu isotopes during separation step. Therefore, it is necessary to develop a simple and robust radiochemical separation method for nano- or pico gram amounts of uranium and plutonium in safeguard swipe samples. Chemical yields of plutonium and uranium with extraction chromatographic method of Pu and U upgrades in this study were compared with several separation methods for Pu and U generally used in the radiochemistry field. Also, the redox reactions of hydrogen peroxide with plutonium in the nitric acid media were investigated by UV-Vis-NIR absorption spectroscopy. Based on general extraction chromatography method with UTEVA resin, the separation method of nano- and picogram amounts of uranium and plutonium in safeguard swipe samples was developed in this study

  14. Comparison of supercritical fluid extraction and Soxhlet extraction for the determination of PCBs in seaweed samples.

    Science.gov (United States)

    Punín Crespo, M O; Lage Yusty, M A

    2005-06-01

    The efficiency of supercritical fluid extraction for the determination of 12 polychlorinated biphenyls from algae samples is compared to Soxhlet extraction. Analytical detection limits for the individual congeners ranged from 0.62 microgl(-1) to 19 microgl(-1). Recovery was tested for both methods using standard addition procedure. At maximum spike level of concentration, the mean recoveries were not significantly different (P>0.05) of all PCBs studied, with the exception of PCBs 28, 52, 77 and 169. Method precision for Soxhlet extraction (yield comparable results, SFE offers the advantage of detecting all PCBs studied at lower concentrations, reducing extraction time, and reducing the amount of solvents needed. The optimized methods were applied to the analysis of three real seaweed samples, except for PCB101 the concentrations of all PCBs were low or below the detection limits. The levels of PCB101 found in sample 1 were 6.6+/-0.54 ng g(-1) d.w., in sample 2 the levels were 8.2+/-0.86 ng g(-1) d.w. and in sample 3 they were 7.7+/-0.08 ng g(-1) d.w.

  15. Enzyme-linked immunosorbent assay for ultratrace determination of antibiotics in aqueous samples.

    Science.gov (United States)

    Kumar, Kuldip; Thompson, Anita; Singh, Ashok K; Chander, Yogesh; Gupta, Satish C

    2004-01-01

    Two commercially available enzyme-linked immunosorbent assay (ELISA) kits that are commonly used for tylosin or tetracycline residues in meat and milk were adapted for ultratrace analysis of these antibiotics in surface and ground waters. These two antibiotics are commonly fed to swine, turkeys, and cattle at subtherapeutic doses for growth promotion purposes. Both ELISA techniques were found to be highly sensitive and selective for the respective antibiotics with detection limits of 0.10 and 0.05 microg L(-1) for tylosin and tetracycline, respectively. The recovery of both tylosin and tetracycline from spiked samples of lake waters, runoff samples, soil saturation extracts, and nanopure water was close to 100%. Tetracycline ELISA was highly specific for tetracycline and chlortetracycline but not for other forms of tetracycline (oxytetracycline, demeclocycline, and doxycycline). Analysis of a few liquid swine manure samples by liquid chromatography-mass spectrometry (LC-MS) showed lower concentrations for chlortetracycline as compared with concentrations obtained using ELISA. However, the concentrations of tylosin from ELISA were comparable with that of LC-MS. The lower concentrations of chlortetracycline obtained by LC-MS in manure samples indicate the presence of other similar or transformed compounds that were detected by ELISA but not determined by LC-MS. These results indicate that both ELISA kits can be useful tools for low-cost screening of tylosin, tetracycline, and chlortetracycline in environmental waters. Furthermore, both ELISA procedures are rapid, portable, and easily adaptable for testing of multiple samples simultaneously.

  16. Determination of uranium in tree bark samples by epithermal neutron activation analysis

    International Nuclear Information System (INIS)

    Lima, Nicole Pereira de; Saiki, Mitiko

    2017-01-01

    In this study uranium (U) concentrations were determined in certified reference materials (CRMs) and in tree bark samples collected in 'Cidade Universitaria Armando de Salles Oliveira' (CUASO) USP, Sao Paulo, SP, Brazil). The barks were collected from different species namely Poincianella pluviosa and Tipuana tipu. These bark samples were cleaned, dried, grated and milled for the analyses by epithermal neutron activation analysis method (ENAA). This method consists on irradiating samples and U standard in IEAR1 nuclear reactor with thermal neutron flux of 1:9 x 10 12 n cm -2 s -1 during 40 to 60 seconds depending on the samples matrices. The samples and standard were measured by gamma ray spectroscopy. U was identified by the peak of 74.66 keV of 239 U with half life of 23.47 minutes. Concentration of U was calculated by comparative method. For analytical quality control of U results, certified reference materials were analysed. Results obtained for CRMs presented good precision and accuracy, with |Z score| <= 0.39. Uranium concentrations in tree barks varied from 83.1 to 627.6 ng g - 1 and the relative standard deviations of these results ranged from 1.8 to 10%. (author)

  17. Determination of uranium in tree bark samples by epithermal neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Lima, Nicole Pereira de; Saiki, Mitiko, E-mail: mitiko@ipen.com [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2017-11-01

    In this study uranium (U) concentrations were determined in certified reference materials (CRMs) and in tree bark samples collected in 'Cidade Universitaria Armando de Salles Oliveira' (CUASO) USP, Sao Paulo, SP, Brazil). The barks were collected from different species namely Poincianella pluviosa and Tipuana tipu. These bark samples were cleaned, dried, grated and milled for the analyses by epithermal neutron activation analysis method (ENAA). This method consists on irradiating samples and U standard in IEAR1 nuclear reactor with thermal neutron flux of 1:9 x 10{sup 12} n cm{sup -2} s{sup -1} during 40 to 60 seconds depending on the samples matrices. The samples and standard were measured by gamma ray spectroscopy. U was identified by the peak of 74.66 keV of {sup 239}U with half life of 23.47 minutes. Concentration of U was calculated by comparative method. For analytical quality control of U results, certified reference materials were analysed. Results obtained for CRMs presented good precision and accuracy, with |Z score| <= 0.39. Uranium concentrations in tree barks varied from 83.1 to 627.6 ng g{sup -} {sup 1} and the relative standard deviations of these results ranged from 1.8 to 10%. (author)

  18. Development of pre-concentration procedure for the determination of Hg isotope ratios in seawater samples.

    Science.gov (United States)

    Štrok, Marko; Hintelmann, Holger; Dimock, Brian

    2014-12-03

    Hg concentrations in seawater are usually too low to allow direct (without pre-concentration and removal of salt matrix) measurement of its isotope ratios with multicollector-inductively coupled plasma mass spectrometry (MC-ICP-MS). Therefore, a new method for the pre-concentration of Hg from large volumes of seawater was developed. The final method allows for relatively fast (about 2.5Lh(-1)) and quantitative pre-concentration of Hg from seawater samples with an average Hg recovery of 98±6%. Using this newly developed method we determined Hg isotope ratios in seawater. Reference seawater samples were compared to samples potentially impacted by anthropogenic activity. The results show negative mass dependent fractionation relative to the NIST 3133 Hg standard with δ(202)Hg values in the range from -0.50‰ to -1.50‰. In addition, positive mass independent fractionation of (200)Hg was observed for samples from reference sites, while impacted sites did not show significant Δ(200)Hg values. Although the influence of the impacted sediments is limited to the seawater and particulate matter in very close proximity to the sediment, this observation may raise the possibility of using Δ(200)Hg to distinguish between samples from impacted and reference sites. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. Determination of rhenium in biological and environmental samples by radiochemical neutron activation analysis

    International Nuclear Information System (INIS)

    Kucera, J.; Mizera, J.; Randa, Z.; Byrne, A.R.; Lucanikova, M.

    2006-01-01

    Radiochemical neutron activation procedures using liquid-liquid extraction with tetraphenylarsonium chloride in chloroform from 1 M HCl and solid extraction with ALIQUAT 336 incorporated in a polyacrylonitrile binding matrix from 0.1 M HCl were developed for accurate determination of rhenium in biological and environmental samples at the sub-ng.g -1 level. Concentrations of Re in the range of 0.1 to 2.4 ng.g -1 were determined in several botanical reference materials (RM), while in a RM of road dust a value of approx. 10 ng.g -1 was found. Significantly elevated values of Re, up to 90 ng.g -1 , were found in seaweed (brown algae). Results for Re in the brown algae Fucus vesiculosus in which elevated 99 Tc values had previously been determined suggest possible competition between Re and Tc in the accumulation process. (author)

  20. An axisymmetric diffusion experiment for the determination of diffusion and sorption coefficients of rock samples.

    Science.gov (United States)

    Takeda, M; Hiratsuka, T; Ito, K; Finsterle, S

    2011-04-25

    Diffusion anisotropy is a critical property in predicting migration of substances in sedimentary formations with very low permeability. The diffusion anisotropy of sedimentary rocks has been evaluated mainly from laboratory diffusion experiments, in which the directional diffusivities are separately estimated by through-diffusion experiments using different rock samples, or concurrently by in-diffusion experiments in which only the tracer profile in a rock block is measured. To estimate the diffusion anisotropy from a single rock sample, this study proposes an axisymmetric diffusion test, in which tracer diffuses between a cylindrical rock sample and a surrounding solution reservoir. The tracer diffusion between the sample and reservoir can be monitored from the reservoir tracer concentrations, and the tracer profile could also be obtained after dismantling the sample. Semi-analytical solutions are derived for tracer concentrations in both the reservoir and sample, accounting for an anisotropic diffusion tensor of rank two as well as the dilution effects from sampling and replacement of reservoir solution. The transient and steady-state analyses were examined experimentally and numerically for different experimental configurations, but without the need for tracer profiling. These experimental configurations are tested for in- and out-diffusion experiments using Koetoi and Wakkanai mudstones and Shirahama sandstone, and are scrutinized by a numerical approach to identify favorable conditions for parameter estimation. The analysis reveals the difficulty in estimating diffusion anisotropy; test configurations are proposed for enhanced identifiability of diffusion anisotropy. Moreover, it is demonstrated that the axisymmetric diffusion test is efficient in obtaining the sorption parameter from both steady-state and transient data, and in determining the effective diffusion coefficient if isotropic diffusion is assumed. Moreover, measuring reservoir concentrations in an

  1. An asixymmetric diffusion experiment for the determination of diffusion and sorption coefficients of rock samples

    Energy Technology Data Exchange (ETDEWEB)

    Takeda, M.; Hiratsuka, T.; Ito, K.; Finsterle, S.

    2011-02-01

    Diffusion anisotropy is a critical property in predicting migration of substances in sedimentary formations with very low permeability. The diffusion anisotropy of sedimentary rocks has been evaluated mainly from laboratory diffusion experiments, in which the directional diffusivities are separately estimated by through-diffusion experiments using different rock samples, or concurrently by in-diffusion experiments in which only the tracer profile in a rock block is measured. To estimate the diffusion anisotropy from a single rock sample, this study proposes an axisymmetric diffusion test, in which tracer diffuses between a cylindrical rock sample and a surrounding solution reservoir. The tracer diffusion between the sample and reservoir can be monitored from the reservoir tracer concentrations, and the tracer profile could also be obtained after dismantling the sample. Semi-analytical solutions are derived for tracer concentrations in both the reservoir and sample, accounting for an anisotropic diffusion tensor of rank two as well as the dilution effects from sampling and replacement of reservoir solution. The transient and steady-state analyses were examined experimentally and numerically for different experimental configurations, but without the need for tracer profiling. These experimental configurations are tested for in- and out-diffusion experiments using Koetoi and Wakkanai mudstones and Shirahama sandstone, and are scrutinized by a numerical approach to identify favorable conditions for parameter estimation. The analysis reveals the difficulty in estimating diffusion anisotropy; test configurations are proposed for enhanced identifiability of diffusion anisotropy. Moreover, it is demonstrated that the axisymmetric diffusion test is efficient in obtaining the sorption parameter from both steady-state and transient data, and in determining the effective diffusion coefficient if isotropic diffusion is assumed. Moreover, measuring reservoir concentrations in an

  2. Determination of uranium concentration in an ore sample using laser-induced breakdown spectroscopy

    International Nuclear Information System (INIS)

    Kim, Y.-S.; Han, B.-Y.; Shin, H.S.; Kim, H.D.; Jung, E.C.; Jung, J.H.; Na, S.H.

    2012-01-01

    Laser-induced breakdown spectroscopy (LIBS) has been recognized as a promising technique for analyzing sensitive nuclear materials such as uranium, plutonium, and curium in a high-radiation environment, especially since the implementation of IAEA (International Atomic Energy Agency) safeguards. The uranium spectra of ore samples were quantitatively analyzed prior to analyzing sensitive materials in the nuclear industry. The purpose of this experiment is to extract quantitative information about the uranium in a uranium ore using a standard addition approach. The uranium ore samples containing different concentrations of U were prepared by mixing raw ore powder with natural uranium oxide powders. Calibration sets of 0.2, 0.4, 0.6, 0.8 and 1.0 wt.% uranium concentrations within the uranium ore sample were achieved. A pulsed and Q-switched Nd:YAG laser at a wavelength of 532 nm was used as a light source. An echelle spectrometer that covers a 190–420 nm wavelength range is used to generate a calibration curve and determine the detection limit of uranium in the ore matrix. The neutral atomic-emission peak at a wavelength of 356.659 nm indicated a detection limit of ∼ 158 ppm for uranium, and the uranium concentration was determined in a raw ore sample that has an unknown quantity of uranium. - Highlights: ► The feasibility of LIBS application to monitor uranium element was carried out. ► The detection limit of U in ore was determined by a standard additional approach. ► Quantitative analyses of U concentration in a natural uranium ore were performed.

  3. Extraction X-ray fluorescence determination of gold in natural samples

    International Nuclear Information System (INIS)

    Dmitriev, S.N.; Shishkina, T.V.; Zhuravleva, E.L.; Chimehg, Zh.

    1990-01-01

    The behaviour of gold and other elements impeding its X-ray fluorescence (XRF) determination, namely, of zinc, lead, and arsenic, has been studied during their extraction by TBP from hydrochloric, nitric, and aqua regia solutions using solid extractant (SE(TBP)). Gold extraction from pulps after aqua regia leaching, with the gold distribution coefficient (D) being equal to about 10 4 , was observed as the most favourable one for the quantitative and selective recovery of gold. For extraction from hydrochloric solutions the D Au value does not depend on the gold content of initial solutions (10 -8 - 10 -4 M), but it decreases substantially with increasing extraction temperature (from 5x10 5 at 20 deg C to 9x10 3 at 70 deg C). An anomalously high distribution coefficient of lead (D Pb =10 3 ) was observed during extraction from hydrochloric solutions in the presence of chlorine. This fact could be explained by the formation of the chlorocomplexes of lead (IV). The XRF method of gold determination in natural samples has been developed, which includes the aqua regia decomposition of the samples, recovery of gold from the pulp after its leaching by SE(TBP) and back - extraction using a 0.025 M hot thiourea solution providing a thin sample film for secondary XRF spectrometry. For 25 g of the sample material the limit of determination is set at 0.01 g per ton (10 -6 %). The accuracy of the technique has been checked on different reference materials. The results agree within 10%. 16 refs.; 5 figs.; 1 tab

  4. 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

  5. Influence of Sampling on the Determination of Warfarin and Warfarin Alcohols in Oral Fluid

    Science.gov (United States)

    Lomonaco, Tommaso; Ghimenti, Silvia; Piga, Isabella; Biagini, Denise; Onor, Massimo; Fuoco, Roger; Di Francesco, Fabio

    2014-01-01

    Background and Objective The determination of warfarin, RS/SR- and RR/SS-warfarin alcohols in oral fluid may offer additional information to the INR assay. This study aimed to establish an optimized sampling technique providing the best correlation between the oral fluid and the unbound plasma concentrations of these compounds. Materials and Methods Samples of non-stimulated and stimulated oral fluid, and blood were collected from 14 patients undergoing warfarin therapy. After acidification, analytes were extracted with a dichloromethane/hexane mixture and determined by HPLC with fluorescence detection. Plasma samples were also ultrafiltered for the determination of the unbound fraction. The chromatographic separation was carried out in isocratic conditions with a phosphate buffer/methanol mobile phase on a C-18 reversed-phase column. The absence of interfering compounds was verified by HPLC-ESI-Q-TOF. Results Stimulation generally increased the oral fluid pH to values close to blood pH in about 6 minutes. The concentration of warfarin and RS/SR-warfarin alcohols in oral fluid followed the same trend, whereas the concentration of RR/SS-warfarin alcohols was not affected. Six minute stimulation with chewing gum followed by collection with a polyester swab was the best sampling procedure, with a good repeatability (RSD warfarin (r  =  0.92, p warfarin alcohols (r  =  0.84, p warfarin (r  =  0.78, p warfarin alcohols (r  =  0.81, p warfarin and RS/SR-warfarin alcohols suggests that oral fluid analysis could provide clinically useful information for the monitoring of anticoagulant therapy, complementary to the INR assay. PMID:25478864

  6. Sequential determination of environmental levels of isotopic thorium, uranium and the light rare earth elements within the terrestrial food chain by induced coupled plasma (ICP) and alpha spectrometry

    International Nuclear Information System (INIS)

    Linsalata, P.; Morse, R.; Ford, H.

    1986-01-01

    A radioecological study designed to measure soil to plant and soil to animal (livestock) transfer of Th, U, Ra and the light rare earth elements (REE) in typical and naturally-enhanced radiation environments required the development of radiochemical methods suitable for low-level determinations in a broad suite of environmental matrices including soil, edible vegetables and vegetation, and the major organs and tissues of various livestock. Earlier work has demonstrate the reliability of the methods summarized here for measuring the isotopic thorium and REE content of human feces, and that in the edible portions of various vegetables grown under field conditions. The very high degree of biological discrimination against Th and REE uptake in plants as well as in animal soft tissues necessitated the analysis of typical sample masses of 1-4 kg (fresh weight) to insure reasonably precise (eg., 10-20%) concentration estimates for most of the elements and isotopes of interest. As a result of the ''bone-seeking'' nature and relatively long retention times for these elements in skeletal tissue, typical analytical masses required for analysis of bone range from 40 to 70 g (fresh weight) except for the REE's in which a larger aliquot is recommended when determination is by induced coupled plasma spectrometry

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  8. De determination for young samples using the standardised OSL response of coarse-grain quartz

    International Nuclear Information System (INIS)

    Burbidge, C.I.; Duller, G.A.T.; Roberts, H.M.

    2006-01-01

    It has recently been shown that it is possible to construct standardised curves of the sensitivity corrected growth in optically stimulated luminescence (OSL) with exposure to ionising radiation, and that they may be used in the dating of quartz and polymineral samples. Standardised growth curves are particularly advantageous where measurement time is limited, as once they have been defined, only the natural signal and the response to a subsequent test dose are required in order to determine the equivalent dose of a sub-sample. The present study is concerned with the application of the standardised growth curve approach to OSL dating of Holocene age samples. Systematic changes in the shape of the standardised growth curve of coarse-grain quartz are identified as the size of the test dose is varied, because of non-proportionality between the test dose and the luminescence test response. The effect is characterised by fitting the change in gradient of the standardised growth curve as test dose is varied. An equation is defined to describe standardised growth as a function of regenerative dose and test dose. Regenerative dose responses of other samples in this study are treated as unknowns and recovered through different growth curves to compare precision and accuracy of various methods of D e determination. The standardised growth curve is found to yield similar precision to conventional fits of single aliquot regenerative data, but slightly poorer accuracy. The standardised growth curve approach was refined by incorporating the measurement of one regenerative response for each aliquot as well as its natural signal. Measurements of this additional data point for aliquots of 22 samples were used to adjust the standardised growth equation, improving its accuracy. The incorporation of this additional data point also indicated a systematic uncertainty of 2.4% in the estimates of D e

  9. Determination of colloidal and dissolved silver in water samples using colorimetric solid-phase extraction.

    Science.gov (United States)

    Hill, April A; Lipert, Robert J; Porter, Marc D

    2010-03-15

    The increase in bacterial resistance to antibiotics has led to resurgence in the use of silver as a biocidal agent in applications ranging from washing machine additives to the drinking water treatment system on the International Space Station (ISS). However, growing concerns about the possible toxicity of colloidal silver to bacteria, aquatic organisms and humans have led to recently issued regulations by the US EPA and FDA regarding the usage of silver. As part of an ongoing project, we have developed a rapid, simple method for determining total silver, both ionic (silver(I)) and colloidal, in 0.1-1mg/L aqueous samples, which spans the ISS potable water target of 0.3-0.5mg/L (total silver) and meets the US EPA limit of 0.1mg/L in drinking water. The method is based on colorimetric solid-phase extraction (C-SPE) and involves the extraction of silver(I) from water samples by passage through a solid-phase membrane impregnated with the colorimetric reagent DMABR (5-[4-(dimethylamino)benzylidene]rhodanine). Silver(I) exhaustively reacts with impregnated DMABR to form a colored compound, which is quantified using a handheld diffuse reflectance spectrophotometer. Total silver is determined by first passing the sample through a cartridge containing Oxone, which exhaustively oxidizes colloidal silver to dissolved silver(I). The method, which takes less than 2 min to complete and requires only approximately 1 mL of sample, has been validated through a series of tests, including a comparison with the ICP-MS analysis of a water sample from ISS that contained both silver(I) and colloidal silver. Potential earth-bound applications are also briefly discussed. Copyright (c) 2009 Elsevier B.V. All rights reserved.

  10. Hydrogen concentration determination in pressure tube samples using differential scanning calorimetry (dsc)

    International Nuclear Information System (INIS)

    Marinescu, R.; Mincu, M.

    2015-01-01

    Zirconium alloys are widely used as a structural material in nuclear reactors. It is known that zirconium based cladding alloys absorb hydrogen as a result of service in a pressurized water reactor. Hydrogen absorbed (during operation of the reactor) in the zirconium alloy, out of which the pressure tube is made, is one of the major factors determining the life time of the pressure tube. For monitoring the hydrides, samples of the pressure tube are periodically taken and analyzed. At normal reactor operating temperature, hydrogen has limited solubility in the zirconium lattice and precipitates out of solid solution as zirconium hydride when the solid solubility is exceeded. As a consequences material characterization of Zr-2.5Nb CANDU pressure tubes is required after manufacturing but also during the operation to assess its structural integrity and to predict its behavior until the next in-service inspection. Hydrogen and deuterium concentration determination is one of the most important parameters to be evaluated during the experimental tests. Hydrogen present in zirconium alloys has a strong effect of weakening. Following the zirconium-hydrogen reaction, the resulting zirconium hydride precipitates in the mass of material. Weakening of the material, due to the presence of 10 ppm of precipitated hydrogen significantly affects some of its properties. The concentration of hydrogen in a sample can be determined by several methods, one of them being the differential scanning calorimetry (DSC). The principle of the method consists in measuring the difference between the amount of heat required to raise the temperature of a sample and a reference to a certain value. The experiments were made using a TA Instruments DSC Q2000 calorimeter. This paper contains experimental work for hydrogen concentration determination by Differential Scanning Calorimetry (DSC) method. Also, the reproducibility and accuracy of the method used at INR Pitesti are presented. (authors)

  11. Presence and significant determinants of cognitive impairment in a large sample of patients with multiple sclerosis.

    Directory of Open Access Journals (Sweden)

    Martina Borghi

    Full Text Available OBJECTIVES: To investigate the presence and the nature of cognitive impairment in a large sample of patients with Multiple Sclerosis (MS, and to identify clinical and demographic determinants of cognitive impairment in MS. METHODS: 303 patients with MS and 279 healthy controls were administered the Brief Repeatable Battery of Neuropsychological tests (BRB-N; measures of pre-morbid verbal competence and neuropsychiatric measures were also administered. RESULTS: Patients and healthy controls were matched for age, gender, education and pre-morbid verbal Intelligence Quotient. Patients presenting with cognitive impairment were 108/303 (35.6%. In the overall group of participants, the significant predictors of the most sensitive BRB-N scores were: presence of MS, age, education, and Vocabulary. The significant predictors when considering MS patients only were: course of MS, age, education, vocabulary, and depression. Using logistic regression analyses, significant determinants of the presence of cognitive impairment in relapsing-remitting MS patients were: duration of illness (OR = 1.053, 95% CI = 1.010-1.097, p = 0.015, Expanded Disability Status Scale score (OR = 1.247, 95% CI = 1.024-1.517, p = 0.028, and vocabulary (OR = 0.960, 95% CI = 0.936-0.984, p = 0.001, while in the smaller group of progressive MS patients these predictors did not play a significant role in determining the cognitive outcome. CONCLUSIONS: Our results corroborate the evidence about the presence and the nature of cognitive impairment in a large sample of patients with MS. Furthermore, our findings identify significant clinical and demographic determinants of cognitive impairment in a large sample of MS patients for the first time. Implications for further research and clinical practice were discussed.

  12. Determination of total alpha activity index in samples of radioactive wastes

    International Nuclear Information System (INIS)

    Galicia C, F. J.

    2015-01-01

    This study aimed to develop a methodology of preparation and quantification of samples containing radionuclides beta and/or alpha emitters, to determine the rates of alpha and beta total activity of radioactive waste samples. For this, a device of planchettes preparer was designed, to assist the planchettes preparation in a controlled environment and free of corrosive vapors. Planchettes were prepared in three means: nitrate, carbonate and sulfate, to different mass thickness, natural uranium (alpha and beta emitter) and in case of Sr-90 (beta emitter pure) only in half nitrate; and these planchettes were quantified in an alpha/beta counter, in order to construct the self-absorption curves for alpha and beta particles. These curves are necessary to determine the rate of alpha-beta activity of any sample because they provide the self-absorption correction factor to be applied in calculating the index. Samples with U were prepared with the help of the device of planchettes preparer and subsequently were analyzed in the proportional counter Mpc-100 Pic brand. Samples with Sr-90 were prepared without the device to see if there was a different behavior with respect to obtaining mass thickness. Similarly they were calcined and carried out count in the Mpc-100. To perform the count, first the parameters of counter operating were determined: operating voltages for alpha and beta particles 630 and 1500 V respectively, a count routine was generated where the time and count type were adjusted, and counting efficiencies for alpha and beta particles, with the aid of calibration sources of 210 Po for alphas and 90 Sr for betas. According to the results, the counts per minute will decrease as increasing the mass thickness of the sample (self-absorption curve), adjusting this behavior to an exponential function in all cases studied. The minor self-absorption of alpha and beta particles in the case of U was obtained in sulfate medium. The self-absorption curves of Sr-90 follow the

  13. Determination of arsenic species in rice samples using CPE and ETAAS.

    Science.gov (United States)

    Costa, Bruno Elias Dos Santos; Coelho, Nívia Maria Melo; Coelho, Luciana Melo

    2015-07-01

    A highly sensitive and selective procedure for the determination of arsenate and total arsenic in food by electrothermal atomic absorption spectrometry after cloud point extraction (ETAAS/CPE) was developed. The procedure is based on the formation of a complex of As(V) ions with molybdate in the presence of 50.0 mmol L(-1) sulfuric acid. The complex was extracted into the surfactant-rich phase of 0.06% (w/v) Triton X-114. The variables affecting the complex formation, extraction and phase separation were optimized using factorial designs. Under the optimal conditions, the calibration graph was linear in the range of 0.05-10.0 μg L(-1). The detection and quantification limits were 10 and 33 ng L(-1), respectively and the corresponding value for the relative standard deviation for 10 replicates was below 5%. Recovery values of between 90.8% and 113.1% were obtained for spiked samples. The accuracy of the method was evaluated by comparison with the results obtained for the analysis of a rice flour sample (certified material IRMM-804) and no significant difference at the 95% confidence level was observed. The method was successfully applied to the determination of As(V) and total arsenic in rice samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

  14. Reverse flow injection spectrophotometric determination of thiram and nabam fungicides in natural water samples

    International Nuclear Information System (INIS)

    Asghar, M.; Yaqoob, M.; Nabi, A.

    2014-01-01

    A reverse flow injection (rFI) spectrophotometric method is reported for determination of thiram and nabam fungicides in natural water samples. The method is based on the reduction of iron(III) in the presence of thiram/nabam in acidic medium at 60 degree C and formation of iron(II)-ferricyanide complex was measured at 790 nm. The limits of detection (3s blank) were 0.01 and 0.05 micro g mL1 for thiram and nabam respectively with a sample throughput of 60 h1. Calibration graphs were linear over the range of 0.02 - 8.0 micro g mL1 (R2 = 0.9999, n = 8) and 0.1 - 30 micro g mL1 (R2 = 0.9982, n = 10) for thiram and nabam with relative standard deviations (RSDs; n = 3) in the range of 0.8 - 1.6% respectively. Experimental parameters and potential interferences were examined. Thiram and nabam were determined in natural water samples using solid-phase extraction (SPE) procedure and recoveries were in the range of 93+-3 - 105+-2% and 87+-4 - 102+-3% respectively. The results obtained were not significantly different compared with a HPLC method. (author)

  15. Sources of variability in the determination by evaporation method of gross alpha activity in water samples

    Energy Technology Data Exchange (ETDEWEB)

    Baeza, A.; Corbacho, J.A. [LARUEX, Caceres (Spain). Environmental Radioactivity Lab.

    2013-07-01

    Determining the gross alpha activity concentration of water samples is one way to screen for waters whose radionuclide content is so high that its consumption could imply surpassing the Total Indicative Dose as defined in European Directive 98/83/EC. One of the most commonly used methods to prepare the sources to measure gross alpha activity in water samples is desiccation. Its main advantages are the simplicity of the procedure, the low cost of source preparation, and the possibility of simultaneously determining the gross beta activity. The preparation of the source, the construction of the calibration curves, and the measurement procedure itself involve, however, various factors that may introduce sufficient variability into the results to significantly affect the screening process. We here identify the main sources of this variability, and propose specific procedures to follow in the desiccation process that will reduce the uncertainties, and ensure that the result is indeed representative of the sum of the activities of the alpha emitters present in the sample. (orig.)

  16. A modified FOX-1 method for Micro-determination of hydrogen peroxide in honey samples.

    Science.gov (United States)

    Li, Dan; Wang, Meng; Cheng, Ni; Xue, Xiaofeng; Wu, Liming; Cao, Wei

    2017-12-15

    Hydrogen peroxide (H 2 O 2 ) is a major antibacterial activity-associated biomarker in honey. Measurement of endogenous H 2 O 2 in honey is of great value in prediction of the H 2 O 2 -depended antibacterial activity and characterization or selection of honey samples for their use as an antibacterial agent or natural food preservative. Considering current methods for H 2 O 2 determination are either time-consuming or complicated with their high-cost, a study was conducted to modify and validate the spectrophotometry-based ferrous oxidation-xylenol orange (FOX-1) method for micro-determination of H 2 O 2 in honey samples. The result suggested that the proposed FOX-1 method is fast, sensitive, precise and repeatable. The method was successfully applied for the analysis of a total of 35 honey samples from 5 floral origins and 33 geographical origins. The proposed method is low-cost and easy-to-run, and it can be considered by researchers and industry for routine analysis. Copyright © 2017 Elsevier Ltd. All rights reserved.

  17. Sensitive Electrochemical Determination of Gallic Acid: Application in Estimation of Total Polyphenols in Plant Samples

    Directory of Open Access Journals (Sweden)

    Mohammad Ali Sheikh-Mohseni

    2016-12-01

    Full Text Available A modified electrode was prepared by modification of the carbon paste electrode (CPE with graphene nano-sheets. The fabricated modified electrode exhibited an electrocatalytic activity toward gallic acid (GA oxidation because of good conductivity, low electron transfer resistance and catalytic effect. The graphene modified CPE had a lower overvoltage and enhanced electrical current respect to the bare CPE for the oxidation of GA. The oxidation potential of GA decreased more than 210 mV by the modified electrode. The modified electrode responded to the GA in the concentration range of 3.0 × 10-5-1.5 × 10-4 M with high sensitivity by the technique of differential pulse voltammetry. Also, detection limit of 1.1 × 10-7 M was obtained by this modified electrode for GA. This electrode was used for the successful determination of GA in plant samples. Therefore, the content of total polyphenols in plant samples can be determined by the proposed modified electrode based on the concentration of GA in the sample.

  18. Gas chromatographic determination of cholesterol from food samples using extraction/saponification method

    International Nuclear Information System (INIS)

    Ali, Z.M.; Soomro, A.S.A.

    2007-01-01

    A simple and fast one-step extraction/saponification with Na/OH/KOH (Ethanolic, Sodium Hydroxide/Potassium Hydroxide was compared and validated for determination of cholesterol from locally available 10 edible oil and egg samples. The importance of the use of edible oils and eggs in routine diet is unquestionable, but presence of cholesterol is considered as a risk factor for coronary heart disease and hypertension. The lowering of cholesterol level in order to reduce the risk is widely accepted. The cholesterol in the edible oil and eggs was determined by gas chromatography, through elution from the column (2x3 mm i.d) packed with 3% OV-I01, on Chromosorb G/'NAW 80-100 mesh size at 250-300C with programmed heating rate of 3 degree C/min. Nitrogen gas flow rate was 40 ml/min. The cholesterol samples were run under the conditions after selective extraction in diethyl ether. The calibration was linear within 50-500 IJg/ml concentration range. The amount of cholesterol detected were from 12.92-18.05 mg/g in edible oil and 117.54-143.42 mg/g in egg samples with RSD 1.3-2.7%. (author)

  19. HPLC determination of chlorine in air and water samples following precolumn derivatization to 4-bromoacetanilide

    Energy Technology Data Exchange (ETDEWEB)

    Jain, A. (Rani Durgavati Univ., Jabalpur (India). Dept. of Chemistry); Verma, K.K. (Rani Durgavati Univ., Jabalpur (India). Dept. of Chemistry)

    1993-11-01

    Chlorine has been determined in air and water samples by a rapid and sensitive method entailing precolumn derivatization to 4-bromoacetanilide. A mixed potassium bromide - acetanilide reagent was used as a trapping agent for chlorine in air, and for its derivatization. The 4-bromoacetanilide formed was determined by reversed-phase HPLC on an ODS column, using methanol-water, 65:35 (v/v) as mobile phase; detection was at 240 nm. A rectilinear calibration graph was obtained for the range 0.1-30 [mu]g mL[sup -1] chlorine; the limit of detection found to be 0.01 [mu]g mL[sup -1]. The precolumn derivative has been found to have a shelf-life of at least 21 days; this enables the use of the method for samples transported from the field to the analytical laboratory, or the testing of a variety of conditions for chlorine scrubbing studies without the need for immediate analysis of samples. Humic substances do not cause any interference with the proposed method and the presence of nitrite does not lead to artificially high results and consequent misleading conclusions of the presence of high levels of chlorine. (orig.)

  20. HPLC determination of chlorine in air and water samples following precolumn derivatization to 4-bromoacetanilide

    International Nuclear Information System (INIS)

    Jain, A.; Verma, K.K.

    1993-01-01

    Chlorine has been determined in air and water samples by a rapid and sensitive method entailing precolumn derivatization to 4-bromoacetanilide. A mixed potassium bromide - acetanilide reagent was used as a trapping agent for chlorine in air, and for its derivatization. The 4-bromoacetanilide formed was determined by reversed-phase HPLC on an ODS column, using methanol-water, 65:35 (v/v) as mobile phase; detection was at 240 nm. A rectilinear calibration graph was obtained for the range 0.1-30 μg mL -1 chlorine; the limit of detection found to be 0.01 μg mL -1 . The precolumn derivative has been found to have a shelf-life of at least 21 days; this enables the use of the method for samples transported from the field to the analytical laboratory, or the testing of a variety of conditions for chlorine scrubbing studies without the need for immediate analysis of samples. Humic substances do not cause any interference with the proposed method and the presence of nitrite does not lead to artificially high results and consequent misleading conclusions of the presence of high levels of chlorine. (orig.)