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Sample records for sample analysis techniques

  1. Microextraction sample preparation techniques in biomedical analysis.

    Science.gov (United States)

    Szultka, Malgorzata; Pomastowski, Pawel; Railean-Plugaru, Viorica; Buszewski, Boguslaw

    2014-11-01

    Biologically active compounds are found in biological samples at relatively low concentration levels. The sample preparation of target compounds from biological, pharmaceutical, environmental, and food matrices is one of the most time-consuming steps in the analytical procedure. The microextraction techniques are dominant. Metabolomic studies also require application of proper analytical technique for the determination of endogenic metabolites present in biological matrix on trace concentration levels. Due to the reproducibility of data, precision, relatively low cost of the appropriate analysis, simplicity of the determination, and the possibility of direct combination of those techniques with other methods (combination types on-line and off-line), they have become the most widespread in routine determinations. Additionally, sample pretreatment procedures have to be more selective, cheap, quick, and environmentally friendly. This review summarizes the current achievements and applications of microextraction techniques. The main aim is to deal with the utilization of different types of sorbents for microextraction and emphasize the use of new synthesized sorbents as well as to bring together studies concerning the systematic approach to method development. This review is dedicated to the description of microextraction techniques and their application in biomedical analysis. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Development of environmental sample analysis techniques for safeguards

    International Nuclear Information System (INIS)

    Magara, Masaaki; Hanzawa, Yukiko; Esaka, Fumitaka

    1999-01-01

    JAERI has been developing environmental sample analysis techniques for safeguards and preparing a clean chemistry laboratory with clean rooms. Methods to be developed are a bulk analysis and a particle analysis. In the bulk analysis, Inductively-Coupled Plasma Mass Spectrometer or Thermal Ionization Mass Spectrometer are used to measure nuclear materials after chemical treatment of sample. In the particle analysis, Electron Probe Micro Analyzer and Secondary Ion Mass Spectrometer are used for elemental analysis and isotopic analysis, respectively. The design of the clean chemistry laboratory has been carried out and construction will be completed by the end of March, 2001. (author)

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

    Science.gov (United States)

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

    2014-12-01

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

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

    Science.gov (United States)

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

    2014-01-01

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

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

    Science.gov (United States)

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

    2012-01-01

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

  6. Techniques of sample attack used in soil and mineral analysis. Phase I

    International Nuclear Information System (INIS)

    Chiu, N.W.; Dean, J.R.; Sill, C.W.

    1984-07-01

    Several techniques of sample attack for the determination of radioisotopes are reviewed. These techniques include: 1) digestion with nitric or hydrochloric acid in Parr digestion bomb, 2) digestion with a mixture of nitric and hydrochloric acids, 3) digestion with a mixture of hydrofluoric, nitric and perchloric acids, and 4) fusion with sodium carbonate, potassium fluoride or alkali pyrosulfates. The effectiveness of these techniques to decompose various soils and minerals containing radioisotopes such as lead-210 uranium, thorium and radium-226 are discussed. The combined procedure of potassium fluoride fusion followed by alkali pyrosulfate fusion is recommended for radium-226, uranium and thorium analysis. This technique guarantees the complete dissolution of samples containing refractory materials such as silica, silicates, carbides, oxides and sulfates. For the lead-210 analysis, the procedure of digestion with a mixture of hydrofluoric, nitric and perchloric acids followed by fusion with alkali pyrosulfate is recommended. These two procedures are detailed. Schemes for the sequential separation of the radioisotopes from a dissolved sample solution are outlined. Procedures for radiochemical analysis are suggested

  7. Prompt Gamma Activation Analysis (PGAA): Technique of choice for nondestructive bulk analysis of returned comet samples

    International Nuclear Information System (INIS)

    Lindstrom, D.J.; Lindstrom, R.M.

    1989-01-01

    Prompt gamma activation analysis (PGAA) is a well-developed analytical technique. The technique involves irradiation of samples in an external neutron beam from a nuclear reactor, with simultaneous counting of gamma rays produced in the sample by neutron capture. Capture of neutrons leads to excited nuclei which decay immediately with the emission of energetic gamma rays to the ground state. PGAA has several advantages over other techniques for the analysis of cometary materials: (1) It is nondestructive; (2) It can be used to determine abundances of a wide variety of elements, including most major and minor elements (Na, Mg, Al, Si, P, K, Ca, Ti, Cr, Mn, Fe, Co, Ni), volatiles (H, C, N, F, Cl, S), and some trace elements (those with high neutron capture cross sections, including B, Cd, Nd, Sm, and Gd); and (3) It is a true bulk analysis technique. Recent developments should improve the technique's sensitivity and accuracy considerably

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-12-01

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

  10. Critical evaluation of sample pretreatment techniques.

    Science.gov (United States)

    Hyötyläinen, Tuulia

    2009-06-01

    Sample preparation before chromatographic separation is the most time-consuming and error-prone part of the analytical procedure. Therefore, selecting and optimizing an appropriate sample preparation scheme is a key factor in the final success of the analysis, and the judicious choice of an appropriate procedure greatly influences the reliability and accuracy of a given analysis. The main objective of this review is to critically evaluate the applicability, disadvantages, and advantages of various sample preparation techniques. Particular emphasis is placed on extraction techniques suitable for both liquid and solid samples.

  11. Proteomic Challenges: Sample Preparation Techniques for Microgram-Quantity Protein Analysis from Biological Samples

    Directory of Open Access Journals (Sweden)

    Peter Feist

    2015-02-01

    Full Text Available Proteins regulate many cellular functions and analyzing the presence and abundance of proteins in biological samples are central focuses in proteomics. The discovery and validation of biomarkers, pathways, and drug targets for various diseases can be accomplished using mass spectrometry-based proteomics. However, with mass-limited samples like tumor biopsies, it can be challenging to obtain sufficient amounts of proteins to generate high-quality mass spectrometric data. Techniques developed for macroscale quantities recover sufficient amounts of protein from milligram quantities of starting material, but sample losses become crippling with these techniques when only microgram amounts of material are available. To combat this challenge, proteomicists have developed micro-scale techniques that are compatible with decreased sample size (100 μg or lower and still enable excellent proteome coverage. Extraction, contaminant removal, protein quantitation, and sample handling techniques for the microgram protein range are reviewed here, with an emphasis on liquid chromatography and bottom-up mass spectrometry-compatible techniques. Also, a range of biological specimens, including mammalian tissues and model cell culture systems, are discussed.

  12. Proteomic Challenges: Sample Preparation Techniques for Microgram-Quantity Protein Analysis from Biological Samples

    Science.gov (United States)

    Feist, Peter; Hummon, Amanda B.

    2015-01-01

    Proteins regulate many cellular functions and analyzing the presence and abundance of proteins in biological samples are central focuses in proteomics. The discovery and validation of biomarkers, pathways, and drug targets for various diseases can be accomplished using mass spectrometry-based proteomics. However, with mass-limited samples like tumor biopsies, it can be challenging to obtain sufficient amounts of proteins to generate high-quality mass spectrometric data. Techniques developed for macroscale quantities recover sufficient amounts of protein from milligram quantities of starting material, but sample losses become crippling with these techniques when only microgram amounts of material are available. To combat this challenge, proteomicists have developed micro-scale techniques that are compatible with decreased sample size (100 μg or lower) and still enable excellent proteome coverage. Extraction, contaminant removal, protein quantitation, and sample handling techniques for the microgram protein range are reviewed here, with an emphasis on liquid chromatography and bottom-up mass spectrometry-compatible techniques. Also, a range of biological specimens, including mammalian tissues and model cell culture systems, are discussed. PMID:25664860

  13. Proteomic challenges: sample preparation techniques for microgram-quantity protein analysis from biological samples.

    Science.gov (United States)

    Feist, Peter; Hummon, Amanda B

    2015-02-05

    Proteins regulate many cellular functions and analyzing the presence and abundance of proteins in biological samples are central focuses in proteomics. The discovery and validation of biomarkers, pathways, and drug targets for various diseases can be accomplished using mass spectrometry-based proteomics. However, with mass-limited samples like tumor biopsies, it can be challenging to obtain sufficient amounts of proteins to generate high-quality mass spectrometric data. Techniques developed for macroscale quantities recover sufficient amounts of protein from milligram quantities of starting material, but sample losses become crippling with these techniques when only microgram amounts of material are available. To combat this challenge, proteomicists have developed micro-scale techniques that are compatible with decreased sample size (100 μg or lower) and still enable excellent proteome coverage. Extraction, contaminant removal, protein quantitation, and sample handling techniques for the microgram protein range are reviewed here, with an emphasis on liquid chromatography and bottom-up mass spectrometry-compatible techniques. Also, a range of biological specimens, including mammalian tissues and model cell culture systems, are discussed.

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

    International Nuclear Information System (INIS)

    Valkovic, V.

    1983-11-01

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

  15. Stratified source-sampling techniques for Monte Carlo eigenvalue analysis

    International Nuclear Information System (INIS)

    Mohamed, A.

    1998-01-01

    In 1995, at a conference on criticality safety, a special session was devoted to the Monte Carlo ''Eigenvalue of the World'' problem. Argonne presented a paper, at that session, in which the anomalies originally observed in that problem were reproduced in a much simplified model-problem configuration, and removed by a version of stratified source-sampling. In this paper, stratified source-sampling techniques are generalized and applied to three different Eigenvalue of the World configurations which take into account real-world statistical noise sources not included in the model problem, but which differ in the amount of neutronic coupling among the constituents of each configuration. It is concluded that, in Monte Carlo eigenvalue analysis of loosely-coupled arrays, the use of stratified source-sampling reduces the probability of encountering an anomalous result over that if conventional source-sampling methods are used. However, this gain in reliability is substantially less than that observed in the model-problem results

  16. Large-volume constant-concentration sampling technique coupling with surface-enhanced Raman spectroscopy for rapid on-site gas analysis

    Science.gov (United States)

    Zhang, Zhuomin; Zhan, Yisen; Huang, Yichun; Li, Gongke

    2017-08-01

    In this work, a portable large-volume constant-concentration (LVCC) sampling technique coupling with surface-enhanced Raman spectroscopy (SERS) was developed for the rapid on-site gas analysis based on suitable derivatization methods. LVCC sampling technique mainly consisted of a specially designed sampling cell including the rigid sample container and flexible sampling bag, and an absorption-derivatization module with a portable pump and a gas flowmeter. LVCC sampling technique allowed large, alterable and well-controlled sampling volume, which kept the concentration of gas target in headspace phase constant during the entire sampling process and made the sampling result more representative. Moreover, absorption and derivatization of gas target during LVCC sampling process were efficiently merged in one step using bromine-thiourea and OPA-NH4+ strategy for ethylene and SO2 respectively, which made LVCC sampling technique conveniently adapted to consequent SERS analysis. Finally, a new LVCC sampling-SERS method was developed and successfully applied for rapid analysis of trace ethylene and SO2 from fruits. It was satisfied that trace ethylene and SO2 from real fruit samples could be actually and accurately quantified by this method. The minor concentration fluctuations of ethylene and SO2 during the entire LVCC sampling process were proved to be samples were achieved in range of 95.0-101% and 97.0-104% respectively. It is expected that portable LVCC sampling technique would pave the way for rapid on-site analysis of accurate concentrations of trace gas targets from real samples by SERS.

  17. Non destructive multi elemental analysis using prompt gamma neutron activation analysis techniques: Preliminary results for concrete sample

    Energy Technology Data Exchange (ETDEWEB)

    Dahing, Lahasen Normanshah [School of Applied Physics, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor, Malaysia and Malaysian Nuclear Agency (Nuklear Malaysia), Bangi 43000, Kajang (Malaysia); Yahya, Redzuan [School of Applied Physics, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor (Malaysia); Yahya, Roslan; Hassan, Hearie [Malaysian Nuclear Agency (Nuklear Malaysia), Bangi 43000, Kajang (Malaysia)

    2014-09-03

    In this study, principle of prompt gamma neutron activation analysis has been used as a technique to determine the elements in the sample. The system consists of collimated isotopic neutron source, Cf-252 with HPGe detector and Multichannel Analysis (MCA). Concrete with size of 10×10×10 cm{sup 3} and 15×15×15 cm{sup 3} were analysed as sample. When neutrons enter and interact with elements in the concrete, the neutron capture reaction will occur and produce characteristic prompt gamma ray of the elements. The preliminary result of this study demonstrate the major element in the concrete was determined such as Si, Mg, Ca, Al, Fe and H as well as others element, such as Cl by analysis the gamma ray lines respectively. The results obtained were compared with NAA and XRF techniques as a part of reference and validation. The potential and the capability of neutron induced prompt gamma as tool for multi elemental analysis qualitatively to identify the elements present in the concrete sample discussed.

  18. Improved mesh based photon sampling techniques for neutron activation analysis

    International Nuclear Information System (INIS)

    Relson, E.; Wilson, P. P. H.; Biondo, E. D.

    2013-01-01

    The design of fusion power systems requires analysis of neutron activation of large, complex volumes, and the resulting particles emitted from these volumes. Structured mesh-based discretization of these problems allows for improved modeling in these activation analysis problems. Finer discretization of these problems results in large computational costs, which drives the investigation of more efficient methods. Within an ad hoc subroutine of the Monte Carlo transport code MCNP, we implement sampling of voxels and photon energies for volumetric sources using the alias method. The alias method enables efficient sampling of a discrete probability distribution, and operates in 0(1) time, whereas the simpler direct discrete method requires 0(log(n)) time. By using the alias method, voxel sampling becomes a viable alternative to sampling space with the 0(1) approach of uniformly sampling the problem volume. Additionally, with voxel sampling it is straightforward to introduce biasing of volumetric sources, and we implement this biasing of voxels as an additional variance reduction technique that can be applied. We verify our implementation and compare the alias method, with and without biasing, to direct discrete sampling of voxels, and to uniform sampling. We study the behavior of source biasing in a second set of tests and find trends between improvements and source shape, material, and material density. Overall, however, the magnitude of improvements from source biasing appears to be limited. Future work will benefit from the implementation of efficient voxel sampling - particularly with conformal unstructured meshes where the uniform sampling approach cannot be applied. (authors)

  19. Multi-element analysis of lubricant oil by WDXRF technique using thin-film sample preparation

    International Nuclear Information System (INIS)

    Scapin, M. A.; Salvador, V. L. R.; Lopes, C. D.; Sato, I. M.

    2006-01-01

    The quantitative analysis of the chemical elements in matrices like oils or gels represents a challenge for the analytical chemists. The classics methods or instrumental techniques such as atomic absorption spectrometry (AAS) and plasma optical emission spectrometry (ICP-OES) need chemical treatments, mainly sample dissolution and degradation processes. X-ray fluorescence technique allows a direct and multi-element analysis without previous sample treatments. In this work, a sensible method for the determination of elements Mg, Al, Si, P, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Mo, Ag, Sn, Ba and Pb in lubricating oil is presented. The x-ray fluorescence (WDXRF) technique using linear regression method and thin film sample preparation was used. The validation of the methodology (repeatability and accuracy) was obtained by the analysis of the standard reference materials SRM Alpha AESAR lot 703527D, applying the Chauvenet, Cochrane, ANOVA and Z-score statistical tests. The method presents a relative standard deviation lower than 10% for all the elements, except for Pb determination (RSD Pb 15%). The Z-score values for all the elements were in the range -2 < Z < 2, indicating a very good accuracy.(Full text)

  20. Large Sample Neutron Activation Analysis of Heterogeneous Samples

    International Nuclear Information System (INIS)

    Stamatelatos, I.E.; Vasilopoulou, T.; Tzika, F.

    2018-01-01

    A Large Sample Neutron Activation Analysis (LSNAA) technique was developed for non-destructive analysis of heterogeneous bulk samples. The technique incorporated collimated scanning and combining experimental measurements and Monte Carlo simulations for the identification of inhomogeneities in large volume samples and the correction of their effect on the interpretation of gamma-spectrometry data. Corrections were applied for the effect of neutron self-shielding, gamma-ray attenuation, geometrical factor and heterogeneous activity distribution within the sample. A benchmark experiment was performed to investigate the effect of heterogeneity on the accuracy of LSNAA. Moreover, a ceramic vase was analyzed as a whole demonstrating the feasibility of the technique. The LSNAA results were compared against results obtained by INAA and a satisfactory agreement between the two methods was observed. This study showed that LSNAA is a technique capable to perform accurate non-destructive, multi-elemental compositional analysis of heterogeneous objects. It also revealed the great potential of the technique for the analysis of precious objects and artefacts that need to be preserved intact and cannot be damaged for sampling purposes. (author)

  1. Nonactivation interaction techniques in the analysis of environmental samples

    International Nuclear Information System (INIS)

    Tolgyessy, J.

    1986-01-01

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

  2. Comparison of correlation analysis techniques for irregularly sampled time series

    Directory of Open Access Journals (Sweden)

    K. Rehfeld

    2011-06-01

    Full Text Available Geoscientific measurements often provide time series with irregular time sampling, requiring either data reconstruction (interpolation or sophisticated methods to handle irregular sampling. We compare the linear interpolation technique and different approaches for analyzing the correlation functions and persistence of irregularly sampled time series, as Lomb-Scargle Fourier transformation and kernel-based methods. In a thorough benchmark test we investigate the performance of these techniques.

    All methods have comparable root mean square errors (RMSEs for low skewness of the inter-observation time distribution. For high skewness, very irregular data, interpolation bias and RMSE increase strongly. We find a 40 % lower RMSE for the lag-1 autocorrelation function (ACF for the Gaussian kernel method vs. the linear interpolation scheme,in the analysis of highly irregular time series. For the cross correlation function (CCF the RMSE is then lower by 60 %. The application of the Lomb-Scargle technique gave results comparable to the kernel methods for the univariate, but poorer results in the bivariate case. Especially the high-frequency components of the signal, where classical methods show a strong bias in ACF and CCF magnitude, are preserved when using the kernel methods.

    We illustrate the performances of interpolation vs. Gaussian kernel method by applying both to paleo-data from four locations, reflecting late Holocene Asian monsoon variability as derived from speleothem δ18O measurements. Cross correlation results are similar for both methods, which we attribute to the long time scales of the common variability. The persistence time (memory is strongly overestimated when using the standard, interpolation-based, approach. Hence, the Gaussian kernel is a reliable and more robust estimator with significant advantages compared to other techniques and suitable for large scale application to paleo-data.

  3. Neutron activation analysis technique and X-ray fluorescence in bovine liver sample

    International Nuclear Information System (INIS)

    Maihara, V.A.; Favaro, D.I.T.; Vasconcellos, M.B.A.; Sato, I.M.; Salvador, V.L.

    2002-01-01

    Many analytical techniques have been used in food and diet analysis in order to determine a great number of nutritional elements, ranging from percentage to ng g -1 , with high sensitivity and accuracy. Instrumental Neutron activation Analysis (INAA) has been employed to certificate many trace elements in biological reference materials. More recently, the X-Ray Fluorescence (FRX-WD) has been also used to determine some essential elements in food samples. The INAA has been applied in nutrition studies in our laboratory at IPEN since the 80 s. For the development of analytical methodologies the use of the reference materials with the same characteristics of the sample analyzed is essential. Several Brazilian laboratories do not have conditions to use these materials due their high cost.In this paper preliminary results of commercial bovine liver sample analyses obtained by INAA and WD-XRF methods are presented. This sample was prepared to be a Brazilian candidate of reference material for a group of laboratories participating in a research project sponsored by FAPESP. The concentrations of some elements like Cl, K, Na, P, S and trace elements Br, Ca, Co, Cu, Fe, Mg, Mn, Mo, Rb, Se and Zn were determined by INAA and WD-XFR. For validation methodology of both techniques, NIST SRM 1577b Bovine Liver reference material was analyzed and the detection limits were calculated. The concentrations of elements determined by both analytical techniques were compared by using the Student's t-test and for Cl, Cu, Fe, K, Mg, Na, Rn and Zn the results do show no statistical difference for 95% significance level. (author)

  4. Large-volume constant-concentration sampling technique coupling with surface-enhanced Raman spectroscopy for rapid on-site gas analysis.

    Science.gov (United States)

    Zhang, Zhuomin; Zhan, Yisen; Huang, Yichun; Li, Gongke

    2017-08-05

    In this work, a portable large-volume constant-concentration (LVCC) sampling technique coupling with surface-enhanced Raman spectroscopy (SERS) was developed for the rapid on-site gas analysis based on suitable derivatization methods. LVCC sampling technique mainly consisted of a specially designed sampling cell including the rigid sample container and flexible sampling bag, and an absorption-derivatization module with a portable pump and a gas flowmeter. LVCC sampling technique allowed large, alterable and well-controlled sampling volume, which kept the concentration of gas target in headspace phase constant during the entire sampling process and made the sampling result more representative. Moreover, absorption and derivatization of gas target during LVCC sampling process were efficiently merged in one step using bromine-thiourea and OPA-NH 4 + strategy for ethylene and SO 2 respectively, which made LVCC sampling technique conveniently adapted to consequent SERS analysis. Finally, a new LVCC sampling-SERS method was developed and successfully applied for rapid analysis of trace ethylene and SO 2 from fruits. It was satisfied that trace ethylene and SO 2 from real fruit samples could be actually and accurately quantified by this method. The minor concentration fluctuations of ethylene and SO 2 during the entire LVCC sampling process were proved to be gas targets from real samples by SERS. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. ANALYSIS OF MONTE CARLO SIMULATION SAMPLING TECHNIQUES ON SMALL SIGNAL STABILITY OF WIND GENERATOR- CONNECTED POWER SYSTEM

    Directory of Open Access Journals (Sweden)

    TEMITOPE RAPHAEL AYODELE

    2016-04-01

    Full Text Available Monte Carlo simulation using Simple Random Sampling (SRS technique is popularly known for its ability to handle complex uncertainty problems. However, to produce a reasonable result, it requires huge sample size. This makes it to be computationally expensive, time consuming and unfit for online power system applications. In this article, the performance of Latin Hypercube Sampling (LHS technique is explored and compared with SRS in term of accuracy, robustness and speed for small signal stability application in a wind generator-connected power system. The analysis is performed using probabilistic techniques via eigenvalue analysis on two standard networks (Single Machine Infinite Bus and IEEE 16–machine 68 bus test system. The accuracy of the two sampling techniques is determined by comparing their different sample sizes with the IDEAL (conventional. The robustness is determined based on a significant variance reduction when the experiment is repeated 100 times with different sample sizes using the two sampling techniques in turn. Some of the results show that sample sizes generated from LHS for small signal stability application produces the same result as that of the IDEAL values starting from 100 sample size. This shows that about 100 sample size of random variable generated using LHS method is good enough to produce reasonable results for practical purpose in small signal stability application. It is also revealed that LHS has the least variance when the experiment is repeated 100 times compared to SRS techniques. This signifies the robustness of LHS over that of SRS techniques. 100 sample size of LHS produces the same result as that of the conventional method consisting of 50000 sample size. The reduced sample size required by LHS gives it computational speed advantage (about six times over the conventional method.

  6. The particle analysis based on FT-TIMS technique for swipe sample under the frame of nuclear safeguard

    International Nuclear Information System (INIS)

    Yang Tianli; Liu Xuemei; Liu Zhao; Tang Lei; Long Kaiming

    2008-06-01

    Under the frame of nuclear safeguard, the particles analysis for swipe sample is an advance mean to detect the undeclared uranium enriched facilities and undeclared uranium enriched activity. The technique of particle analysis based on fission track-thermal ionization mass spectrometry (FT-TIMS) for swipe sample have been built. The reliability and the experimental background for selecting particles consisting of uranium from swipe sample by FT method have been verified. In addition, the utilization coefficient of particles on the surface of swipe sample have also been tested. These works have provided the technique support for application in the area of nuclear verification. (authors)

  7. Radioisotope Sample Measurement Techniques in Medicine and Biology. Proceedings of the Symposium on Radioisotope Sample Measurement Techniques

    International Nuclear Information System (INIS)

    1965-01-01

    The medical and biological applications of radioisotopes depend on two basically different types of measurements, those on living subjects in vivo and those on samples in vitro. The International Atomic Energy Agency has in the past held several meetings on in vivo measurement techniques, notably whole-body counting and radioisotope scanning. The present volume contains the Proceedings of the first Symposium the Agency has organized to discuss the various aspects of techniques for sample measurement in vitro. The range of these sample measurement techniques is very wide. The sample may weigh a few milligrams or several hundred grams, and may be in the gaseous, liquid or solid state. Its radioactive content may consist of a single, known radioisotope or several unknown ones. The concentration of radioactivity may be low, medium or high. The measurements may be made manually or automatically and any one of the many radiation detectors now available may be used. The 53 papers presented at the Symposium illustrate the great variety of methods now in use for radioactive- sample measurements. The first topic discussed is gamma-ray spectrometry, which finds an increasing number of applications in sample measurements. Other sections of the Proceedings deal with: the use of computers in gamma-ray spectrometry and multiple tracer techniques; recent developments in activation analysis where both gamma-ray spectrometry and computing techniques are applied; thin-layer and paper radio chromatographic techniques for use with low energy beta-ray emitters; various aspects of liquid scintillation counting techniques in the measurement of alpha- and beta-ray emitters, including chemical and colour quenching; autoradiographic techniques; calibration of equipment; and standardization of radioisotopes. Finally, some applications of solid-state detectors are presented; this section may be regarded as a preview of important future developments. The meeting was attended by 203 participants

  8. Comparison of sampling techniques for use in SYVAC

    International Nuclear Information System (INIS)

    Dalrymple, G.J.

    1984-01-01

    The Stephen Howe review (reference TR-STH-1) recommended the use of a deterministic generator (DG) sampling technique for sampling the input values to the SYVAC (SYstems Variability Analysis Code) program. This technique was compared with Monte Carlo simple random sampling (MC) by taking a 1000 run case of SYVAC using MC as the reference case. The results show that DG appears relatively inaccurate for most values of consequence when used with 11 sample intervals. If 22 sample intervals are used then DG generates cumulative distribution functions that are statistically similar to the reference distribution. 400 runs of DG or MC are adequate to generate a representative cumulative distribution function. The MC technique appears to perform better than DG for the same number of runs. However, the DG predicts higher doses and in view of the importance of generating data in the high dose region this sampling technique with 22 sample intervals is recommended for use in SYVAC. (author)

  9. New materials for sample preparation techniques in bioanalysis.

    Science.gov (United States)

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

    2017-02-01

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

  10. Sample application of sensitivity/uncertainty analysis techniques to a groundwater transport problem. National Low-Level Waste Management Program

    International Nuclear Information System (INIS)

    Seitz, R.R.; Rood, A.S.; Harris, G.A.; Maheras, S.J.; Kotecki, M.

    1991-06-01

    The primary objective of this document is to provide sample applications of selected sensitivity and uncertainty analysis techniques within the context of the radiological performance assessment process. These applications were drawn from the companion document Guidelines for Sensitivity and Uncertainty Analyses of Low-Level Radioactive Waste Performance Assessment Computer Codes (S. Maheras and M. Kotecki, DOE/LLW-100, 1990). Three techniques are illustrated in this document: one-factor-at-a-time (OFAT) analysis, fractional factorial design, and Latin hypercube sampling. The report also illustrates the differences in sensitivity and uncertainty analysis at the early and latter stages of the performance assessment process, and potential pitfalls that can be encountered when applying the techniques. The emphasis is on application of the techniques as opposed to the actual results, since the results are hypothetical and are not based on site-specific conditions

  11. Application of digital sampling techniques to particle identification

    International Nuclear Information System (INIS)

    Bardelli, L.; Poggi, G.; Bini, M.; Carraresi, L.; Pasquali, G.; Taccetti, N.

    2003-01-01

    An application of digital sampling techniques is presented which can greatly simplify experiments involving sub-nanosecond time-mark determinations and energy measurements with nuclear detectors, used for Pulse Shape Analysis and Time of Flight measurements in heavy ion experiments. In this work a 100 M Sample/s, 12 bit analog to digital converter has been used: examples of this technique applied to Silicon and CsI(Tl) detectors in heavy-ions experiments involving particle identification via Pulse Shape analysis and Time of Flight measurements are presented. The system is suited for applications to large detector arrays and to different kinds of detectors. Some preliminary results regarding the simulation of current signals in Silicon detectors are also discussed. (authors)

  12. Sample size estimation and sampling techniques for selecting a representative sample

    Directory of Open Access Journals (Sweden)

    Aamir Omair

    2014-01-01

    Full Text Available Introduction: The purpose of this article is to provide a general understanding of the concepts of sampling as applied to health-related research. Sample Size Estimation: It is important to select a representative sample in quantitative research in order to be able to generalize the results to the target population. The sample should be of the required sample size and must be selected using an appropriate probability sampling technique. There are many hidden biases which can adversely affect the outcome of the study. Important factors to consider for estimating the sample size include the size of the study population, confidence level, expected proportion of the outcome variable (for categorical variables/standard deviation of the outcome variable (for numerical variables, and the required precision (margin of accuracy from the study. The more the precision required, the greater is the required sample size. Sampling Techniques: The probability sampling techniques applied for health related research include simple random sampling, systematic random sampling, stratified random sampling, cluster sampling, and multistage sampling. These are more recommended than the nonprobability sampling techniques, because the results of the study can be generalized to the target population.

  13. Macro elemental analysis of food samples by nuclear analytical technique

    Science.gov (United States)

    Syahfitri, W. Y. N.; Kurniawati, S.; Adventini, N.; Damastuti, E.; Lestiani, D. D.

    2017-06-01

    Energy-dispersive X-ray fluorescence (EDXRF) spectrometry is a non-destructive, rapid, multi elemental, accurate, and environment friendly analysis compared with other detection methods. Thus, EDXRF spectrometry is applicable for food inspection. The macro elements calcium and potassium constitute important nutrients required by the human body for optimal physiological functions. Therefore, the determination of Ca and K content in various foods needs to be done. The aim of this work is to demonstrate the applicability of EDXRF for food analysis. The analytical performance of non-destructive EDXRF was compared with other analytical techniques; neutron activation analysis and atomic absorption spectrometry. Comparison of methods performed as cross checking results of the analysis and to overcome the limitations of the three methods. Analysis results showed that Ca found in food using EDXRF and AAS were not significantly different with p-value 0.9687, whereas p-value of K between EDXRF and NAA is 0.6575. The correlation between those results was also examined. The Pearson correlations for Ca and K were 0.9871 and 0.9558, respectively. Method validation using SRM NIST 1548a Typical Diet was also applied. The results showed good agreement between methods; therefore EDXRF method can be used as an alternative method for the determination of Ca and K in food samples.

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  15. Elemental analysis of brazing alloy samples by neutron activation technique

    International Nuclear Information System (INIS)

    Eissa, E.A.; Rofail, N.B.; Hassan, A.M.; El-Shershaby, A.; Walley El-Dine, N.

    1996-01-01

    Two brazing alloy samples (C P 2 and C P 3 ) have been investigated by Neutron activation analysis (NAA) technique in order to identify and estimate their constituent elements. The pneumatic irradiation rabbit system (PIRS), installed at the first egyptian research reactor (ETRR-1) was used for short-time irradiation (30 s) with a thermal neutron flux of 1.6 x 10 1 1 n/cm 2 /s in the reactor reflector, where the thermal to epithermal neutron flux ratio is 106. Long-time irradiation (48 hours) was performed at reactor core periphery with thermal neutron flux of 3.34 x 10 1 2 n/cm 2 /s, and thermal to epithermal neutron flux ratio of 79. Activation by epithermal neutrons was taken into account for the (1/v) and resonance neutron absorption in both methods. A hyper pure germanium detection system was used for gamma-ray acquisitions. The concentration values of Al, Cr, Fe, Co, Cu, Zn, Se, Ag and Sb were estimated as percentages of the sample weight and compared with reported values. 1 tab

  16. Elemental analysis of brazing alloy samples by neutron activation technique

    Energy Technology Data Exchange (ETDEWEB)

    Eissa, E A; Rofail, N B; Hassan, A M [Reactor and Neutron physics Department, Nuclear Research Centre, Atomic Energy Authority, Cairo (Egypt); El-Shershaby, A; Walley El-Dine, N [Physics Department, Faculty of Girls, Ain Shams Universty, Cairo (Egypt)

    1997-12-31

    Two brazing alloy samples (C P{sup 2} and C P{sup 3}) have been investigated by Neutron activation analysis (NAA) technique in order to identify and estimate their constituent elements. The pneumatic irradiation rabbit system (PIRS), installed at the first egyptian research reactor (ETRR-1) was used for short-time irradiation (30 s) with a thermal neutron flux of 1.6 x 10{sup 1}1 n/cm{sup 2}/s in the reactor reflector, where the thermal to epithermal neutron flux ratio is 106. Long-time irradiation (48 hours) was performed at reactor core periphery with thermal neutron flux of 3.34 x 10{sup 1}2 n/cm{sup 2}/s, and thermal to epithermal neutron flux ratio of 79. Activation by epithermal neutrons was taken into account for the (1/v) and resonance neutron absorption in both methods. A hyper pure germanium detection system was used for gamma-ray acquisitions. The concentration values of Al, Cr, Fe, Co, Cu, Zn, Se, Ag and Sb were estimated as percentages of the sample weight and compared with reported values. 1 tab.

  17. Differences in sampling techniques on total post-mortem tryptase.

    Science.gov (United States)

    Tse, R; Garland, J; Kesha, K; Elstub, H; Cala, A D; Ahn, Y; Stables, S; Palmiere, C

    2017-11-20

    The measurement of mast cell tryptase is commonly used to support the diagnosis of anaphylaxis. In the post-mortem setting, the literature recommends sampling from peripheral blood sources (femoral blood) but does not specify the exact sampling technique. Sampling techniques vary between pathologists, and it is unclear whether different sampling techniques have any impact on post-mortem tryptase levels. The aim of this study is to compare the difference in femoral total post-mortem tryptase levels between two sampling techniques. A 6-month retrospective study comparing femoral total post-mortem tryptase levels between (1) aspirating femoral vessels with a needle and syringe prior to evisceration and (2) femoral vein cut down during evisceration. Twenty cases were identified, with three cases excluded from analysis. There was a statistically significant difference (paired t test, p sampling methods. The clinical significance of this finding and what factors may contribute to it are unclear. When requesting post-mortem tryptase, the pathologist should consider documenting the exact blood collection site and method used for collection. In addition, blood samples acquired by different techniques should not be mixed together and should be analyzed separately if possible.

  18. Nuclear analytical techniques and their application to environmental samples

    International Nuclear Information System (INIS)

    Lieser, K.H.

    1986-01-01

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

  19. Two sampling techniques for game meat

    OpenAIRE

    van der Merwe, Maretha; Jooste, Piet J.; Hoffman, Louw C.; Calitz, Frikkie J.

    2013-01-01

    A study was conducted to compare the excision sampling technique used by the export market and the sampling technique preferred by European countries, namely the biotrace cattle and swine test. The measuring unit for the excision sampling was grams (g) and square centimetres (cm2) for the swabbing technique. The two techniques were compared after a pilot test was conducted on spiked approved beef carcasses (n = 12) that statistically proved the two measuring units correlated. The two sampling...

  20. Standardization of proton-induced x-ray emission technique for analysis of thick samples

    Science.gov (United States)

    Ali, Shad; Zeb, Johar; Ahad, Abdul; Ahmad, Ishfaq; Haneef, M.; Akbar, Jehan

    2015-09-01

    This paper describes the standardization of the proton-induced x-ray emission (PIXE) technique for finding the elemental composition of thick samples. For the standardization, three different samples of standard reference materials (SRMs) were analyzed using this technique and the data were compared with the already known data of these certified SRMs. These samples were selected in order to cover the maximum range of elements in the periodic table. Each sample was irradiated for three different values of collected beam charges at three different times. A proton beam of 2.57 MeV obtained using 5UDH-II Pelletron accelerator was used for excitation of x-rays from the sample. The acquired experimental data were analyzed using the GUPIXWIN software. The results show that the SRM data and the data obtained using the PIXE technique are in good agreement.

  1. Two sampling techniques for game meat

    Directory of Open Access Journals (Sweden)

    Maretha van der Merwe

    2013-03-01

    Full Text Available A study was conducted to compare the excision sampling technique used by the export market and the sampling technique preferred by European countries, namely the biotrace cattle and swine test. The measuring unit for the excision sampling was grams (g and square centimetres (cm2 for the swabbing technique. The two techniques were compared after a pilot test was conducted on spiked approved beef carcasses (n = 12 that statistically proved the two measuring units correlated. The two sampling techniques were conducted on the same game carcasses (n = 13 and analyses performed for aerobic plate count (APC, Escherichia coli and Staphylococcus aureus, for both techniques. A more representative result was obtained by swabbing and no damage was caused to the carcass. Conversely, the excision technique yielded fewer organisms and caused minor damage to the carcass. The recovery ratio from the sampling technique improved 5.4 times for APC, 108.0 times for E. coli and 3.4 times for S. aureus over the results obtained from the excision technique. It was concluded that the sampling methods of excision and swabbing can be used to obtain bacterial profiles from both export and local carcasses and could be used to indicate whether game carcasses intended for the local market are possibly on par with game carcasses intended for the export market and therefore safe for human consumption.

  2. Two sampling techniques for game meat.

    Science.gov (United States)

    van der Merwe, Maretha; Jooste, Piet J; Hoffman, Louw C; Calitz, Frikkie J

    2013-03-20

    A study was conducted to compare the excision sampling technique used by the export market and the sampling technique preferred by European countries, namely the biotrace cattle and swine test. The measuring unit for the excision sampling was grams (g) and square centimetres (cm2) for the swabbing technique. The two techniques were compared after a pilot test was conducted on spiked approved beef carcasses (n = 12) that statistically proved the two measuring units correlated. The two sampling techniques were conducted on the same game carcasses (n = 13) and analyses performed for aerobic plate count (APC), Escherichia coli and Staphylococcus aureus, for both techniques. A more representative result was obtained by swabbing and no damage was caused to the carcass. Conversely, the excision technique yielded fewer organisms and caused minor damage to the carcass. The recovery ratio from the sampling technique improved 5.4 times for APC, 108.0 times for E. coli and 3.4 times for S. aureus over the results obtained from the excision technique. It was concluded that the sampling methods of excision and swabbing can be used to obtain bacterial profiles from both export and local carcasses and could be used to indicate whether game carcasses intended for the local market are possibly on par with game carcasses intended for the export market and therefore safe for human consumption.

  3. Laser-Assisted Sampling Techniques in Combination with ICP-MS: A Novel Approach for Particle Analysis at the IAEA Environmental Samples Laboratory

    International Nuclear Information System (INIS)

    Dzigal, N.; Chinea-Cano, E.

    2015-01-01

    Researchers have found many applications for lasers. About two decades ago, scientists started using lasers as sample introduction instruments for mass spectrometry measurements. Similarly, lasers as micro-dissection tools have also been increasingly on demand in the fields of life sciences, materials science, forensics, etc. This presentation deals with the interception of these aforementioned laser-assisted techniques to the field of particle analysis. Historically, the use of a nanosecond laser to ablate material has been used in materials science. Recently, it has been proven that in the analysis of particulate materials the disadvantages associated with the utilization of nanosecond lasers such as overheating and melting of the sample are suppressed when using femtosecond lasers. Further, due to the length of a single laser shot, fs-LA allows a more controlled ablation to occur and therefore the sample plasma is more homogeneous and less mass-fractionation events are detected. The use of laser micro-dissection devices enables the physical segmentation of microsized artefacts previously performed by a laborious manual procedure. By combining the precision of the laser cutting inherent to the LMD technique together with a particle identification methodology, one can increase the efficiency of single particle isolation. Further, besides the increase in throughput of analyses, this combination enhances the signal-to-noise ratio by removing matrix particles effectively. Specifically, this contribution describes the use of an Olympus+MMI laser microdissection device in improving the sample preparation of environmental swipe samples and the installation of an Applied Spectra J200 fs-LA/LIBS (laser ablation/laser inducedbreakdown spectroscopy) system as a sample introduction device to a quadrupole mass spectrometer, the iCap Q from Thermofisher Scientific at the IAEA Environmental Samples Laboratory are explored. Preliminary results of the ongoing efforts for the

  4. Direct Trace Element Analysis of Liquid Blood Samples by In-Air Ion Beam Analytical Techniques (PIXE-PIGE).

    Science.gov (United States)

    Huszank, Robert; Csedreki, László; Török, Zsófia

    2017-02-07

    There are various liquid materials whose elemental composition is of interest in various fields of science and technology. In many cases, sample preparation or the extraction can be complicated, or it would destroy the original environment before the analysis (for example, in the case of biological samples). However, multielement direct analysis of liquid samples can be realized by an external PIXE-PIGE measurement system. Particle-induced X-ray and gamma-ray emission spectroscopy (PIXE, PIGE) techniques were applied in external (in-air) microbeam configuration for the trace and main element determination of liquid samples. The direct analysis of standard solutions of several metal salts and human blood samples (whole blood, blood serum, blood plasma, and formed elements) was realized. From the blood samples, Na, P, S, Cl, K, Ca, Fe, Cu, Zn, and Br elemental concentrations were determined. The focused and scanned ion beam creates an opportunity to analyze very small volume samples (∼10 μL). As the sample matrix consists of light elements, the analysis is possible at ppm level. Using this external beam setup, it was found that it is possible to determine elemental composition of small-volume liquid samples routinely, while the liquid samples do not require any preparation processes, and thus, they can be analyzed directly. In the case of lower concentrations, the method is also suitable for the analysis (down to even ∼1 ppm level) but with less accuracy and longer measurement times.

  5. Nuclear techniques for analysis of environmental samples

    International Nuclear Information System (INIS)

    1986-12-01

    The main purposes of this meeting were to establish the state-of-the-art in the field, to identify new research and development that is required to provide an adequate framework for analysis of environmental samples and to assess needs and possibilities for international cooperation in problem areas. This technical report was prepared on the subject based on the contributions made by the participants. A separate abstract was prepared for each of the 9 papers

  6. Analysis of techniques of sample attack for soil and mineral analysis

    International Nuclear Information System (INIS)

    Dean, J.R.; Chiu, N.W.

    1985-05-01

    Four methods of sample attack were evaluated in the laboratory for use in the determination of uranium, radium-226, thorium-232, thorium-230, thorium-228, and lead-210. The methods evaluated were (1) KF/pyrosulfate fusion; (2) Sodium carbonate fusion; (3) Nitric, perchloric, hydrofluoric acid digestion; and, (4) combination nitric, perchloric, hydrofluoric acid/pyrosulfate fusion. Five samples were chosen for evaluation; two were mine tailings from Bancroft, Ontario and Beaverlodge, Saskatchewan, one was a synthetic uranium ore-silica mixture and two were soil samples supplied by AECB. The KF/pyrosulfate dissolution procedure was found to be the fastest and, overall, most accurate dissolution method for the analysis of 1-20 samples. For larger numbers of samples the three acid/pyrosulfate fusion combination was shown to have some merit

  7. Soil sample preparation using microwave digestion for uranium analysis

    International Nuclear Information System (INIS)

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

    2000-01-01

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

  8. Environmental sampling for trace analysis

    International Nuclear Information System (INIS)

    Markert, B.

    1994-01-01

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

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

    International Nuclear Information System (INIS)

    1997-06-01

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

  10. Coacervative extraction as a green technique for sample preparation for the analysis of organic compounds.

    Science.gov (United States)

    Melnyk, A; Wolska, L; Namieśnik, J

    2014-04-25

    One of the present trends in analytical chemistry is miniaturization, which is one of the methods of green analytical chemistry application. A particular emphasis is placed on the elimination of the use of large amounts of organic solvents which are toxic and harmful to the environment, maintaining high efficiency of the extraction process, high recovery values and low values of quantification (LOQ) and detection (LOD) limits. These requirements are fulfilled by coacervative extraction (CAE) technique. In this review, theoretical aspects of the coacervation process are presented along with environmental and bioanalytical applications of this technique, its advantages, limitations and competitiveness with other techniques. Due to its simplicity and rapidity, CAE is an excellent alternative for currently practiced procedures of sample preparation for the analysis of organic compounds. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Sample preparation techniques of biological material for isotope analysis

    International Nuclear Information System (INIS)

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

    1990-01-01

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

  12. Analysis of atmospheric particulate samples via instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Greenberg, R.R.

    1990-01-01

    Instrumental neutron activation analysis (INAA) is a powerful analytical technique for the elemental characterization of atmospheric particulate samples. It is a true multielement technique with adequate sensitivity to determine 30 to 40 elements in a sample of atmospheric particulate material. Its nondestructive nature allows sample reanalysis by the same or a different analytical technique. In this paper as an example of the applicability of INAA to the study of atmospheric particulate material, a study of the emissions from municipal incinerators is described

  13. Application of neutron activation analysis technique in elemental determination of lichen samples

    International Nuclear Information System (INIS)

    Djoko Prakoso Dwi Atmodjo; Syukria Kurniawati; Woro Yatu Niken Syahfitri; Nana Suherman; Dadang Supriatna

    2010-01-01

    Lichen is one of the biological materials as pollution monitor that can give information about level, direction, and history of various pollutants in environment. Small sample weights and elemental content of lichens is on the order of ppm, so that its characterization requires advanced analytical techniques that has high sensitivity and capable of analyzing samples with weight of - 25 mg, such as neutron activation analysis. In this research, determination of elements was done in lichen samples obtained from Kiaracondong and Holis areas in Bandung city, to understanding the difference of industrial exposure level on surrounding environment. Samples were irradiated in RSG GA Siwabessy, Serpong, at 15 MW for 1-2 and 60 minutes for short irradiation and long irradiation, respectively. The samples were then counted using HPGe detector with GENIE 2000 software. The level of element in lichen for Kiaracondong area were Co, Cr, Cs, Fe, Mg, Mn, Sb, Sc, and V in the range of 0.55-0.86, 1.47-2.57, 0.87-1.19, 540-1005, 949-1674, 34.91-45.94, 0.08-0.14, 0.16-0.31, and ≤ 2.33 mg/kg, respectively, while for Holis area were 1.04-2.37, 4.41-10.36, 0.41-0.89, 3166-709, 1131-1422, 40.97-72.51, 0.33-0.50, 0.98-2.18, and 5.30-13.05 mg/kg respectively. From these results, it is known that pollution exposure from the semi industrial area Holis provide greater influence than in the semi industrial area Kiaracondong. (author)

  14. Soil analysis. Modern instrumental technique

    International Nuclear Information System (INIS)

    Smith, K.A.

    1993-01-01

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

  15. Analysis of pure and malachite green doped polysulfone sample using FT-IR technique

    Science.gov (United States)

    Nayak, Rashmi J.; Khare, P. K.; Nayak, J. G.

    2018-05-01

    The sample of pure and malachite green doped Polysulfone in the form of foil was prepared by isothermal immersion technique. For the preparation of pure sample 4 gm of Polysulfone was dissolved in 50 ml of Dimethyl farmamide (DMF) solvent, while for the preparation of doped sample 10 mg, 50 mg and 100 mg Malachite Green was mixed with 4 gm of Polysulfone respectively. For the study of structural characterization of these pure and doped sample, Fourier Transform Infra-Red Spectroscopy (FT-IR) technique was used. This study shows that the intensity of transmittance decreases as the ratio of doping increases in pure polysulfone. The reduction in intensity of transmittance is clearly apparent in the present case more over the bands were broader which indicates towards charge transfer interaction between the donar and acceptor molecule.

  16. Application of nuclear and allied techniques for the characterisation of forensic samples

    International Nuclear Information System (INIS)

    Sudersanan, M.; Kayasth, S.R.; Pant, D.R.; Chattopadhyay, N.; Bhattacharyya, C.N.

    2002-01-01

    Full text: Forensic science deals with the application of various techniques for physics, chemistry and biology for crime investigation. The legal implication of such analysis put considerable restriction on the choice of analytical techniques. Moreover, the unknown nature of the materials, the limited availability of samples and the large number of elements to be analysed put considerable strain on the analytical chemist on the selection of the appropriate technique. The availability of nuclear techniques has considerably enhanced the scope of forensic analysis. This paper deals with the recent results on the use of nuclear and allied analytical techniques for forensic applications. One of the important types of samples of forensic importance pertain to the identification of gunshot residues. The use of nuclear techniques has considerably simplified the interpretation of results through the use of appropriate elements like Ba, Cu, Sb, Zn, As and Sn etc. The combination of non-nuclear techniques for elements like Pb and Ni which are not easily amenable to be analysed by NAA and the use of appropriate separation procedure has led to the use of this method as a valid and versatile analytical procedure. In view of the presence of a large amounts of extraneous materials like cloth, body tissues etc in these samples and the limited availability of materials, the procedures for sample collection, dissolution and analysis have been standardized. Analysis of unknown materials like powders, metallic pieces etc. for the possible presence of nuclear materials or as materials in illicit trafficking is becoming important in recent years. The use of multi-technique approach is important in this case. Use of non-destructive techniques like XRF and radioactive counting enables the preliminary identification of materials and for the detection of radioactivity. Subsequent analysis by NAA or other appropriate analytical methods allows the characterization of the materials. Such

  17. Design and building of a homemade sample changer for automation of the irradiation in neutron activation analysis technique

    International Nuclear Information System (INIS)

    Gago, Javier; Hernandez, Yuri; Baltuano, Oscar; Bedregal, Patricia; Lopez, Yon; Urquizo, Rafael

    2014-01-01

    Because the RP-10 research reactor operates during weekends, it was necessary to design and build a sample changer for irradiation as part of the automation process of neutron activation analysis technique. The device is formed by an aluminum turntable disk which can accommodate 19 polyethylene capsules, containing samples to be sent using the pneumatic transfer system from the laboratory to the irradiation position. The system is operate by a control switchboard to send and return capsules in a variable preset time and by two different ways, allowing the determination of short, medium and long lived radionuclides. Also another mechanism is designed called 'exchange valve' for changing travel paths (pipelines) allowing the irradiated samples to be stored for a longer time in the reactor hall. The system design has allowed complete automation of this technique, enabling the irradiation of samples without the presence of an analyst. The design, construction and operation of the device is described and presented in this article. (authors).

  18. Flow analysis techniques for phosphorus: an overview.

    Science.gov (United States)

    Estela, José Manuel; Cerdà, Víctor

    2005-04-15

    A bibliographical review on the implementation and the results obtained in the use of different flow analytical techniques for the determination of phosphorus is carried out. The sources, occurrence and importance of phosphorus together with several aspects regarding the analysis and terminology used in the determination of this element are briefly described. A classification as well as a brief description of the basis, advantages and disadvantages of the different existing flow techniques, namely; segmented flow analysis (SFA), flow injection analysis (FIA), sequential injection analysis (SIA), all injection analysis (AIA), batch injection analysis (BIA), multicommutated FIA (MCFIA), multisyringe FIA (MSFIA) and multipumped FIA (MPFIA) is also carried out. The most relevant manuscripts regarding the analysis of phosphorus by means of flow techniques are herein classified according to the detection instrumental technique used with the aim to facilitate their study and obtain an overall scope. Finally, the analytical characteristics of numerous flow-methods reported in the literature are provided in the form of a table and their applicability to samples with different matrixes, namely water samples (marine, river, estuarine, waste, industrial, drinking, etc.), soils leachates, plant leaves, toothpaste, detergents, foodstuffs (wine, orange juice, milk), biological samples, sugars, fertilizer, hydroponic solutions, soils extracts and cyanobacterial biofilms are tabulated.

  19. Sampling techniques for thrips (Thysanoptera: Thripidae) in preflowering tomato.

    Science.gov (United States)

    Joost, P Houston; Riley, David G

    2004-08-01

    Sampling techniques for thrips (Thysanoptera: Thripidae) were compared in preflowering tomato plants at the Coastal Plain Experiment Station in Tifton, GA, in 2000 and 2003, to determine the most effective method of determining abundance of thrips on tomato foliage early in the growing season. Three relative sampling techniques, including a standard insect aspirator, a 946-ml beat cup, and an insect vacuum device, were compared for accuracy to an absolute method and to themselves for precision and efficiency of sampling thrips. Thrips counts of all relative sampling methods were highly correlated (R > 0.92) to the absolute method. The aspirator method was the most accurate compared with the absolute sample according to regression analysis in 2000. In 2003, all sampling methods were considered accurate according to Dunnett's test, but thrips numbers were lower and sample variation was greater than in 2000. In 2000, the beat cup method had the lowest relative variation (RV) or best precision, at 1 and 8 d after transplant (DAT). Only the beat cup method had RV values <25 for all sampling dates. In 2003, the beat cup method had the lowest RV value at 15 and 21 DAT. The beat cup method also was the most efficient method for all sample dates in both years. Frankliniella fusca (Pergande) was the most abundant thrips species on the foliage of preflowering tomato in both years of study at this location. Overall, the best thrips sampling technique tested was the beat cup method in terms of precision and sampling efficiency.

  20. Modified emission-transmission method for determining trace elements in solid samples using the XRF techniques

    International Nuclear Information System (INIS)

    Poblete, V.; Alvarez, M.; Hermosilla, M.

    2000-01-01

    This is a study of an analysis of trace elements in medium thick solid samples, by the modified transmission emission method, using the energy dispersion X-ray fluorescence technique (EDXRF). The effects of absorption and reinforcement are the main disadvantages of the EDXRF technique for the quantitative analysis of bigger elements and trace elements in solid samples. The implementation of this method and its application to a variety of samples was carried out using an infinitely thick multi-element white sample that calculates the correction factors by absorbing all the analytes in the sample. The discontinuities in the masic absorption coefficients versus energies association for each element, with medium thick and homogenous samples, are analyzed and corrected. A thorough analysis of the different theoretical and test variables are proven by using real samples, including certified material with known concentration. The simplicity of the calculation method and the results obtained show the method's major precision, with possibilities for the non-destructive routine analysis of different solid samples, using the EDXRF technique (author)

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  2. Comparison of laser fluorimetry, high resolution gamma-ray spectrometry and neutron activation analysis techniques for determination of uranium content in soil samples

    International Nuclear Information System (INIS)

    Ghods, A.; Asgharizadeh, F.; Salimi, B.; Abbasi, A.

    2004-01-01

    Much more concern is given nowadays for exposure of the world population to natural radiation especially to uranium since 57% of that exposure is due to radon-222, which is a member of uranium decay series. Most of the methods used for uranium determination is low concentration require either tedious separation and preconcentration or the accessibility to special instrumentation for detection of uranium at this low level. this study compares three techniques and methods for uranium analysis among different soil sample with variable uranium contents. Two of these techniques, neutron activation analysis and high resolution gamma-ray spectrometry , are non-destructive while the other, laser fluorimetry is done via chemical extraction of uranium. Analysis of standard materials is done also to control the quality and accuracy of the work. In spite of having quite variable ranges of detection limit, results obtained by high resolution gamma-ray spectrometry based on the assumption of having secular equilibrium between uranium and its daughters, which causes deviation whenever this condition was missed. For samples with reasonable uranium content, neutron activation analysis would be a rapid and reliable technique, while for low uranium content laser fluorimetry would be the most appropriate and accurate technique

  3. A new analysis technique for microsamples

    International Nuclear Information System (INIS)

    Boyer, R.; Journoux, J.P.; Duval, C.

    1989-01-01

    For many decades, isotopic analysis of Uranium or Plutonium has been performed by mass spectrometry. The most recent analytical techniques, using the counting method or a plasma torch combined with a mass spectrometer (ICP.MS) have not yet to reach a greater degree of precision than the older methods in this field. The two means of ionization for isotopic analysis - by electronic bombardment of atoms or molecules (source of gas ions) and - by thermal effect (thermoionic source) are compared revealing some inconsistency between the quantity of sample necessary for analysis and the luminosity. In fact, the quantity of sample necessary for the gas source mass spectrometer is 10 to 20 times greater than that for the thermoionization spectrometer, while the sample consumption is between 10 5 to 10 6 times greater. This proves that almost the entire sample is not necessary for the measurement; it is only required because of the system of introduction for the gas spectrometer. The new analysis technique referred to as ''Microfluorination'' corrects this anomaly and exploits the advantages of the electron bombardment method of ionization

  4. A comparative study of 232Th and 238U activity estimation in soil samples by gamma spectrometry and neutron activation analysis technique

    International Nuclear Information System (INIS)

    Anilkumar, Rekha; Anilkumar, S.; Narayani, K.; Babu, D.A.R.; Sharma, D.N.

    2012-01-01

    Neutron activation analysis (NAA) is a well-established analytical technique. It has many advantages as compared to the other commonly used techniques. NAA can be performed in a variety of ways depending on the element, its activity level in the sample, interference from the sample matrix and other elements, etc. This technique is used to get high analytical sensitivity and low detection limits (ppm to ppb). The high sensitivity is due to the irradiation at high neutron flux available from the research reactors and the activity measurement is done using high resolution HPGe detectors. In this paper, the activity estimation of soil samples using neutron activation and direct gamma spectrometry methods are compared. Even though the weights of samples considered and samples preparation methods are different for these two methods, the estimated activity values are comparable. (author)

  5. Application of the Sampling Selection Technique in Approaching Financial Audit

    Directory of Open Access Journals (Sweden)

    Victor Munteanu

    2018-03-01

    Full Text Available In his professional approach, the financial auditor has a wide range of working techniques, including selection techniques. They are applied depending on the nature of the information available to the financial auditor, the manner in which they are presented - paper or electronic format, and, last but not least, the time available. Several techniques are applied, successively or in parallel, to increase the safety of the expressed opinion and to provide the audit report with a solid basis of information. Sampling is used in the phase of control or clarification of the identified error. The main purpose is to corroborate or measure the degree of risk detected following a pertinent analysis. Since the auditor does not have time or means to thoroughly rebuild the information, the sampling technique can provide an effective response to the need for valorization.

  6. 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)

  7. SWOT ANALYSIS ON SAMPLING METHOD

    Directory of Open Access Journals (Sweden)

    CHIS ANCA OANA

    2014-07-01

    Full Text Available Audit sampling involves the application of audit procedures to less than 100% of items within an account balance or class of transactions. Our article aims to study audit sampling in audit of financial statements. As an audit technique largely used, in both its statistical and nonstatistical form, the method is very important for auditors. It should be applied correctly for a fair view of financial statements, to satisfy the needs of all financial users. In order to be applied correctly the method must be understood by all its users and mainly by auditors. Otherwise the risk of not applying it correctly would cause loose of reputation and discredit, litigations and even prison. Since there is not a unitary practice and methodology for applying the technique, the risk of incorrectly applying it is pretty high. The SWOT analysis is a technique used that shows the advantages, disadvantages, threats and opportunities. We applied SWOT analysis in studying the sampling method, from the perspective of three players: the audit company, the audited entity and users of financial statements. The study shows that by applying the sampling method the audit company and the audited entity both save time, effort and money. The disadvantages of the method are difficulty in applying and understanding its insight. Being largely used as an audit method and being a factor of a correct audit opinion, the sampling method’s advantages, disadvantages, threats and opportunities must be understood by auditors.

  8. Technique of sample preparation for analysis of gasoline and lubricating oils by X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Avila P, P.

    1990-03-01

    The X-ray fluorescence laboratory of the National Institute of Nuclear Research when not having a technique for the analysis of oils it has intended, with this work, to develop a preparation technique for the analysis of the metals of Pb, Cr, Ni, V and Mo in gasolines and oils, by means of the spectrometry by X-ray fluorescence analysis. The obtained results, its will be of great utility for the one mentioned laboratory. (Author)

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

    International Nuclear Information System (INIS)

    Anon.

    1979-01-01

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

  10. Electrodeposition as a sample preparation technique for TXRF analysis

    International Nuclear Information System (INIS)

    Griesel, S.; Reus, U.; Prange, A.

    2000-01-01

    TXRF analysis of trace elements at concentrations in the μg/L range and below in high salt matrices normally requires a number of sample preparation steps that include separation of the salt matrix and preconcentration of the trace elements. A neat approach which allows samples to be prepared straightforwardly in a single step involves the application of electrochemical deposition using the TXRF sample support itself as an electrode. For this work a common three-electrode arrangement (radiometer analytical) with a rotating disc electrode as the working electrode, as is frequently employed in voltametric analysis, has been used. A special electrode tip has been constructed as a holder for the sample carrier which consists of polished glassy carbon. This material has been proven to be suitable for both its electrical and chemical properties. Measurements of the trace elements were performed using the ATOMIKA 8030C TXRF spectrometer, with the option of variable incident angles. In first experiments an artificial sea water matrix containing various trace elements in the μg/L range has been used. Elements such as Cr, Mn, Fe, Co, Ni, Cu, Zn, Ag, Cd, Hg, and Pb deposited on glassy carbon carriers. The deposition can be optimized by controlling the potential of the working electrode with respect to the reference electrode. Metal ions with a suitable standard potential are reduced to the metallic state and plated onto the electrode surface. When deposition is finished the sample carrier is demounted, rinsed with ultra-pure water and measured directly. Deposition yields for the elements under investigation are quite similar, and with an appropriate choice of the reference element, quantification can be achieved directly by internal standardization. The influence of parameters such as time, pH value, and trace element concentration on the deposition yield has been examined, and the results will be presented along with reproducibility studies. (author)

  11. Uranium-233 analysis of biological samples

    International Nuclear Information System (INIS)

    Gies, R.A.; Ballou, J.E.; Case, A.C.

    1979-01-01

    Two liquid scintillation techniques were compared for 233 U analysis: a two-phase extraction system (D2EHPA) developed by Keough and Powers, 1970, for Pu analysis; and a single-phase emulsion system (TT21) that holds the total sample in suspension with the scintillator. The first system (D2EHPA) was superior in reducing background (two- to threefold) and in accommodating a larger sample volume (fivefold). Samples containing > 50 mg/ml of slats were not extracted quantitatively by D2EHPA

  12. Large sample neutron activation analysis of a reference inhomogeneous sample

    International Nuclear Information System (INIS)

    Vasilopoulou, T.; Athens National Technical University, Athens; Tzika, F.; Stamatelatos, I.E.; Koster-Ammerlaan, M.J.J.

    2011-01-01

    A benchmark experiment was performed for Neutron Activation Analysis (NAA) of a large inhomogeneous sample. The reference sample was developed in-house and consisted of SiO 2 matrix and an Al-Zn alloy 'inhomogeneity' body. Monte Carlo simulations were employed to derive appropriate correction factors for neutron self-shielding during irradiation as well as self-attenuation of gamma rays and sample geometry during counting. The large sample neutron activation analysis (LSNAA) results were compared against reference values and the trueness of the technique was evaluated. An agreement within ±10% was observed between LSNAA and reference elemental mass values, for all matrix and inhomogeneity elements except Samarium, provided that the inhomogeneity body was fully simulated. However, in cases that the inhomogeneity was treated as not known, the results showed a reasonable agreement for most matrix elements, while large discrepancies were observed for the inhomogeneity elements. This study provided a quantification of the uncertainties associated with inhomogeneity in large sample analysis and contributed to the identification of the needs for future development of LSNAA facilities for analysis of inhomogeneous samples. (author)

  13. Newly introduced sample preparation techniques: towards miniaturization.

    Science.gov (United States)

    Costa, Rosaria

    2014-01-01

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

  14. Sampling and sample processing in pesticide residue analysis.

    Science.gov (United States)

    Lehotay, Steven J; Cook, Jo Marie

    2015-05-13

    Proper sampling and sample processing in pesticide residue analysis of food and soil have always been essential to obtain accurate results, but the subject is becoming a greater concern as approximately 100 mg test portions are being analyzed with automated high-throughput analytical methods by agrochemical industry and contract laboratories. As global food trade and the importance of monitoring increase, the food industry and regulatory laboratories are also considering miniaturized high-throughput methods. In conjunction with a summary of the symposium "Residues in Food and Feed - Going from Macro to Micro: The Future of Sample Processing in Residue Analytical Methods" held at the 13th IUPAC International Congress of Pesticide Chemistry, this is an opportune time to review sampling theory and sample processing for pesticide residue analysis. If collected samples and test portions do not adequately represent the actual lot from which they came and provide meaningful results, then all costs, time, and efforts involved in implementing programs using sophisticated analytical instruments and techniques are wasted and can actually yield misleading results. This paper is designed to briefly review the often-neglected but crucial topic of sample collection and processing and put the issue into perspective for the future of pesticide residue analysis. It also emphasizes that analysts should demonstrate the validity of their sample processing approaches for the analytes/matrices of interest and encourages further studies on sampling and sample mass reduction to produce a test portion.

  15. Quality assurance techniques for activation analysis

    International Nuclear Information System (INIS)

    Becker, D.A.

    1984-01-01

    The principles and techniques of quality assurance are applied to the measurement method of activation analysis. Quality assurance is defined to include quality control and quality assessment. Plans for quality assurance include consideration of: personnel; facilities; analytical design; sampling and sample preparation; the measurement process; standards; and documentation. Activation analysis concerns include: irradiation; chemical separation; counting/detection; data collection, and analysis; and calibration. Types of standards discussed include calibration materials and quality assessment materials

  16. Statistical evaluation of vibration analysis techniques

    Science.gov (United States)

    Milner, G. Martin; Miller, Patrice S.

    1987-01-01

    An evaluation methodology is presented for a selection of candidate vibration analysis techniques applicable to machinery representative of the environmental control and life support system of advanced spacecraft; illustrative results are given. Attention is given to the statistical analysis of small sample experiments, the quantification of detection performance for diverse techniques through the computation of probability of detection versus probability of false alarm, and the quantification of diagnostic performance.

  17. Water sampling techniques for continuous monitoring of pesticides in water

    Directory of Open Access Journals (Sweden)

    Šunjka Dragana

    2017-01-01

    Full Text Available Good ecological and chemical status of water represents the most important aim of the Water Framework Directive 2000/60/EC, which implies respect of water quality standards at the level of entire river basin (2008/105/EC and 2013/39/EC. This especially refers to the control of pesticide residues in surface waters. In order to achieve the set goals, a continuous monitoring program that should provide a comprehensive and interrelated overview of water status should be implemented. However, it demands the use of appropriate analysis techniques. Until now, the procedure for sampling and quantification of residual pesticide quantities in aquatic environment was based on the use of traditional sampling techniques that imply periodical collecting of individual samples. However, this type of sampling provides only a snapshot of the situation in regard to the presence of pollutants in water. As an alternative, the technique of passive sampling of pollutants in water, including pesticides has been introduced. Different samplers are available for pesticide sampling in surface water, depending on compounds. The technique itself is based on keeping a device in water over a longer period of time which varies from several days to several weeks, depending on the kind of compound. In this manner, the average concentrations of pollutants dissolved in water during a time period (time-weighted average concentrations, TWA are obtained, which enables monitoring of trends in areal and seasonal variations. The use of these techniques also leads to an increase in sensitivity of analytical methods, considering that pre-concentration of analytes takes place within the sorption medium. However, the use of these techniques for determination of pesticide concentrations in real water environments requires calibration studies for the estimation of sampling rates (Rs. Rs is a volume of water per time, calculated as the product of overall mass transfer coefficient and area of

  18. Study of uranium mineralization in rock samples from marwat range bannu basin by fission track analysis technique

    International Nuclear Information System (INIS)

    Qureshi, A.Z.; Ullah, K.; Ullah, N.; Akram, M.

    2004-07-01

    The Geophysics Division, Atomic Energy Minerals Centre (AEMC), Lahore has planned a uranium exploration program in Marwat Range, Bannu Basin. In this connection 30 thin sections of rock samples, collected from four areas; namely, Darra Tang, Simukili, Karkanwal and Sheikhillah from Marwat Range, and one from Salt Range were provided to Nuclear Geology Group of Physics Research Division, PINSTECH for the study of nature and mechanism of uranium mineralization These studies are aimed to help in designing uranium exploration strategy by providing the loci of uranium sources in the Marwat and Salt Ranges. The samples have been studied using fission track analysis technique. (author)

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

    Science.gov (United States)

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

    2004-01-01

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

  20. Elemental analysis of water and soil environmental samples in Tabuk area by neutron capture gamma-ray spectroscopy techniques

    International Nuclear Information System (INIS)

    Al-Aseery, Sh.M.; Alamoudi, Z.; Hassan, A.M.

    2006-01-01

    The prompt and delayed gamma-rays due to neutron capture in the nuclei of the constituent elements of three soil samples and one drinking water sample have been measured. The 252 Cf and 226 Ra/Be isotopic neutron sources are used for neutron irradiation. Also, the hyper pure germanium detection system is used. The soil samples were from Astra, Tadco and El-Gammaz farms, while the water sample was taken from Tabuk city. In case of prompt gamma-ray analysis, a total of 16 elements were identified and the concentration percentage values by weight were calculated for: C, Na, Mg, Al, Si, S, Cl,, Ca, Ti, Cr, Mn, Fe, Co, Zn, Sr ad Pb elements. A comparative study between the results obtained in this work and the results obtained by ICP-MS and EDX-Ray techniques for the same samples is given

  1. In-air micro-pixe analysis of tissue samples

    International Nuclear Information System (INIS)

    Tanaka, A.; Ishii, K.; Komori, Y.

    2002-01-01

    Micro-PIXE is capable of providing spatial distributions of elements in the micro-meter scale and its application to biology is useful to elucidate the cellular metabolism. Since, in this method, a sample target is usually irradiated with proton or α-particle beams in vacuum, beam heating results in evaporation of volatile elements an shrinking of the sample. In order to avoid these side effects, we previously developed a technique of in-air micro-PIXE analysis for samples of cultured cells. In addition to these, analysis of exposed tissue samples from living subjects is highly desirable in biological and medical research. Here, we describe a technique of in-air micro-PIXE analysis of such tissue samples. The target samples of exposed tissue slices from a Donryu rat, in which a tumor had been transplanted, were analyzed with proton micro-beams of 2.6 MeV. We report that the shape of cells and the distribution of volatile elements in the tissue sample remain uncharged when using a target preparation based on a freeze-drying method. (author)

  2. Neutron activation analysis of certified samples by the absolute method

    Science.gov (United States)

    Kadem, F.; Belouadah, N.; Idiri, Z.

    2015-07-01

    The nuclear reactions analysis technique is mainly based on the relative method or the use of activation cross sections. In order to validate nuclear data for the calculated cross section evaluated from systematic studies, we used the neutron activation analysis technique (NAA) to determine the various constituent concentrations of certified samples for animal blood, milk and hay. In this analysis, the absolute method is used. The neutron activation technique involves irradiating the sample and subsequently performing a measurement of the activity of the sample. The fundamental equation of the activation connects several physical parameters including the cross section that is essential for the quantitative determination of the different elements composing the sample without resorting to the use of standard sample. Called the absolute method, it allows a measurement as accurate as the relative method. The results obtained by the absolute method showed that the values are as precise as the relative method requiring the use of standard sample for each element to be quantified.

  3. NAIL SAMPLING TECHNIQUE AND ITS INTERPRETATION

    Directory of Open Access Journals (Sweden)

    TZAR MN

    2011-01-01

    Full Text Available The clinical suspicion of onychomyosis based on appearance of the nails, requires culture for confirmation. This is because treatment requires prolonged use of systemic agents which may cause side effects. One of the common problems encountered is improper nail sampling technique which results in loss of essential information. The unfamiliar terminologies used in reporting culture results may intimidate physicians resulting in misinterpretation and hamper treatment decision. This article provides a simple guide on nail sampling technique and the interpretation of culture results.

  4. Gamma self-shielding correction factors calculation for aqueous bulk sample analysis by PGNAA technique

    International Nuclear Information System (INIS)

    Nasrabadi, M.N.; Mohammadi, A.; Jalali, M.

    2009-01-01

    In this paper bulk sample prompt gamma neutron activation analysis (BSPGNAA) was applied to aqueous sample analysis using a relative method. For elemental analysis of an unknown bulk sample, gamma self-shielding coefficient was required. Gamma self-shielding coefficient of unknown samples was estimated by an experimental method and also by MCNP code calculation. The proposed methodology can be used for the determination of the elemental concentration of unknown aqueous samples by BSPGNAA where knowledge of the gamma self-shielding within the sample volume is required.

  5. 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)

  6. Development of sampling techniques for ITER Type B radwaste

    International Nuclear Information System (INIS)

    Hong, Kwon Pyo; Kim, Sung Geun; Jung, Sang Hee; Oh, Wan Ho; Park, Myung Chul; Kim, Hee Moon; Ahn, Sang Bok

    2016-01-01

    There are several difficulties and limitation in sampling activities. As the Type B radwaste components are mostly metallic(mostly stainless steel) and bulk(∼ 1 m in size and ∼ 100 mm in thickness), it is difficult in taking samples from the surface of Type B radwaste by remote operation. But also, sampling should be performed without use of any liquid coolant to avoid the spread of contamination. And all sampling procedures are carried in the hot cell red zone with remote operation. Three kinds of sampling techniques are being developed. They are core sampling, chip sampling, and wedge sampling, which are the candidates of sampling techniques to be applied to ITER hot cell. Object materials for sampling are stainless steel or Cu alloy block in order to simulate ITER Type B radwaste. The best sampling technique for ITER Type B radwaste among the three sampling techniques will be suggested in several months after finishing the related experiment

  7. Development of sampling techniques for ITER Type B radwaste

    Energy Technology Data Exchange (ETDEWEB)

    Hong, Kwon Pyo; Kim, Sung Geun; Jung, Sang Hee; Oh, Wan Ho; Park, Myung Chul; Kim, Hee Moon; Ahn, Sang Bok [KAERI, Daejeon (Korea, Republic of)

    2016-05-15

    There are several difficulties and limitation in sampling activities. As the Type B radwaste components are mostly metallic(mostly stainless steel) and bulk(∼ 1 m in size and ∼ 100 mm in thickness), it is difficult in taking samples from the surface of Type B radwaste by remote operation. But also, sampling should be performed without use of any liquid coolant to avoid the spread of contamination. And all sampling procedures are carried in the hot cell red zone with remote operation. Three kinds of sampling techniques are being developed. They are core sampling, chip sampling, and wedge sampling, which are the candidates of sampling techniques to be applied to ITER hot cell. Object materials for sampling are stainless steel or Cu alloy block in order to simulate ITER Type B radwaste. The best sampling technique for ITER Type B radwaste among the three sampling techniques will be suggested in several months after finishing the related experiment.

  8. Current trends in sample preparation for cosmetic analysis.

    Science.gov (United States)

    Zhong, Zhixiong; Li, Gongke

    2017-01-01

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

  9. Boat sampling technique for assessment of ageing of components

    International Nuclear Information System (INIS)

    Kumar, Kundan; Shyam, T.V.; Kayal, J.N.; Rupani, B.B.

    2006-01-01

    Boat sampling technique (BST) is a surface sampling technique, which has been developed for obtaining, in-situ, metal samples from the surface of an operating component without affecting its operating service life. The BST is non-destructive in nature and the sample is obtained without plastic deformation or without thermal degradation of the parent material. The shape and size of the sample depends upon the shape of the cutter and the surface geometry of the parent material. Miniature test specimens are generated from the sample and the specimens are subjected to various tests, viz. Metallurgical Evaluation, Metallographic Evaluation, Micro-hardness Evaluation, sensitisation test, small punch test etc. to confirm the integrity and assessment of safe operating life of the component. This paper highlights design objective of boat sampling technique, description of sampling module, sampling cutter and its performance evaluation, cutting process, boat samples, operational sequence of sampling module, qualification of sampling module, qualification of sampling technique, qualification of scooped region of the parent material, sample retrieval system, inspection, testing and examination to be carried out on the boat samples and scooped region. (author)

  10. Urine sampling techniques in symptomatic primary-care patients

    DEFF Research Database (Denmark)

    Holm, Anne; Aabenhus, Rune

    2016-01-01

    in infection rate between mid-stream-clean-catch, mid-stream-urine and random samples. Conclusions: At present, no evidence suggests that sampling technique affects the accuracy of the microbiological diagnosis in non-pregnant women with symptoms of urinary tract infection in primary care. However......Background: Choice of urine sampling technique in urinary tract infection may impact diagnostic accuracy and thus lead to possible over- or undertreatment. Currently no evidencebased consensus exists regarding correct sampling technique of urine from women with symptoms of urinary tract infection...... a randomized or paired design to compare the result of urine culture obtained with two or more collection techniques in adult, female, non-pregnant patients with symptoms of urinary tract infection. We evaluated quality of the studies and compared accuracy based on dichotomized outcomes. Results: We included...

  11. [Amanitine determination as an example of peptide analysis in the biological samples with HPLC-MS technique].

    Science.gov (United States)

    Janus, Tomasz; Jasionowicz, Ewa; Potocka-Banaś, Barbara; Borowiak, Krzysztof

    Routine toxicological analysis is mostly focused on the identification of non-organic and organic, chemically different compounds, but generally with low mass, usually not greater than 500–600 Da. Peptide compounds with atomic mass higher than 900 Da are a specific analytical group. Several dozen of them are highly-toxic substances well known in toxicological practice, for example mushroom toxin and animal venoms. In the paper the authors present an example of alpha-amanitin to explain the analytical problems and different original solutions in identifying peptides in urine samples with the use of the universal LC MS/MS procedure. The analyzed material was urine samples collected from patients with potential mushroom intoxication, routinely diagnosed for amanitin determination. Ultra filtration with centrifuge filter tubes (limited mass cutoff 3 kDa) was used. Filtrate fluid was directly injected on the chromatographic column and analyzed with a mass detector (MS/MS). The separation of peptides as organic, amphoteric compounds from biological material with the use of the SPE technique is well known but requires dedicated, specific columns. The presented paper proved that with the fast and simple ultra filtration technique amanitin can be effectively isolated from urine, and the procedure offers satisfactory sensitivity of detection and eliminates the influence of the biological matrix on analytical results. Another problem which had to be solved was the non-characteristic fragmentation of peptides in the MS/MS procedure providing non-selective chromatograms. It is possible to use higher collision energies in the analytical procedure, which results in more characteristic mass spectres, although it offers lower sensitivity. The ultra filtration technique as a procedure of sample preparation is effective for the isolation of amanitin from the biological matrix. The monitoring of selected mass corresponding to transition with the loss of water molecule offers

  12. Quantitative portable gamma-spectroscopy sample analysis for non-standard sample geometries

    International Nuclear Information System (INIS)

    Ebara, S.B.

    1998-01-01

    Utilizing a portable spectroscopy system, a quantitative method for analysis of samples containing a mixture of fission and activation products in nonstandard geometries was developed. This method was not developed to replace other methods such as Monte Carlo or Discrete Ordinates but rather to offer an alternative rapid solution. The method can be used with various sample and shielding configurations where analysis on a laboratory based gamma-spectroscopy system is impractical. The portable gamma-spectroscopy method involves calibration of the detector and modeling of the sample and shielding to identify and quantify the radionuclides present in the sample. The method utilizes the intrinsic efficiency of the detector and the unattenuated gamma fluence rate at the detector surface per unit activity from the sample to calculate the nuclide activity and Minimum Detectable Activity (MDA). For a complex geometry, a computer code written for shielding applications (MICROSHIELD) is utilized to determine the unattenuated gamma fluence rate per unit activity at the detector surface. Lastly, the method is only applicable to nuclides which emit gamma-rays and cannot be used for pure beta or alpha emitters. In addition, if sample self absorption and shielding is significant, the attenuation will result in high MDA's for nuclides which solely emit low energy gamma-rays. The following presents the analysis technique and presents verification results using actual experimental data, rather than comparisons to other approximations such as Monte Carlo techniques, to demonstrate the accuracy of the method given a known geometry and source term. (author)

  13. Bulk analysis using nuclear techniques

    International Nuclear Information System (INIS)

    Borsaru, M.; Holmes, R.J.; Mathew, P.J.

    1983-01-01

    Bulk analysis techniques developed for the mining industry are reviewed. Using penetrating neutron and #betta#-radiations, measurements are obtained directly from a large volume of sample (3-30 kg) #betta#-techniques were used to determine the grade of iron ore and to detect shale on conveyor belts. Thermal neutron irradiation was developed for the simultaneous determination of iron and aluminium in iron ore on a conveyor belt. Thermal-neutron activation analysis includes the determination of alumina in bauxite, and manganese and alumina in manganese ore. Fast neutron activation analysis is used to determine silicon in iron ores, and alumina and silica in bauxite. Fast and thermal neutron activation has been used to determine the soil in shredded sugar cane. (U.K.)

  14. Non-terminal blood sampling techniques in guinea pigs.

    Science.gov (United States)

    Birck, Malene M; Tveden-Nyborg, Pernille; Lindblad, Maiken M; Lykkesfeldt, Jens

    2014-10-11

    Guinea pigs possess several biological similarities to humans and are validated experimental animal models(1-3). However, the use of guinea pigs currently represents a relatively narrow area of research and descriptive data on specific methodology is correspondingly scarce. The anatomical features of guinea pigs are slightly different from other rodent models, hence modulation of sampling techniques to accommodate for species-specific differences, e.g., compared to mice and rats, are necessary to obtain sufficient and high quality samples. As both long and short term in vivo studies often require repeated blood sampling the choice of technique should be well considered in order to reduce stress and discomfort in the animals but also to ensure survival as well as compliance with requirements of sample size and accessibility. Venous blood samples can be obtained at a number of sites in guinea pigs e.g., the saphenous and jugular veins, each technique containing both advantages and disadvantages(4,5). Here, we present four different blood sampling techniques for either conscious or anaesthetized guinea pigs. The procedures are all non-terminal procedures provided that sample volumes and number of samples do not exceed guidelines for blood collection in laboratory animals(6). All the described methods have been thoroughly tested and applied for repeated in vivo blood sampling in studies within our research facility.

  15. The collection and field chemical analysis of water samples

    International Nuclear Information System (INIS)

    Korte, N.E.; Ealey, D.T.; Hollenbach, M.H.

    1984-01-01

    A successful water sampling program requires a clear understanding of appropriate measurement and sampling procedures in order to obtain reliable field data and representative samples. It is imperative that the personnel involved have a thorough knowledge of the limitations of the techniques being used. Though this seems self-evident, many sampling and field-chemical-analysis programs are still not properly conducted. Recognizing these problems, the Department of Energy contracted with Bendix Field Engineering Corporation through the Technical Measurements Center to develop and select procedures for water sampling and field chemical analysis at waste sites. The fundamental causese of poor field programs are addressed in this paper, largely through discussion of specific field-measurement techniques and their limitations. Recommendations for improvement, including quality-assurance measures, are also presented

  16. Analysis of Angolan human hair samples by the k0-NAA technique on the Dalat research reactor

    International Nuclear Information System (INIS)

    Lemos, P.C.D; Ho Manh Dung; Cao Dong Vu; Nguyen Thi Sy; Nguyen Mong Sinh

    2006-01-01

    There is personal difference in concentrations of trace elements in the human hair according to human life or history such as occupation, sex, age, food, habit, social condition and so on. It is also found that the individual's deviation of elemental concentrations reflecting the degree of environmental pollutants exposure to the human body, intakes of food and metabolism. The k 0 -standardization method of neutron activation analysis (k 0 -NAA) on research reactor has been recommended by WHO and IAEA as a main analytical technique with the advantages of sensitivity, precision, accuracy, multi-element and routine. This report presents the results of determination of about 20 elements in 23 human hair samples, which have been collected from different places in Angola by using k 0 -NAA technique on Dalat nuclear research reactor. Accuracy of the method was ascertained by analysis of two human hair certified reference materials (CRMs), i.e. NIES-5 and GBW-09101 and assessed by the deviation of experiment to certified values generally within 10% and U-score values mostly lower 2. (author)

  17. Detection, characterization and quantification of inorganic engineered nanomaterials: A review of techniques and methodological approaches for the analysis of complex samples

    Energy Technology Data Exchange (ETDEWEB)

    Laborda, Francisco, E-mail: flaborda@unizar.es; Bolea, Eduardo; Cepriá, Gemma; Gómez, María T.; Jiménez, María S.; Pérez-Arantegui, Josefina; Castillo, Juan R.

    2016-01-21

    dealing with complex samples. Single- and multi-method approaches applied to solve the nanometrological challenges posed by a variety of stakeholders are also presented. - Highlights: • The challenge to analyze inorganic nanomaterials is described. • Techniques for detection, characterization and quantification of inorganic nanomaterials are presented. • Sample preparation methods for the analysis of nanomaterials in complex samples are presented. • Methodological approaches posed by stakeholders for solving nanometrological problems are discussed.

  18. Detection, characterization and quantification of inorganic engineered nanomaterials: A review of techniques and methodological approaches for the analysis of complex samples

    International Nuclear Information System (INIS)

    Laborda, Francisco; Bolea, Eduardo; Cepriá, Gemma; Gómez, María T.; Jiménez, María S.; Pérez-Arantegui, Josefina; Castillo, Juan R.

    2016-01-01

    dealing with complex samples. Single- and multi-method approaches applied to solve the nanometrological challenges posed by a variety of stakeholders are also presented. - Highlights: • The challenge to analyze inorganic nanomaterials is described. • Techniques for detection, characterization and quantification of inorganic nanomaterials are presented. • Sample preparation methods for the analysis of nanomaterials in complex samples are presented. • Methodological approaches posed by stakeholders for solving nanometrological problems are discussed.

  19. A comparative study of 232Th and 238U activity estimation in soil samples by gamma spectrometry and Neutron Activation Analysis (NAA) technique

    International Nuclear Information System (INIS)

    Rekha, A.K.; Anilkumar, S.; Narayani, K.; Babu, D.A.R.

    2012-01-01

    Radioactivity in the environment is mainly due to the naturally occurring radionuclides like uranium, thorium with their daughter products and potassium. Even though Gamma spectrometry is the most commonly used non destructive method for the quantification of these naturally occurring radionuclides, Neutron Activation Analysis (NAA), a well established analytical technique, can also be used. But the NAA technique is a time consuming process and needs proper standards, proper sample preparation etc. In this paper, the 232 Th and 238 U activity estimated using gamma ray spectrometry and NAA technique are compared. In the case of direct gamma spectrometry method, the samples were analysed after sealing in a 250 ml container. Whereas for the NAA, about 300 mg of each sample, after irradiation were subjected to gamma spectrometry. The 238 U and 232 Th activities (in Bq/kg) in samples were estimated after the proper efficiency correction and were compared. The estimated activities by these two methods are in good agreement. The variation in 238 U and 232 Th activity values are within ± 15% which are acceptable for environmental samples

  20. Enhanced AFCI Sampling, Analysis, and Safeguards Technology Review

    Energy Technology Data Exchange (ETDEWEB)

    John Svoboda

    2009-09-01

    The focus of this study includes the investigation of sampling technologies used in industry and their potential application to nuclear fuel processing. The goal is to identify innovative sampling methods using state of the art techniques that could evolve into the next generation sampling and analysis system for metallic elements. Sampling and analysis of nuclear fuel recycling plant processes is required both to monitor the operations and ensure Safeguards and Security goals are met. In addition, environmental regulations lead to additional samples and analysis to meet licensing requirements. The volume of samples taken by conventional means, can restrain productivity while results samples are analyzed, require process holding tanks that are sized to meet analytical issues rather than process issues (and that create a larger facility footprint), or, in some cases, simply overwhelm analytical laboratory capabilities. These issues only grow when process flowsheets propose new separations systems and new byproduct material for transmutation purposes. Novel means of streamlining both sampling and analysis are being evaluated to increase the efficiency while meeting all requirements for information. This report addresses just a part of the effort to develop and study novel methods by focusing on the sampling and analysis of aqueous samples for metallic elements. It presents an overview of the sampling requirements, including frequency, sensitivity, accuracy, and programmatic drivers, to demonstrate the magnitude of the task. The sampling and analysis system needed for metallic element measurements is then discussed, and novel options being applied to other industrial analytical needs are presented. Inductively coupled mass spectrometry instruments are the most versatile for metallic element analyses and are thus chosen as the focus for the study. Candidate novel means of process sampling, as well as modifications that are necessary to couple such instruments to

  1. Systematic comparison of static and dynamic headspace sampling techniques for gas chromatography.

    Science.gov (United States)

    Kremser, Andreas; Jochmann, Maik A; Schmidt, Torsten C

    2016-09-01

    Six automated, headspace-based sample preparation techniques were used to extract volatile analytes from water with the goal of establishing a systematic comparison between commonly available instrumental alternatives. To that end, these six techniques were used in conjunction with the same gas chromatography instrument for analysis of a common set of volatile organic carbon (VOC) analytes. The methods were thereby divided into three classes: static sampling (by syringe or loop), static enrichment (SPME and PAL SPME Arrow), and dynamic enrichment (ITEX and trap sampling). For PAL SPME Arrow, different sorption phase materials were also included in the evaluation. To enable an effective comparison, method detection limits (MDLs), relative standard deviations (RSDs), and extraction yields were determined and are discussed for all techniques. While static sampling techniques exhibited sufficient extraction yields (approx. 10-20 %) to be reliably used down to approx. 100 ng L(-1), enrichment techniques displayed extraction yields of up to 80 %, resulting in MDLs down to the picogram per liter range. RSDs for all techniques were below 27 %. The choice on one of the different instrumental modes of operation (aforementioned classes) was thereby the most influential parameter in terms of extraction yields and MDLs. Individual methods inside each class showed smaller deviations, and the least influences were observed when evaluating different sorption phase materials for the individual enrichment techniques. The option of selecting specialized sorption phase materials may, however, be more important when analyzing analytes with different properties such as high polarity or the capability of specific molecular interactions. Graphical Abstract PAL SPME Arrow during the extraction of volatile analytes from the headspace of an aqueous sample.

  2. A radioanalytical technique using (n,2n) reaction for the elemental analysis of samples

    International Nuclear Information System (INIS)

    Labor, M.

    1985-11-01

    A technique to determine elemental composition of samples is reported. The principle of the technique employs the internal standard method and involves the resolution of complex annihilation spectra. The technique has been applied to the determination of the mass of nitrogen, msub(N), and that of potassium, msub(K), in known masses of potassium nitrate. The percentage difference between the calculated mass and actual masses in 2g and 3g of potassium nitrate is 1.0 and 0.7 respectively for potassium, and 1.0 for nitrogen. The use of more simultaneous equations than necessary in solving for msub(N) and msub(K) offers one of the advantages of the technique. (author)

  3. Sample Preparation Report of the Fourth OPCW Confidence Building Exercise on Biomedical Sample Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Udey, R. N. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Corzett, T. H. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Alcaraz, A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2014-07-03

    Following the successful completion of the 3rd biomedical confidence building exercise (February 2013 – March 2013), which included the analysis of plasma and urine samples spiked at low ppb levels as part of the exercise scenario, another confidence building exercise was targeted to be conducted in 2014. In this 4th exercise, it was desired to focus specifically on the analysis of plasma samples. The scenario was designed as an investigation of an alleged use of chemical weapons where plasma samples were collected, as plasma has been reported to contain CWA adducts which remain present in the human body for several weeks (Solano et al. 2008). In the 3rd exercise most participants used the fluoride regeneration method to analyze for the presence of nerve agents in plasma samples. For the 4th biomedical exercise it was decided to evaluate the analysis of human plasma samples for the presence/absence of the VX adducts and aged adducts to blood proteins (e.g., VX-butyrylcholinesterase (BuChE) and aged BuChE adducts using a pepsin digest technique to yield nonapeptides; or equivalent). As the aging of VX-BuChE adducts is relatively slow (t1/2 = 77 hr at 37 °C [Aurbek et al. 2009]), soman (GD), which ages much more quickly (t1/2 = 9 min at 37 °C [Masson et al. 2010]), was used to simulate an aged VX sample. Additional objectives of this exercise included having laboratories assess novel OP-adducted plasma sample preparation techniques and analytical instrumentation methodologies, as well as refining/designating the reporting formats for these new techniques.

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

    Science.gov (United States)

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

    2017-11-01

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

  5. The role of graphene-based sorbents in modern sample preparation techniques.

    Science.gov (United States)

    de Toffoli, Ana Lúcia; Maciel, Edvaldo Vasconcelos Soares; Fumes, Bruno Henrique; Lanças, Fernando Mauro

    2018-01-01

    The application of graphene-based sorbents in sample preparation techniques has increased significantly since 2011. These materials have good physicochemical properties to be used as sorbent and have shown excellent results in different sample preparation techniques. Graphene and its precursor graphene oxide have been considered to be good candidates to improve the extraction and concentration of different classes of target compounds (e.g., parabens, polycyclic aromatic hydrocarbon, pyrethroids, triazines, and so on) present in complex matrices. Its applications have been employed during the analysis of different matrices (e.g., environmental, biological and food). In this review, we highlight the most important characteristics of graphene-based material, their properties, synthesis routes, and the most important applications in both off-line and on-line sample preparation techniques. The discussion of the off-line approaches includes methods derived from conventional solid-phase extraction focusing on the miniaturized magnetic and dispersive modes. The modes of microextraction techniques called stir bar sorptive extraction, solid phase microextraction, and microextraction by packed sorbent are discussed. The on-line approaches focus on the use of graphene-based material mainly in on-line solid phase extraction, its variation called in-tube solid-phase microextraction, and on-line microdialysis systems. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Instrumental neutron activation analysis of soil sample

    International Nuclear Information System (INIS)

    Abdul Khalik Haji Wood.

    1983-01-01

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

  7. Quantitative portable gamma spectroscopy sample analysis for non-standard sample geometries

    International Nuclear Information System (INIS)

    Enghauser, M.W.; Ebara, S.B.

    1997-01-01

    Utilizing a portable spectroscopy system, a quantitative method for analysis of samples containing a mixture of fission and activation products in nonstandard geometries was developed. The method can be used with various sample and shielding configurations where analysis on a laboratory based gamma spectroscopy system is impractical. The portable gamma spectroscopy method involves calibration of the detector and modeling of the sample and shielding to identify and quantify the radionuclides present in the sample. The method utilizes the intrinsic efficiency of the detector and the unattenuated gamma fluence rate at the detector surface per unit activity from the sample to calculate the nuclide activity and Minimum Detectable Activity (MDA). For a complex geometry, a computer code written for shielding applications (MICROSHIELD) is utilized to determine the unattenuated gamma fluence rate per unit activity at the detector surface. Lastly, the method is only applicable to nuclides which emit gamma rays and cannot be used for pure beta emitters. In addition, if sample self absorption and shielding is significant, the attenuation will result in high MDA's for nuclides which solely emit low energy gamma rays. The following presents the analysis technique and presents verification results demonstrating the accuracy of the method

  8. Ion-trap tandem mass spectrometry. A reliable technique for the analysis of PCDD/Fs and dioxin-like PCBs in food and feed samples

    Energy Technology Data Exchange (ETDEWEB)

    Santos, F J; Malavia, J; Galceran, M T [Barcelona Univ. (Spain). Dept. of Analytical Chemistry; Abalos, M; Abad, E; Rivera, J [Mass Spectrometry Laboratory, Dept. of Ecotechnologies, IIQAB-CSIC, Barcelona (Spain)

    2004-09-15

    The recent establishment of maximum residue limits for polychlorodibenzo-pdioxins (PCDDs) and dibenzofurans (PCDFs) in food and feed samples by the European Community and the future inclusion of dioxin-like polychlorinated biphenyls (dl-PCBs) in these values at the end of 2006, has led to an important increase on the routine analysis of these compounds. Therefore, there is a clear need to have powerful sensitive and selective methods for the analysis of these compounds at low concentration levels. Actually, gas chromatography coupled with high resolution mass spectrometry (GC-HRMS) is the technique of reference for the determination of these analytes in environmental and food samples due to its high sensitivity and selectivity. Nevertheless, this technique is relatively expensive and requires qualifier personnel. Therefore, the development of more economical but reliable methods that can deliver results comparable to GC-HRMS is required. During the last years, gas chromatography coupled with ion trap mass spectrometry (GC-ITMS) working in MS/MS mode has become an interesting alternative technique to GC-HRMS for the analysis of PCDD/Fs and dl-PCBs. The aim of the present work is to demonstrate the ability of the gas chromatography coupled with ion-trap tandem mass spectrometry (GC-ITMS/MS) for the analysis of PCDD/Fs and dl-PCBs in food and feed samples. This work was performed on the framework of the European research project called DIFFERENCE (Dioxins in Food and Feed - Reference methods and New Certified Reference Materials) with the objective to validate the GC-ITMS/MS method as alternative to HRMS in order to reduce the cost of dioxin analysis. The results and conclusions of the evaluation study are presented here.

  9. The use of ICP-MS and LA-ICP-MS techniques for uranium analysis in real-life swipe samples for safeguards purposes

    Energy Technology Data Exchange (ETDEWEB)

    Pestana, Rafael C.B.; Sarkis, Jorge E.S.; Carvalho, Elita F.U., E-mail: rcbpestana@gmail.com, E-mail: jesarkis@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Abreu Junior, Cassio H. [Centro de Energia Nuclear na Agricultura (CENA/USP), Piracicaba, SP (Brazil)

    2013-07-01

    Environmental swipe sampling for safeguards purposes is a powerful tool to detect undeclared materials and activities, and has been used by the International Atomic Energy Agency since 1997. This work describes the utilization of the inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for determining uranium isotopic ratios in a real-life swipe samples collected in a conversion plant at IPEN/CNEN, Brazil. Uncertainties were estimated by following the International Organization for Standardization - Guide to the Expression of Uncertainties in Measurement (ISO GUM), with a confidence level of 95%. The major uncertainties percentage for n({sup 235}U)/n({sup 238}U) ratio for ICP-MS was 3% and for LA-ICP-MS was 30% The values of uranium isotopic ratios obtained for each technique demonstrate the viability of these analytical techniques as an alternative tool for uranium analysis in swipe samples for safeguards purposes. (author)

  10. The use of ICP-MS and LA-ICP-MS techniques for uranium analysis in real-life swipe samples for safeguards purposes

    International Nuclear Information System (INIS)

    Pestana, Rafael C.B.; Sarkis, Jorge E.S.; Carvalho, Elita F.U.; Abreu Junior, Cassio H.

    2013-01-01

    Environmental swipe sampling for safeguards purposes is a powerful tool to detect undeclared materials and activities, and has been used by the International Atomic Energy Agency since 1997. This work describes the utilization of the inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for determining uranium isotopic ratios in a real-life swipe samples collected in a conversion plant at IPEN/CNEN, Brazil. Uncertainties were estimated by following the International Organization for Standardization - Guide to the Expression of Uncertainties in Measurement (ISO GUM), with a confidence level of 95%. The major uncertainties percentage for n( 235 U)/n( 238 U) ratio for ICP-MS was 3% and for LA-ICP-MS was 30% The values of uranium isotopic ratios obtained for each technique demonstrate the viability of these analytical techniques as an alternative tool for uranium analysis in swipe samples for safeguards purposes. (author)

  11. A comparative examination of several techniques for the routine determination of mercury in biological samples by neutron activation analysis

    International Nuclear Information System (INIS)

    Faanhof, A.; Das, H.A.

    1978-01-01

    A comparative examination of the most important techniques for the separation of mercury from irradiated biological material was made. Procedures for routine analysis and results for standard materials are given. Activation was performed at a thermal neutron flux of approximately 5x10 12 nxcm -2 xs -1 during ( 3 ) 2 offers a convenient solution to this problem. The variation of the neutron flux with the irradiation position can be measured by the application of thin iron rings as flux monitors. Losses of mercury due to uptake in the wall of the irradiation containers are negligible. The most powerful destruction technique for large samples is that based on a stainless-steel bomb. (T. I.)

  12. Identification of unknown sample using NAA, EDXRF, XRD techniques

    International Nuclear Information System (INIS)

    Dalvi, Aditi A.; Swain, K.K.; Chavan, Trupti; Remya Devi, P.S.; Wagh, D.N.; Verma, R.

    2015-01-01

    Analytical Chemistry Division (ACD), Bhabha Atomic Research Centre (BARC) receives samples from law enforcement agencies such as Directorate of Revenue Intelligence, Customs for analysis. Five unknown grey powdered samples were received for identification and were suspected to be Iridium (Ir). Identification of unknown sample is always a challenging task and suitable analytical techniques have to be judiciously utilized for arriving at the conclusion. Qualitative analysis was carried out using Jordan Valley, EX-3600 M Energy dispersive X-ray fluorescence (EDXRF) spectrometer at ACD, BARC. A SLP series LEO Si (Li) detector (active area: 30 mm 2 ; thickness: 3.5 mm; resolution: 140 eV at 5.9 keV of Mn K X-ray) was used during the measurement and only characteristic X-rays of Ir (Lα: 9.17 keV and Lβ: 10.70 keV) was seen in the X-ray spectrum. X-ray diffraction (XRD) measurement results indicated that the Ir was in the form of metal. To confirm the XRD data, neutron activation analysis (NAA) was carried out by irradiating samples and elemental standards (as comparator) in graphite reflector position of Advanced Heavy Water Reactor Critical Facility (AHWR CF) reactor, BARC, Mumbai. After suitable decay period, gamma activity measurements were carried out using 45% HPGe detector coupled to 8 k multi channel analyzer. Characteristic gamma line at 328.4 keV of the activation product 194 Ir was used for quantification of iridium and relative method of NAA was used for concentration calculations. NAA results confirmed that all the samples were Iridium metal. (author)

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

    Science.gov (United States)

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

    2017-01-01

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

  14. Gold analysis by the gamma absorption technique

    International Nuclear Information System (INIS)

    Kurtoglu, Arzu; Tugrul, A.B.

    2003-01-01

    Gold (Au) analyses are generally performed using destructive techniques. In this study, the Gamma Absorption Technique has been employed for gold analysis. A series of different gold alloys of known gold content were analysed and a calibration curve was obtained. This curve was then used for the analysis of unknown samples. Gold analyses can be made non-destructively, easily and quickly by the gamma absorption technique. The mass attenuation coefficients of the alloys were measured around the K-shell absorption edge of Au. Theoretical mass attenuation coefficient values were obtained using the WinXCom program and comparison of the experimental results with the theoretical values showed generally good and acceptable agreement

  15. Sampling and sample preparation development for analytical and on-line measurement techniques of process liquids; Naeytteenoton ja kaesittelyn kehittaeminen prosessinesteiden analytiikan ja on-line mittaustekniikan tarpeisiin - MPKT 11

    Energy Technology Data Exchange (ETDEWEB)

    Karttunen, K. [Oulu Univ. (Finland)

    1998-12-31

    Main goal of the research project is to develop sampling and sample handling methods and techniques for pulp and paper industry to be used for analysis and on-line purposes. The research focus specially on the research and development of the classification and separation methods and techniques needed for liquid and colloidal substances as well as in ion analysis. (orig.)

  16. Sampling and sample preparation development for analytical and on-line measurement techniques of process liquids; Naeytteenoton ja kaesittelyn kehittaeminen prosessinesteiden analytiikan ja on-line mittaustekniikan tarpeisiin - MPKT 11

    Energy Technology Data Exchange (ETDEWEB)

    Karttunen, K [Oulu Univ. (Finland)

    1999-12-31

    Main goal of the research project is to develop sampling and sample handling methods and techniques for pulp and paper industry to be used for analysis and on-line purposes. The research focus specially on the research and development of the classification and separation methods and techniques needed for liquid and colloidal substances as well as in ion analysis. (orig.)

  17. Quality-assurance techniques used with automated analysis of gamma-ray spectra

    International Nuclear Information System (INIS)

    Killian, E.W.; Koeppen, L.D.; Femec, D.A.

    1994-01-01

    In the course of developing gamma-ray spectrum analysis algorithms for use by the Radiation Measurements Laboratory at the Idaho National Engineering Laboratory (INEL), several techniques have been developed that enhance and verify the quality of the analytical results. The use of these quality-assurance techniques is critical when gamma-ray analysis results from low-level environmental samples are used in risk assessment or site restoration and cleanup decisions. This paper describes four of the quality-assurance techniques that are in routine use at the laboratory. They are used for all types of samples, from reactor effluents to environmental samples. The techniques include: (1) the use of precision pulsers (with subsequent removal) to validate the correct operation of the spectrometer electronics for each and every spectrum acquired, (2) the use of naturally occurring and cosmically induced radionuclides in samples to help verify that the data acquisition and analysis were performed properly, (3) the use of an ambient background correction technique that involves superimposing (open-quotes mappingclose quotes) sample photopeak fitting parameters onto multiple background spectra for accurate and more consistent quantification of the background activities, (4) the use of interactive, computer-driven graphics to review the automated locating and fitting of photopeaks and to allow for manual fitting of photopeaks

  18. Elemental analysis and plant samples at el-Manzala lake by neutron activation analysis technique

    Energy Technology Data Exchange (ETDEWEB)

    Eissa, E A; Rofail, N B; Abdel-Haleem, A S; El-Abbady, W H; Hassan, A M [Arab Republic of Egypt, Atomic energy Authority, Reactor and Neutron Physiscs Department, Cairo (Egypt)

    1996-12-31

    A soil and a plant samples were taken from two locations, Bahr el-Bakar and Bahr Kados at the Manzala lake, where a high pollution is expected. The samples were especially treated and prepared for investigation by thermal neutron activation analysis (NAA). The irradiation facilities of the first egyptian research reactor (ET-R R-1) and the hyper pure germanium (HPGe) detection system were used for such a type of analysis. Among the 34 identified elements Fe, Co, As, Ru, Cd, Te, La, Sm, Eu, Tb, Hg, Th, and U are of a special significance because of their toxic deleterious impact to organisms. This work is a part of a research project concerning pollution studies on the river nile and some lakes of egypt. The data obtained in the present work stand as a reference basic record for any future follow up of the contamination level. 1 tab.

  19. Elemental analysis and plant samples at el-Manzala lake by neutron activation analysis technique

    International Nuclear Information System (INIS)

    Eissa, E.A.; Rofail, N.B.; Abdel-Haleem, A.S.; El-Abbady, W.H.; Hassan, A.M.

    1995-01-01

    A soil and a plant samples were taken from two locations, Bahr el-Bakar and Bahr Kados at the Manzala lake, where a high pollution is expected. The samples were especially treated and prepared for investigation by thermal neutron activation analysis (NAA). The irradiation facilities of the first egyptian research reactor (ET-R R-1) and the hyper pure germanium (HPGe) detection system were used for such a type of analysis. Among the 34 identified elements Fe, Co, As, Ru, Cd, Te, La, Sm, Eu, Tb, Hg, Th, and U are of a special significance because of their toxic deleterious impact to organisms. This work is a part of a research project concerning pollution studies on the river nile and some lakes of egypt. The data obtained in the present work stand as a reference basic record for any future follow up of the contamination level. 1 tab

  20. Trace uranium analysis in Indian coal samples using the fission track technique

    International Nuclear Information System (INIS)

    Jojo, P.J.; Rawat, A.; Kumar, Ashavani; Prasad, Rajendra

    1993-01-01

    The ever-growing demand for energy has resulted in the extensive use of fossil fuels, especially coal, for power generation. Coal and its by-products often contain significant amounts of radionuclides, including uranium, which is the ultimate source of the radioactive gas Radon-222. The present study gives the concentration of uranium in coal samples of different collieries in India, collected from various thermal power plants in the state of Uttar Pradesh. The estimates were made using the fission track technique. Latent damage tracks were not found to be uniformly distributed but showed sun bursts and clusters. Non-uniform distributions of trace elements are a very common phenomenon in rocks. The levels of uranium in the coal samples were found to vary from 2.0 to 4.9 ppm in uniform distributions and from 21.3 to 41.0 ppm in non-uniform distributions. Measurements were also made on fly ash samples where the average uranium concentration was found to be 8.4 and 49.3 ppm in uniform and non-uniform distributions, respectively. (author)

  1. Evaluation of primary immunization coverage of infants under universal immunization programme in an urban area of Bangalore city using cluster sampling and lot quality assurance sampling techniques

    Directory of Open Access Journals (Sweden)

    Punith K

    2008-01-01

    Full Text Available Research Question: Is LQAS technique better than cluster sampling technique in terms of resources to evaluate the immunization coverage in an urban area? Objective: To assess and compare the lot quality assurance sampling against cluster sampling in the evaluation of primary immunization coverage. Study Design: Population-based cross-sectional study. Study Setting: Areas under Mathikere Urban Health Center. Study Subjects: Children aged 12 months to 23 months. Sample Size: 220 in cluster sampling, 76 in lot quality assurance sampling. Statistical Analysis: Percentages and Proportions, Chi square Test. Results: (1 Using cluster sampling, the percentage of completely immunized, partially immunized and unimmunized children were 84.09%, 14.09% and 1.82%, respectively. With lot quality assurance sampling, it was 92.11%, 6.58% and 1.31%, respectively. (2 Immunization coverage levels as evaluated by cluster sampling technique were not statistically different from the coverage value as obtained by lot quality assurance sampling techniques. Considering the time and resources required, it was found that lot quality assurance sampling is a better technique in evaluating the primary immunization coverage in urban area.

  2. Direct Analysis of Samples of Various Origin and Composition Using Specific Types of Mass Spectrometry.

    Science.gov (United States)

    Byliński, Hubert; Gębicki, Jacek; Dymerski, Tomasz; Namieśnik, Jacek

    2017-07-04

    One of the major sources of error that occur during chemical analysis utilizing the more conventional and established analytical techniques is the possibility of losing part of the analytes during the sample preparation stage. Unfortunately, this sample preparation stage is required to improve analytical sensitivity and precision. Direct techniques have helped to shorten or even bypass the sample preparation stage; and in this review, we comment of some of the new direct techniques that are mass-spectrometry based. The study presents information about the measurement techniques using mass spectrometry, which allow direct sample analysis, without sample preparation or limiting some pre-concentration steps. MALDI - MS, PTR - MS, SIFT - MS, DESI - MS techniques are discussed. These solutions have numerous applications in different fields of human activity due to their interesting properties. The advantages and disadvantages of these techniques are presented. The trends in development of direct analysis using the aforementioned techniques are also presented.

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

    Science.gov (United States)

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

    2017-07-01

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

  4. A comparative study of sampling techniques for monitoring carcass contamination

    NARCIS (Netherlands)

    Snijders, J.M.A.; Janssen, M.H.W.; Gerats, G.E.; Corstiaensen, G.P.

    1984-01-01

    Four bacteriological sampling techniques i.e. the excision, double swab, agar contract and modified agar contact techniques were compared by sampling pig carcasses before and after chilling. As well as assessing the advantages and disadvantages of the techniques particular attention was paid to

  5. Sample preparation for special PIE-techniques at ITU

    International Nuclear Information System (INIS)

    Toscano, E.H.; Manzel, R.

    2002-01-01

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

  6. Techniques for sensitivity analysis of SYVAC results

    International Nuclear Information System (INIS)

    Prust, J.O.

    1985-05-01

    Sensitivity analysis techniques may be required to examine the sensitivity of SYVAC model predictions to the input parameter values, the subjective probability distributions assigned to the input parameters and to the relationship between dose and the probability of fatal cancers plus serious hereditary disease in the first two generations of offspring of a member of the critical group. This report mainly considers techniques for determining the sensitivity of dose and risk to the variable input parameters. The performance of a sensitivity analysis technique may be improved by decomposing the model and data into subsets for analysis, making use of existing information on sensitivity and concentrating sampling in regions the parameter space that generates high doses or risks. A number of sensitivity analysis techniques are reviewed for their application to the SYVAC model including four techniques tested in an earlier study by CAP Scientific for the SYVAC project. This report recommends the development now of a method for evaluating the derivative of dose and parameter value and extending the Kruskal-Wallis technique to test for interactions between parameters. It is also recommended that the sensitivity of the output of each sub-model of SYVAC to input parameter values should be examined. (author)

  7. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Urine Samples by Isotope Ratio Mass Spectrometry

    International Nuclear Information System (INIS)

    2010-01-01

    The IAEA has fostered the more widespread use of a stable isotope technique to assess body composition in different population groups to address priority areas in public health nutrition in Member States. It has done this by supporting national and regional nutrition projects through its technical cooperation programme and coordinated research projects over many years. This publication was developed by an international group of experts to provide practical hands-on guidance in the use of this technique in settings where analysis of stable isotope ratios in biological samples is to be made by isotope ratio mass spectrometry. The publication is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical applications of state of the art methodologies to monitor changes in body composition can be found in IAEA Human Health Series No. 3, Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques

  8. Sampling methods for rumen microbial counts by Real-Time PCR techniques

    Directory of Open Access Journals (Sweden)

    S. Puppo

    2010-02-01

    Full Text Available Fresh rumen samples were withdrawn from 4 cannulated buffalo females fed a fibrous diets in order to quantify bacteria concentration in the rumen by Real-Time PCR techniques. To obtain DNA of a good quality from whole rumen fluid, eight (M1-M8 different pre-filtration methods (cheese cloths, glass-fibre and nylon filter in combination with various centrifugation speeds (1000, 5000 and 14,000 rpm were tested. Genomic DNA extraction was performed either on fresh or frozen samples (-20°C. The quantitative bacteria analysis was realized according to Real-Time PCR procedure for Butyrivibrio fibrisolvens reported in literature. M5 resulted the best sampling procedure allowing to obtain a suitable genomic DNA. No differences were revealed between fresh and frozen samples.

  9. Determination of silver, gold, zinc and copper in mineral samples by various techniques of instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Rodriguez R, N. I.; Rios M, C.; Pinedo V, J. L.; Yoho, M.; Landsberger, S.

    2015-09-01

    Using the method of instrumental neutron activation analysis, mineral exploration samples were analyzed in order to determine the concentrations of silver, gold, zinc and copper; these minerals being the main products of benefit of Tizapa and Cozamin mines. Samples were subjected to various techniques, where the type of radiation and counting methods were chosen based on the specific isotopic characteristics of each element. For calibration and determination of concentrations the comparator method was used, certified standards were subjected to the same conditions of irradiation and measurement that the prospecting samples. The irradiations were performed at the research reactor TRIGA Mark II of the University of Texas at Austin. The silver concentrations were determined by Cyclical Epithermal Neutron Activation Analysis. This method in combination with the transfer pneumatic system allowed a good analytical precision and accuracy in prospecting for silver, from photo peak measurement 657.7 keV of short half-life radionuclide 110 Ag. For the determination of gold and zinc, Epithermal Neutron Activation Analysis was used, the photo peaks analyzed corresponded to the energies 411.8 keV of radionuclide 199 Au and 438.6 keV of metastable radionuclide 69m Zn. On the other hand, copper quantification was based on the photo peak analysis of 1039.2 keV produced by the short half-life radionuclide 66 Cu, by Thermal Neutron Activation Analysis. The photo peaks measurement corresponding to gold, zinc and copper was performed using a Compton suppression system, which allowed an improvement in the signal to noise relationship, so that better detection limits and low uncertainties associated with the results were obtained. Comparing elemental concentrations the highest values in silver, zinc and copper was for samples of mine Tizapa. Regarding gold values were found in the same range for both mines. To evaluate the precision and accuracy of the methods used, various geological

  10. Improvements and experience in the analysis of reprocessing samples

    International Nuclear Information System (INIS)

    Koch, L.; Cricchio, A.; Meester, R. de; Romkowski, M.; Wilhelmi, M.; Arenz, H.J.; Stijl, E. van der; Baeckmann, A. von

    1976-01-01

    Improvements in the analysis of input samples for reprocessing were obtained. To cope with the decomposition of reprocessing input solutions owling to the high radioactivity, an aluminium capsule technique was developed. A known amount of the dissolver solution was weighed into an aluminium can, dried, and the capsule was sealed. In this form, the sample could be stored over a long period and could be redissolved later for the analysis. The isotope correlation technique offers an attractive alternative for measuring the plutonium isotopic content in the dissolver solution. Moreover, this technique allows for consistency checks of analytical results. For this purpose, a data bank of correlated isotopic data is in use. To improve the efficiency of analytical work, four automatic instruments have been developed. The conditioning of samples for the U-Pu isotopic measurement was achieved by an automatic ion exchanger. A mass spectrometer, to which a high vacuum lock is connected, allows the automatic measurement of U-Pu samples. A process-computer controls the heating, focusing and scanning processes during the measurement and evaluates the data. To ease the data handling, alpha-spectrometry as well as a balance have been automated. (author)

  11. Non-terminal blood sampling techniques in Guinea pigs

    DEFF Research Database (Denmark)

    Birck, Malene Muusfeldt; Tveden-Nyborg, Pernille; Lindblad, Maiken Marie

    2014-01-01

    Guinea pigs possess several biological similarities to humans and are validated experimental animal models(1-3). However, the use of guinea pigs currently represents a relatively narrow area of research and descriptive data on specific methodology is correspondingly scarce. The anatomical features...... of guinea pigs are slightly different from other rodent models, hence modulation of sampling techniques to accommodate for species-specific differences, e.g., compared to mice and rats, are necessary to obtain sufficient and high quality samples. As both long and short term in vivo studies often require...... repeated blood sampling the choice of technique should be well considered in order to reduce stress and discomfort in the animals but also to ensure survival as well as compliance with requirements of sample size and accessibility. Venous blood samples can be obtained at a number of sites in guinea pigs e...

  12. Solid-phase microextraction for the analysis of biological samples

    NARCIS (Netherlands)

    Theodoridis, G; Koster, EHM; de Jong, GJ

    2000-01-01

    Solid-phase microextraction (SPME) has been introduced for the extraction of organic compounds from environmental samples. This relatively new extraction technique has now also gained a lot of interest in a broad field of analysis including food, biological and pharmaceutical samples. SPME has a

  13. Trace uranium analysis in geological sample by isotope dilution-alpha spectrometry and comparison with other techniques

    International Nuclear Information System (INIS)

    Shihomatsu, H.M.; Iyer, S.S.

    1988-12-01

    Establishment of uranium determination in geological samples by alpha spectrometric isotope dilution technique using 233 U tracer is described in the present work. The various steps involved in the method namely, preparation of the sample, electrodeposition, alpha spectrometry, isotope dilution, calculation of the concentration and error statistics are discussed in detail. The experimental parameters for the electrodeposition of uranium, like current density, pH concentration of the electrolyte solution, deposition time, electrode distance were all optimised based on the efficiency of the deposition. The total accuracy and precision of the IDAS using 233 U tracer in the determination of uranium in mineral and granite samples were of the order of 1 to 2% for the concentration range of 50-1500 ppm of U. Our results are compared with those obtained by others workers using similar and different techniques. (author) [pt

  14. High-throughput droplet analysis and multiplex DNA detection in the microfluidic platform equipped with a robust sample-introduction technique

    International Nuclear Information System (INIS)

    Chen, Jinyang; Ji, Xinghu; He, Zhike

    2015-01-01

    In this work, a simple, flexible and low-cost sample-introduction technique was developed and integrated with droplet platform. The sample-introduction strategy was realized based on connecting the components of positive pressure input device, sample container and microfluidic chip through the tygon tubing with homemade polydimethylsiloxane (PDMS) adaptor, so the sample was delivered into the microchip from the sample container under the driving of positive pressure. This sample-introduction technique is so robust and compatible that could be integrated with T-junction, flow-focus or valve-assisted droplet microchips. By choosing the PDMS adaptor with proper dimension, the microchip could be flexibly equipped with various types of familiar sample containers, makes the sampling more straightforward without trivial sample transfer or loading. And the convenient sample changing was easily achieved by positioning the adaptor from one sample container to another. Benefiting from the proposed technique, the time-dependent concentration gradient was generated and applied for quantum dot (QD)-based fluorescence barcoding within droplet chip. High-throughput droplet screening was preliminarily demonstrated through the investigation of the quenching efficiency of ruthenium complex to the fluorescence of QD. More importantly, multiplex DNA assay was successfully carried out in the integrated system, which shows the practicability and potentials in high-throughput biosensing. - Highlights: • A simple, robust and low-cost sample-introduction technique was developed. • Convenient and flexible sample changing was achieved in microfluidic system. • Novel strategy of concentration gradient generation was presented for barcoding. • High-throughput droplet screening could be realized in the integrated platform. • Multiplex DNA assay was successfully carried out in the droplet platform

  15. High-throughput droplet analysis and multiplex DNA detection in the microfluidic platform equipped with a robust sample-introduction technique

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Jinyang; Ji, Xinghu [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072 (China); He, Zhike, E-mail: zhkhe@whu.edu.cn [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072 (China); Suzhou Institute of Wuhan University, Suzhou 215123 (China)

    2015-08-12

    In this work, a simple, flexible and low-cost sample-introduction technique was developed and integrated with droplet platform. The sample-introduction strategy was realized based on connecting the components of positive pressure input device, sample container and microfluidic chip through the tygon tubing with homemade polydimethylsiloxane (PDMS) adaptor, so the sample was delivered into the microchip from the sample container under the driving of positive pressure. This sample-introduction technique is so robust and compatible that could be integrated with T-junction, flow-focus or valve-assisted droplet microchips. By choosing the PDMS adaptor with proper dimension, the microchip could be flexibly equipped with various types of familiar sample containers, makes the sampling more straightforward without trivial sample transfer or loading. And the convenient sample changing was easily achieved by positioning the adaptor from one sample container to another. Benefiting from the proposed technique, the time-dependent concentration gradient was generated and applied for quantum dot (QD)-based fluorescence barcoding within droplet chip. High-throughput droplet screening was preliminarily demonstrated through the investigation of the quenching efficiency of ruthenium complex to the fluorescence of QD. More importantly, multiplex DNA assay was successfully carried out in the integrated system, which shows the practicability and potentials in high-throughput biosensing. - Highlights: • A simple, robust and low-cost sample-introduction technique was developed. • Convenient and flexible sample changing was achieved in microfluidic system. • Novel strategy of concentration gradient generation was presented for barcoding. • High-throughput droplet screening could be realized in the integrated platform. • Multiplex DNA assay was successfully carried out in the droplet platform.

  16. Trace elements and As speciation analysis of fly ash samples from an Indonesian coal power plant by means of neutron activation analysis and synchrotron based techniques

    International Nuclear Information System (INIS)

    Muhayatun Santoso; Diah Dwiana Lestiani; Endah Damastuti; Syukria Kurniawat; Bennett, J.W.; Juan Jose Leani; Mateusz Czyzycki; Alessandro Migliori; Germanos Karydas, Andreas

    2016-01-01

    The elemental characterization of coal fly ash samples is required to estimate the coal burning emissions into the environment and to assess the potential impact into the biosphere. Fly ash samples collected from a coal fired power plant in center Java, Indonesia were characterized by instrumental neutron activation analysis at two different facilities (BATAN, ANSTO) and synchrotron based techniques at Elettra Italy. Assessment of thirty (30) elements and an investigation of the potential toxicity of As species in coal fly ash were presented. The results obtained are discussed and compared with those reported from other regions of the world. (author)

  17. Analysis of obsidians by PIXE technique

    International Nuclear Information System (INIS)

    Nuncio Q, A.E.

    1998-01-01

    This work presents the characterization of obsydian samples from different mineral sites in Mexico, undertaken by an Ion Beam Analysis: PIXE (Proton Induced X-ray Emission). As part of an intensive investigation of obsidian in Mesoamerica by anthropologists from Mexico National Institute of Anthropology and History, 818 samples were collected from different volcanic sources in central Mexico for the purpose of establishing a data bank of element concentrations of each source. Part of this collection was analyzed by Neutron activation analysis and most of the important elements concentrations reported. In this work, a non-destructive IBA technique (PIXE) are used to analyze obsydian samples. The application of this technique were carried out at laboratories of the ININ Nuclear Center facilities. The samples consisted of of obsydians from ten different volcanic sources. This pieces were mounted on a sample holder designed for the purpose of exposing each sample to the proton beam. This PIXE analysis was carried out with an ET Tandem Accelerator at the ININ. X-ray spectrometry was carried out with an external beam facility employing a Si(Li) detector set at 52.5 degrees in relation to the target normal (parallel to the beam direction) and 4.2 cm away from the target center. A filter was set in front of the detector, to determine the best attenuation conditions to obtain most of the elements, taking into account that X-ray spectra from obsydians are dominated by intense major elements lines. Thus, a 28 μ m- thick aluminium foil absorber was selected and used to reduce the intensity of the major lines as well as pile-up effects. The mean proton energy was 2.62 MeV, and the beam profile was about 4 mm in diameter. As results were founded elemental concentrations of a set of samples from ten different sources: Altotonga (Veracruz), Penjamo (Guanajuato), Otumba (Mexico), Zinapecuaro (Michoacan), Ucareo (Michoacan), Tres Cabezas (Puebla), Sierra Navajas (Hidalgo), Zaragoza

  18. Development of Large Sample Neutron Activation Technique for New Applications in Thailand

    International Nuclear Information System (INIS)

    Laoharojanaphand, S.; Tippayakul, C.; Wonglee, S.; Channuie, J.

    2018-01-01

    The development of the Large Sample Neutron Activation Analysis (LSNAA) in Thailand is presented in this paper. The technique had been firstly developed with rice sample as the test subject. The Thai Research Reactor-1/Modification 1 (TRR-1/M1) was used as the neutron source. The first step was to select and characterize an appropriate irradiation facility for the research. An out-core irradiation facility (A4 position) was first attempted. The results performed with the A4 facility were then used as guides for the subsequent experiments with the thermal column facility. The characterization of the thermal column was performed with Cu-wire to determine spatial distribution without and with rice sample. The flux depression without rice sample was observed to be less than 30% while the flux depression with rice sample increased to within 60%. The flux monitors internal to the rice sample were used to determine average flux over the rice sample. The gamma selfshielding effect during gamma measurement was corrected using the Monte Carlo simulation. The ratio between the efficiencies of the volume source and the point source for each energy point was calculated by the MCNPX code. The research team adopted the k0-NAA methodology to calculate the element concentration in the research. The k0-NAA program which developed by IAEA was set up to simulate the conditions of the irradiation and measurement facilities used in this research. The element concentrations in the bulk rice sample were then calculated taking into account the flux depression and gamma efficiency corrections. At the moment, the results still show large discrepancies with the reference values. However, more research on the validation will be performed to identify sources of errors. Moreover, this LS-NAA technique was introduced for the activation analysis of the IAEA archaeological mock-up. The results are provided in this report. (author)

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

    International Nuclear Information System (INIS)

    Smith, L. L.

    1998-01-01

    water samples. In this SPME technique, a fused-silica fiber coated with a polymeric film is exposed to the sample, extraction is allowed to take place, and then the analytes are thermally desorbed for GC analysis. Unlike liquid-liquid extraction or solid-phase extraction, SPME consumes all of the extracted sample in the analysis, significantly reducing the required sample volume

  20. Comparative Study of Radon Concentration with Two Techniques and Elemental Analysis in Drinking Water Samples of the Jammu District, Jammu and Kashmir, India.

    Science.gov (United States)

    Kumar, Ajay; Kaur, Manpreet; Mehra, Rohit; Sharma, Dinesh Kumar; Mishra, Rosaline

    2017-10-01

    The level of radon concentration has been assessed using the Advanced SMART RnDuo technique in 30 drinking water samples from Jammu district, Jammu and Kashmir, India. The water samples were collected from wells, hand pumps, submersible pumps, and stored waters. The randomly obtained 14 values of radon concentration in water sources using the SMART RnDuo technique have been compared and cross checked by a RAD7 device. A good positive correlation (R = 0.88) has been observed between the two techniques. The overall value of radon concentration in various water sources has ranged from 2.45 to 18.43 Bq L, with a mean value of 8.24 ± 4.04 Bq L, and it agreed well with the recommended limit suggested by the European Commission and UNSCEAR. However, the higher activity of mean radon concentration was found in groundwater drawn from well, hand and submersible pumps as compared to stored water. The total annual effective dose due to radon inhalation and ingestion ranged from 6.69 to 50.31 μSv y with a mean value of 22.48 ± 11.03 μSv y. The total annual effective dose was found to lie within the safe limit (100 μSv y) suggested by WHO. Heavy metal analysis was also carried out in various water sources by using an atomic absorption spectrophotometer (AAS), and the highest value of heavy metals was found mostly in groundwater samples. The obtained results were compared with Indian and International organizations like WHO and the EU Council. Among all the samples, the elemental analysis is not on the exceeding side of the permissible limit.

  1. Investigation of an egyptian phosphate ore sample by neutron activation analysis technique

    International Nuclear Information System (INIS)

    Eissa, E.A.; Aly, R.A.; Rofail, N.B.; Hassan, A.M.

    1995-01-01

    A domestic phosphate ore sample has been analysed by means of prompt and delayed gamma-ray spectrometry following the activation by thermal neutron capture technique. The rabbit pneumatic transfer system (RPTS), long irradiation facility and two Pu/Be (2,5 Ci each) neutron sources set-Pu for prompt (n,gamma) were applied. The high purity germanium (HPGe) gamma-ray spectrometer with a personal computer analyzer (PCA) system were used for spectrum measurements. Programmes on the VAX computer were utilized for estimating the elemental concentrations of 22 out of 36 elements identified in this work. 2 tabs

  2. Multivariate analysis of remote LIBS spectra using partial least squares, principal component analysis, and related techniques

    Energy Technology Data Exchange (ETDEWEB)

    Clegg, Samuel M [Los Alamos National Laboratory; Barefield, James E [Los Alamos National Laboratory; Wiens, Roger C [Los Alamos National Laboratory; Sklute, Elizabeth [MT HOLYOKE COLLEGE; Dyare, Melinda D [MT HOLYOKE COLLEGE

    2008-01-01

    Quantitative analysis with LIBS traditionally employs calibration curves that are complicated by the chemical matrix effects. These chemical matrix effects influence the LIBS plasma and the ratio of elemental composition to elemental emission line intensity. Consequently, LIBS calibration typically requires a priori knowledge of the unknown, in order for a series of calibration standards similar to the unknown to be employed. In this paper, three new Multivariate Analysis (MV A) techniques are employed to analyze the LIBS spectra of 18 disparate igneous and highly-metamorphosed rock samples. Partial Least Squares (PLS) analysis is used to generate a calibration model from which unknown samples can be analyzed. Principal Components Analysis (PCA) and Soft Independent Modeling of Class Analogy (SIMCA) are employed to generate a model and predict the rock type of the samples. These MV A techniques appear to exploit the matrix effects associated with the chemistries of these 18 samples.

  3. Solid phase microextraction headspace sampling of chemical warfare agent contaminated samples : method development for GC-MS analysis

    Energy Technology Data Exchange (ETDEWEB)

    Jackson Lepage, C.R.; Hancock, J.R. [Defence Research and Development Canada, Medicine Hat, AB (Canada); Wyatt, H.D.M. [Regina Univ., SK (Canada)

    2004-07-01

    Defence R and D Canada-Suffield (DRDC-Suffield) is responsible for analyzing samples that are suspected to contain chemical warfare agents, either collected by the Canadian Forces or by first-responders in the event of a terrorist attack in Canada. The analytical techniques used to identify the composition of the samples include gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), Fourier-transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance spectroscopy. GC-MS and LC-MS generally require solvent extraction and reconcentration, thereby increasing sample handling. The authors examined analytical techniques which reduce or eliminate sample manipulation. In particular, this paper presented a screening method based on solid phase microextraction (SPME) headspace sampling and GC-MS analysis for chemical warfare agents such as mustard, sarin, soman, and cyclohexyl methylphosphonofluoridate in contaminated soil samples. SPME is a method which uses small adsorbent polymer coated silica fibers that trap vaporous or liquid analytes for GC or LC analysis. Collection efficiency can be increased by adjusting sampling time and temperature. This method was tested on two real-world samples, one from excavated chemical munitions and the second from a caustic decontamination mixture. 7 refs., 2 tabs., 3 figs.

  4. Nuclear techniques for trace element analysis. PIXE and its applications to biomedical samples

    International Nuclear Information System (INIS)

    Cata-Danil, I.; Moro, R.; Gialanella, G.

    1996-01-01

    Problems in understanding the role of trace elements in the functioning of life processes are discussed. A brief review of the state of the PIXE technique is given. Principles and recent advances in beam systems, instrumentation and sample handling are covered. A rather comprehensive list of references regarding varies methodological aspects and biomedical applications is given. Some applications are discussed. In particular, preliminary results of an investigation regarding pediatric obesity are presented. (author) 5 tabs., 21 refs

  5. Sample preparation procedure for PIXE elemental analysis on soft tissues

    International Nuclear Information System (INIS)

    Kubica, B.; Kwiatek, W.M.; Dutkiewicz, E.M.; Lekka, M.

    1997-01-01

    Trace element analysis is one of the most important field in analytical chemistry. There are several instrumental techniques which are applied for determinations of microscopic elemental content. The PIXE (Proton Induced X-ray Emission) technique is one of the nuclear techniques that is commonly applied for such purpose due to its multielemental analysis possibilities. The aim of this study was to establish the optimal conditions for target preparation procedure. In this paper two different approaches to the topic are presented and widely discussed. The first approach was the traditional pellet technique and the second one was mineralization procedure. For the analysis soft tissue such as liver was used. Some results are also presented on water samples. (author)

  6. A comparison of two common sample preparation techniques for lipid and fatty acid analysis in three different coral morphotypes reveals quantitative and qualitative differences.

    Science.gov (United States)

    Conlan, Jessica A; Rocker, Melissa M; Francis, David S

    2017-01-01

    Lipids are involved in a host of biochemical and physiological processes in corals. Therefore, changes in lipid composition reflect changes in the ecology, nutrition, and health of corals. As such, accurate lipid extraction, quantification, and identification is critical to obtain comprehensive insight into a coral's condition. However, discrepancies exist in sample preparation methodology globally, and it is currently unknown whether these techniques generate analogous results. This study compared the two most common sample preparation techniques for lipid analysis in corals: (1) tissue isolation by air-spraying and (2) crushing the coral in toto . Samples derived from each preparation technique were subsequently analysed to quantify lipids and their constituent classes and fatty acids in four common, scleractinian coral species representing three distinct morphotypes ( Acropora millepora , Montipora crassotuberculata , Porites cylindrica , and Pocillopora damicornis ). Results revealed substantial amounts of organic material, including lipids, retained in the skeletons of all species following air-spraying, causing a marked underestimation of total lipid concentration using this method. Moreover, lipid class and fatty acid compositions between the denuded skeleton and sprayed tissue were substantially different. In particular, the majority of the total triacylglycerol and total fatty acid concentrations were retained in the skeleton (55-69% and 56-64%, respectively). As such, the isolated, sprayed tissue cannot serve as a reliable proxy for lipid quantification or identification in the coral holobiont. The in toto crushing method is therefore recommended for coral sample preparation prior to lipid analysis to capture the lipid profile of the entire holobiont, permitting accurate diagnoses of coral condition.

  7. A comparison of two common sample preparation techniques for lipid and fatty acid analysis in three different coral morphotypes reveals quantitative and qualitative differences

    Directory of Open Access Journals (Sweden)

    Jessica A. Conlan

    2017-08-01

    Full Text Available Lipids are involved in a host of biochemical and physiological processes in corals. Therefore, changes in lipid composition reflect changes in the ecology, nutrition, and health of corals. As such, accurate lipid extraction, quantification, and identification is critical to obtain comprehensive insight into a coral’s condition. However, discrepancies exist in sample preparation methodology globally, and it is currently unknown whether these techniques generate analogous results. This study compared the two most common sample preparation techniques for lipid analysis in corals: (1 tissue isolation by air-spraying and (2 crushing the coral in toto. Samples derived from each preparation technique were subsequently analysed to quantify lipids and their constituent classes and fatty acids in four common, scleractinian coral species representing three distinct morphotypes (Acropora millepora, Montipora crassotuberculata, Porites cylindrica, and Pocillopora damicornis. Results revealed substantial amounts of organic material, including lipids, retained in the skeletons of all species following air-spraying, causing a marked underestimation of total lipid concentration using this method. Moreover, lipid class and fatty acid compositions between the denuded skeleton and sprayed tissue were substantially different. In particular, the majority of the total triacylglycerol and total fatty acid concentrations were retained in the skeleton (55–69% and 56–64%, respectively. As such, the isolated, sprayed tissue cannot serve as a reliable proxy for lipid quantification or identification in the coral holobiont. The in toto crushing method is therefore recommended for coral sample preparation prior to lipid analysis to capture the lipid profile of the entire holobiont, permitting accurate diagnoses of coral condition.

  8. A microhistological technique for analysis of food habits of mycophagous rodents.

    Science.gov (United States)

    Patrick W. McIntire; Andrew B. Carey

    1989-01-01

    We present a technique, based on microhistological analysis of fecal pellets, for quantifying the diets of forest rodents. This technique provides for the simultaneous recording of fungal spores and vascular plant material. Fecal samples should be freeze dried, weighed, and rehydrated with distilled water. We recommend a minimum sampling intensity of 50 fields of view...

  9. Introduction to body composition assessment using the deuterium dilution technique with analysis of saliva samples by fourier transform infrared spectrometry

    International Nuclear Information System (INIS)

    2010-01-01

    For many years, the IAEA has fostered the more widespread use of stable isotope techniques to assess body composition in different population groups to address priority areas in public health nutrition in Member States. The objective is to support national and regional nutrition projects through both the IAEA's technical cooperation programme and its coordinated research projects. In particular, during the last few years, the increased access to analyses of deuterium enrichment by Fourier transform infrared (FTIR) spectrometry has increased the application of this technique in Africa, Asia and Latin America. This publication was developed by an international group of experts to provide practical, hands-on guidance in the use of this technique in settings where the analysis of deuterium enrichment in saliva samples will be made by FTIR. It is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical application of state of the art methodologies to monitor changes in body composition can be found in an IAEA publication entitled Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques (IAEA Human Health Series No. 3)

  10. Characterization of decommissioned reactor internals: Monte Carlo analysis technique

    International Nuclear Information System (INIS)

    Reid, B.D.; Love, E.F.; Luksic, A.T.

    1993-03-01

    This study discusses computer analysis techniques for determining activation levels of irradiated reactor component hardware to yield data for the Department of Energy's Greater-Than-Class C Low-Level Radioactive Waste Program. The study recommends the Monte Carlo Neutron/Photon (MCNP) computer code as the best analysis tool for this application and compares the technique to direct sampling methodology. To implement the MCNP analysis, a computer model would be developed to reflect the geometry, material composition, and power history of an existing shutdown reactor. MCNP analysis would then be performed using the computer model, and the results would be validated by comparison to laboratory analysis results from samples taken from the shutdown reactor. The report estimates uncertainties for each step of the computational and laboratory analyses; the overall uncertainty of the MCNP results is projected to be ±35%. The primary source of uncertainty is identified as the material composition of the components, and research is suggested to address that uncertainty

  11. Uranium content measurement in drinking water samples using track etch technique

    International Nuclear Information System (INIS)

    Kumar, Mukesh; Kumar, Ajay; Singh, Surinder; Mahajan, R.K.; Walia, T.P.S.

    2003-01-01

    The concentration of uranium has been assessed in drinking water samples collected from different locations in Bathinda district, Punjab, India. The water samples are taken from hand pumps and tube wells. Uranium is determined using fission track technique. Uranium concentration in the water samples varies from 1.65±0.06 to 74.98±0.38 μg/l. These values are compared with safe limit values recommended for drinking water. Most of the water samples are found to have uranium concentration above the safe limit. Analysis of some heavy metals (Zn, Cd, Pb and Cu) in water is also done in order to see if some correlation exists between the concentration of uranium and these heavy metals. A weak positive correlation has been observed between the concentration of uranium and heavy metals of Pb, Cd and Cu

  12. Survey of sampling-based methods for uncertainty and sensitivity analysis

    International Nuclear Information System (INIS)

    Helton, J.C.; Johnson, J.D.; Sallaberry, C.J.; Storlie, C.B.

    2006-01-01

    Sampling-based methods for uncertainty and sensitivity analysis are reviewed. The following topics are considered: (i) definition of probability distributions to characterize epistemic uncertainty in analysis inputs (ii) generation of samples from uncertain analysis inputs (iii) propagation of sampled inputs through an analysis (iv) presentation of uncertainty analysis results, and (v) determination of sensitivity analysis results. Special attention is given to the determination of sensitivity analysis results, with brief descriptions and illustrations given for the following procedures/techniques: examination of scatterplots, correlation analysis, regression analysis, partial correlation analysis, rank transformations, statistical tests for patterns based on gridding, entropy tests for patterns based on gridding, nonparametric regression analysis, squared rank differences/rank correlation coefficient test, two-dimensional Kolmogorov-Smirnov test, tests for patterns based on distance measures, top down coefficient of concordance, and variance decomposition

  13. Survey of sampling-based methods for uncertainty and sensitivity analysis.

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, Jay Dean; Helton, Jon Craig; Sallaberry, Cedric J. PhD. (.; .); Storlie, Curt B. (Colorado State University, Fort Collins, CO)

    2006-06-01

    Sampling-based methods for uncertainty and sensitivity analysis are reviewed. The following topics are considered: (1) Definition of probability distributions to characterize epistemic uncertainty in analysis inputs, (2) Generation of samples from uncertain analysis inputs, (3) Propagation of sampled inputs through an analysis, (4) Presentation of uncertainty analysis results, and (5) Determination of sensitivity analysis results. Special attention is given to the determination of sensitivity analysis results, with brief descriptions and illustrations given for the following procedures/techniques: examination of scatterplots, correlation analysis, regression analysis, partial correlation analysis, rank transformations, statistical tests for patterns based on gridding, entropy tests for patterns based on gridding, nonparametric regression analysis, squared rank differences/rank correlation coefficient test, two dimensional Kolmogorov-Smirnov test, tests for patterns based on distance measures, top down coefficient of concordance, and variance decomposition.

  14. Large Sample Neutron Activation Analysis: A Challenge in Cultural Heritage Studies

    International Nuclear Information System (INIS)

    Stamatelatos, I.E.; Tzika, F.

    2007-01-01

    Large sample neutron activation analysis compliments and significantly extends the analytical tools available for cultural heritage and authentication studies providing unique applications of non-destructive, multi-element analysis of materials that are too precious to damage for sampling purposes, representative sampling of heterogeneous materials or even analysis of whole objects. In this work, correction factors for neutron self-shielding, gamma-ray attenuation and volume distribution of the activity in large volume samples composed of iron and ceramic material were derived. Moreover, the effect of inhomogeneity on the accuracy of the technique was examined

  15. Remote sampling and analysis of highly radioactive samples in shielded boxes

    International Nuclear Information System (INIS)

    Kirpikov, D.A.; Miroshnichenko, I.V.; Pykhteev, O.Yu.

    2010-01-01

    The sampling procedure used for highly radioactive coolant water is associated with high risk of personnel irradiation and uncontrolled radioactive contamination. Remote sample manipulation with provision for proper radiation shielding is intended for safety enhancement of the sampling procedure. The sampling lines are located in an isolated compartment, a shielded box. Various equipment which enables remote or automatic sample manipulation is used for this purpose. The main issues of development of the shielded box equipment intended for a wider ranger of remote chemical analyses and manipulation techniques for highly radioactive water samples are considered in the paper. There were three principal directions of work: Transfer of chemical analysis performed in the laboratory inside the shielded box; Prevalence of computer-aided and remote techniques of highly radioactive sample manipulation inside the shielded box; and, Increase in control over sampling and determination of thermal-hydraulic parameters of the coolant water in the sampling lines. The developed equipment and solutions enable remote chemical analysis in the restricted volume of the shielded box by using ion-chromatographic, amperometrical, fluorimetric, flow injection, phototurbidimetric, conductometric and potentiometric methods. Extent of control performed in the shielded box is determined taking into account the requirements of the regulatory documents as well as feasibility and cost of the technical adaptation of various methods to the shielded box conditions. The work resulted in highly precise determination of more than 15 indexes of the coolant water quality performed in on-line mode in the shielded box. It averages to 80% of the total extent of control performed at the prototype reactor plants. The novel solutions for highly radioactive sample handling are implemented in the shielded box (for example, packaging, sample transportation to the laboratory, volume measurement). The shielded box is

  16. Analysis of rocks involving the x-ray diffraction, infrared and thermal gravimetric techniques

    International Nuclear Information System (INIS)

    Ikram, M.; Rauf, M.A.; Munir, N.

    1998-01-01

    Chemical analysis of rocks and minerals are usually obtained by a number of analytical techniques. The purpose of present work is to investigate the chemical composition of the rock samples and also to find that how far the results obtained by different instrumental methods are closely related. Chemical tests wee performed before using the instrumental techniques in order to determined the nature of these rocks. The chemical analysis indicated mainly the presence of carbonate and hence the carbonate nature of these rocks. The x-ray diffraction, infrared spectroscopy and thermal gravimetric analysis techniques were used for the determination of chemical composition of these samples. The results obtained by using these techniques have shown a great deal of similarities. (author)

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

    Directory of Open Access Journals (Sweden)

    Abuzar Kabir

    2017-12-01

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

  18. Arsenic, Antimony, Chromium, and Thallium Speciation in Water and Sediment Samples with the LC-ICP-MS Technique

    Directory of Open Access Journals (Sweden)

    Magdalena Jabłońska-Czapla

    2015-01-01

    Full Text Available Chemical speciation is a very important subject in the environmental protection, toxicology, and chemical analytics due to the fact that toxicity, availability, and reactivity of trace elements depend on the chemical forms in which these elements occur. Research on low analyte levels, particularly in complex matrix samples, requires more and more advanced and sophisticated analytical methods and techniques. The latest trends in this field concern the so-called hyphenated techniques. Arsenic, antimony, chromium, and (underestimated thallium attract the closest attention of toxicologists and analysts. The properties of those elements depend on the oxidation state in which they occur. The aim of the following paper is to answer the question why the speciation analytics is so important. The paper also provides numerous examples of the hyphenated technique usage (e.g., the LC-ICP-MS application in the speciation analysis of chromium, antimony, arsenic, or thallium in water and bottom sediment samples. An important issue addressed is the preparation of environmental samples for speciation analysis.

  19. Quantifying ruminal nitrogen metabolism using the omasal sampling technique in cattle--a meta-analysis.

    Science.gov (United States)

    Broderick, G A; Huhtanen, P; Ahvenjärvi, S; Reynal, S M; Shingfield, K J

    2010-07-01

    Mixed model analysis of data from 32 studies (122 diets) was used to evaluate the precision and accuracy of the omasal sampling technique for quantifying ruminal-N metabolism and to assess the relationships between nonammonia-N flow at the omasal canal and milk protein yield. Data were derived from experiments in cattle fed North American diets (n=36) based on alfalfa silage, corn silage, and corn grain and Northern European diets (n=86) composed of grass silage and barley-based concentrates. In all studies, digesta flow was quantified using a triple-marker approach. Linear regressions were used to predict microbial-N flow to the omasum from intake of dry matter (DM), organic matter (OM), or total digestible nutrients. Efficiency of microbial-N synthesis increased with DM intake and there were trends for increased efficiency with elevated dietary concentrations of crude protein (CP) and rumen-degraded protein (RDP) but these effects were small. Regression of omasal rumen-undegraded protein (RUP) flow on CP intake indicated that an average 32% of dietary CP escaped and 68% was degraded in the rumen. The slope from regression of observed omasal flows of RUP on flows predicted by the National Research Council (2001) model indicated that NRC predicted greater RUP supply. Measured microbial-N flow was, on average, 26% greater than that predicted by the NRC model. Zero ruminal N-balance (omasal CP flow=CP intake) was obtained at dietary CP and RDP concentrations of 147 and 106 g/kg of DM, corresponding to ruminal ammonia-N and milk urea N concentrations of 7.1 and 8.3mg/100mL, respectively. Milk protein yield was positively related to the efficiency of microbial-N synthesis and measured RUP concentration. Improved efficiency of microbial-N synthesis and reduced ruminal CP degradability were positively associated with efficiency of capture of dietary N as milk N. In conclusion, the results of this study indicate that the omasal sampling technique yields valuable estimates

  20. Ion beam analysis techniques applied to large scale pollution studies

    Energy Technology Data Exchange (ETDEWEB)

    Cohen, D D; Bailey, G; Martin, J; Garton, D; Noorman, H; Stelcer, E; Johnson, P [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1994-12-31

    Ion Beam Analysis (IBA) techniques are ideally suited to analyse the thousands of filter papers a year that may originate from a large scale aerosol sampling network. They are fast multi-elemental and, for the most part, non-destructive so other analytical methods such as neutron activation and ion chromatography can be performed afterwards. ANSTO in collaboration with the NSW EPA, Pacific Power and the Universities of NSW and Macquarie has established a large area fine aerosol sampling network covering nearly 80,000 square kilometres of NSW with 25 fine particle samplers. This network known as ASP was funded by the Energy Research and Development Corporation (ERDC) and commenced sampling on 1 July 1991. The cyclone sampler at each site has a 2.5 {mu}m particle diameter cut off and runs for 24 hours every Sunday and Wednesday using one Gillman 25mm diameter stretched Teflon filter for each day. These filters are ideal targets for ion beam analysis work. Currently ANSTO receives 300 filters per month from this network for analysis using its accelerator based ion beam techniques on the 3 MV Van de Graaff accelerator. One week a month of accelerator time is dedicated to this analysis. Four simultaneous accelerator based IBA techniques are used at ANSTO, to analyse for the following 24 elements: H, C, N, O, F, Na, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Cu, Ni, Co, Zn, Br and Pb. The IBA techniques were proved invaluable in identifying sources of fine particles and their spatial and seasonal variations accross the large area sampled by the ASP network. 3 figs.

  1. Ion beam analysis techniques applied to large scale pollution studies

    Energy Technology Data Exchange (ETDEWEB)

    Cohen, D.D.; Bailey, G.; Martin, J.; Garton, D.; Noorman, H.; Stelcer, E.; Johnson, P. [Australian Nuclear Science and Technology Organisation, Lucas Heights, NSW (Australia)

    1993-12-31

    Ion Beam Analysis (IBA) techniques are ideally suited to analyse the thousands of filter papers a year that may originate from a large scale aerosol sampling network. They are fast multi-elemental and, for the most part, non-destructive so other analytical methods such as neutron activation and ion chromatography can be performed afterwards. ANSTO in collaboration with the NSW EPA, Pacific Power and the Universities of NSW and Macquarie has established a large area fine aerosol sampling network covering nearly 80,000 square kilometres of NSW with 25 fine particle samplers. This network known as ASP was funded by the Energy Research and Development Corporation (ERDC) and commenced sampling on 1 July 1991. The cyclone sampler at each site has a 2.5 {mu}m particle diameter cut off and runs for 24 hours every Sunday and Wednesday using one Gillman 25mm diameter stretched Teflon filter for each day. These filters are ideal targets for ion beam analysis work. Currently ANSTO receives 300 filters per month from this network for analysis using its accelerator based ion beam techniques on the 3 MV Van de Graaff accelerator. One week a month of accelerator time is dedicated to this analysis. Four simultaneous accelerator based IBA techniques are used at ANSTO, to analyse for the following 24 elements: H, C, N, O, F, Na, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Cu, Ni, Co, Zn, Br and Pb. The IBA techniques were proved invaluable in identifying sources of fine particles and their spatial and seasonal variations accross the large area sampled by the ASP network. 3 figs.

  2. Separation Techniques for Quantification of Radionuclides in Environmental Samples

    Directory of Open Access Journals (Sweden)

    Dusan Galanda

    2009-01-01

    Full Text Available The reliable and quantitative measurement of radionuclides is important in order to determine environmental quality and radiation safety, and to monitor regulatory compliance. We examined soil samples from Podunajske Biskupice, near the city of Bratislava in the Slovak Republic, for the presence of several natural (238U, 232Th, 40K and anthropogenic (137Cs, 90Sr, 239Pu, 240Pu, 241Am radionuclides. The area is adjacent to a refinery and hazardous waste processing center, as well as the municipal incinerator plant, and so might possess an unusually high level of ecotoxic metals. We found that the levels of both naturally occurring and anthropogenic radionuclides fell within the expected ranges, indicating that these facilities pose no radiological threat to the local environment. During the course of our analysis, we modified existing techniques in order to allow us to handle the unusually large and complex samples that were needed to determine the levels of 239Pu, 240Pu, and 241Am activity. We also rated three commercial techniques for the separation of 90Sr from aqueous solutions and found that two of them, AnaLig Sr-01 and Empore Extraction Disks, were suitable for the quantitative and reliable separation of 90Sr, while the third, Sr-Spec Resin, was less so. The main criterion in evaluating these methods was the chemical recovery of 90Sr, which was less than we had expected. We also considered speed of separation and additional steps needed to prepare the sample for separation.

  3. Review of cleaning techniques and their effects on the chemical composition of foliar samples

    Energy Technology Data Exchange (ETDEWEB)

    Rossini Oliva, S.; Raitio, H.

    2003-07-01

    Chemical foliar analysis is a tool widely used to study tree nutrition and to monitor the impact and extent of air pollutants. This paper reviews a number of cleaning methods, and the effects of cleaning on foliar chemistry. Cleaning may include mechanical techniques such as the use of dry or moistened tissues, shaking, blowing, and brushing, or use various washing techniques with water or other solvents. Owing to the diversity of plant species, tissue differences, etc., there is no standard procedure for all kinds of samples. Analysis of uncleaned leaves is considered a good method for assessing the degree of air contamination because it provides an estimate of the element content of the deposits on leaf surfaces or when the analysis is aimed at the investigation of transfer of elements along the food chain. Sample cleaning is recommended in order (1) to investigate the transfer rate of chemical elements from soil to plants, (2) to qualify the washoff of dry deposition from foliage and (3) to separate superficially absorbed and biomass-incorporated elements. Since there is not a standard cleaning procedure for all kinds of samples and aims, it is advised to conduct a pilot study in order to be able to establish a cleaning procedure to provide reliable foliar data. (orig.)

  4. Experimental study of laser ablation as sample introduction technique for inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Van Winckel, S.

    2001-01-01

    The contribution consists of an abstract of a PhD thesis. In the PhD study, several complementary applications of laser-ablation were investigated in order to characterise experimentally laser ablation (LA) as a sample introduction technique for ICP-MS. Three applications of LA as a sample introduction technique are discussed: (1) the microchemical analysis of the patina of weathered marble; (2) the possibility to measure isotope ratios (in particular Pb isotope ratios in archaeological bronze artefacts); and (3) the determination of Si in Al as part of a dosimetric study of the BR2 reactor vessel

  5. Preparation and analysis of standardized waste samples for Controlled Ecological Life Support Systems (CELSS)

    Science.gov (United States)

    Carden, J. L.; Browner, R.

    1982-01-01

    The preparation and analysis of standardized waste samples for controlled ecological life support systems (CELSS) are considered. Analysis of samples from wet oxidation experiments, the development of ion chromatographic techniques utilizing conventional high pressure liquid chromatography (HPLC) equipment, and an investigation of techniques for interfacing an ion chromatograph (IC) with an inductively coupled plasma optical emission spectrometer (ICPOES) are discussed.

  6. A study on the weather sampling method for probabilistic consequence analysis

    International Nuclear Information System (INIS)

    Oh, Hae Cheol

    1996-02-01

    The main task of probabilistic accident consequence analysis model is to predict the radiological situation and to provide a reliable quantitative data base for making decisions on countermeasures. The magnitude of accident consequence is depended on the characteristic of the accident and the weather coincident. In probabilistic accident consequence analysis, it is necessary to repeat the atmospheric dispersion calculation with several hundreds of weather sequences to predict the full distribution of consequences which may occur following a postulated accident release. It is desirable to select a representative sample of weather sequences from a meteorological record which is typical of the area over which the released radionuclides will disperse and which spans a sufficiently long period. The selection process is done by means of sampling techniques from a full year of hourly weather data characteristic of the plant site. In this study, the proposed Weighted importance sampling method selects proportional to the each bin size to closely approximate the true frequency distribution of weather condition at the site. The Weighted importance sampling method results in substantially less sampling uncertainty than the previous technique. The proposed technique can result in improve confidence in risk estimates

  7. Modern methods of sample preparation for GC analysis

    NARCIS (Netherlands)

    de Koning, S.; Janssen, H.-G.; Brinkman, U.A.Th.

    2009-01-01

    Today, a wide variety of techniques is available for the preparation of (semi-) solid, liquid and gaseous samples, prior to their instrumental analysis by means of capillary gas chromatography (GC) or, increasingly, comprehensive two-dimensional GC (GC × GC). In the past two decades, a large number

  8. Rapid Automated Dissolution and Analysis Techniques for Radionuclides in Recycle Process Streams

    International Nuclear Information System (INIS)

    Sudowe, Ralf; Roman, Audrey; Dailey, Ashlee; Go, Elaine

    2013-01-01

    The analysis of process samples for radionuclide content is an important part of current procedures for material balance and accountancy in the different process streams of a recycling plant. The destructive sample analysis techniques currently available necessitate a significant amount of time. It is therefore desirable to develop new sample analysis procedures that allow for a quick turnaround time and increased sample throughput with a minimum of deviation between samples. In particular, new capabilities for rapid sample dissolution and radiochemical separation are required. Most of the radioanalytical techniques currently employed for sample analysis are based on manual laboratory procedures. Such procedures are time- and labor-intensive, and not well suited for situations in which a rapid sample analysis is required and/or large number of samples need to be analyzed. To address this issue we are currently investigating radiochemical separation methods based on extraction chromatography that have been specifically optimized for the analysis of process stream samples. The influence of potential interferences present in the process samples as well as mass loading, flow rate and resin performance is being studied. In addition, the potential to automate these procedures utilizing a robotic platform is evaluated. Initial studies have been carried out using the commercially available DGA resin. This resin shows an affinity for Am, Pu, U, and Th and is also exhibiting signs of a possible synergistic effects in the presence of iron.

  9. Use of nuclear technique in samples for agricultural purposes

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Kerley A. P. de; Sperling, Eduardo Von, E-mail: kerley@ufmg.br, E-mail: kerleyfisica@yahoo.com.br [Department of Sanitary and Environmental Engineering Federal University of Minas Gerais, Belo Horizonte (Brazil); Menezes, Maria Angela B. C.; Jacomino, Vanusa M.F. [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2013-01-15

    The concern related to environment is growing. Due to this, it is needed to determine chemical elements in a large range of concentration. The neutron activation technique (NAA) determines the elemental composition by the measurement of artificial radioactivity in a sample that was submitted to a neutron flux. NAA is a sensitive and accurate technique with low detection limits. An example of application of NAA was the measurement of concentrations of rare earth elements (REE) in waste samples of phosphogypsum (PG) and cerrado soil samples (clayey and sandy soils). Additionally, a soil reference material of the International Atomic Energy Agency (IAEA) was also analyzed. The REE concentration in PG samples was two times higher than those found in national fertilizers, (total of 4,000 mg kg{sup -1}), 154 times greater than the values found in the sandy soil (26 mg kg{sup -1}) and 14 times greater than the in clayey soil (280 mg kg{sup -1}). The experimental results for the reference material were inside the uncertainty of the certified values pointing out the accuracy of the method (95%). The determination of La, Ce, Pr, Nd, Pm, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb and Lu in the samples and reference material confirmed the versatility of the technique on REE determination in soil and phosphogypsum samples that are matrices for agricultural interest. (author)

  10. Use of nuclear technique in samples for agricultural purposes

    International Nuclear Information System (INIS)

    Oliveira, Kerley A. P. de; Sperling, Eduardo Von; Menezes, Maria Angela B. C.; Jacomino, Vanusa M.F.

    2013-01-01

    The concern related to environment is growing. Due to this, it is needed to determine chemical elements in a large range of concentration. The neutron activation technique (NAA) determines the elemental composition by the measurement of artificial radioactivity in a sample that was submitted to a neutron flux. NAA is a sensitive and accurate technique with low detection limits. An example of application of NAA was the measurement of concentrations of rare earth elements (REE) in waste samples of phosphogypsum (PG) and cerrado soil samples (clayey and sandy soils). Additionally, a soil reference material of the International Atomic Energy Agency (IAEA) was also analyzed. The REE concentration in PG samples was two times higher than those found in national fertilizers, (total of 4,000 mg kg -1 ), 154 times greater than the values found in the sandy soil (26 mg kg -1 ) and 14 times greater than the in clayey soil (280 mg kg -1 ). The experimental results for the reference material were inside the uncertainty of the certified values pointing out the accuracy of the method (95%). The determination of La, Ce, Pr, Nd, Pm, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb and Lu in the samples and reference material confirmed the versatility of the technique on REE determination in soil and phosphogypsum samples that are matrices for agricultural interest. (author)

  11. Automatic sample changer for neutron activation analysis at CDTN, Brazil

    International Nuclear Information System (INIS)

    Aimore Dutra Neto; Oliveira Pelaes, Ana Clara; Jacimovic, Radojko

    2018-01-01

    An automatic sample changer was recently developed and installed in the Neutron Activation Analysis (NAA) Laboratory. The certified reference material BCR-320R, Channel Sediment, was analysed in order to verify the reliability of the results obtained by NAA, k 0 -standardisation method, using this automatic system during the gamma-ray measurement step. The results were compared to those manually obtained. The values pointed out that the automatic sample changer is working properly. This changer will increase the productiveness of the neutron activation technique applied at Nuclear Technology Development Centre, CDTN/CNEN expanding its competitiveness as an analytical technique in relation to other techniques. (author)

  12. Optical transmission testing based on asynchronous sampling techniques: images analysis containing chromatic dispersion using convolutional neural network

    Science.gov (United States)

    Mrozek, T.; Perlicki, K.; Tajmajer, T.; Wasilewski, P.

    2017-08-01

    The article presents an image analysis method, obtained from an asynchronous delay tap sampling (ADTS) technique, which is used for simultaneous monitoring of various impairments occurring in the physical layer of the optical network. The ADTS method enables the visualization of the optical signal in the form of characteristics (so called phase portraits) that change their shape under the influence of impairments such as chromatic dispersion, polarization mode dispersion and ASE noise. Using this method, a simulation model was built with OptSim 4.0. After the simulation study, data were obtained in the form of images that were further analyzed using the convolutional neural network algorithm. The main goal of the study was to train a convolutional neural network to recognize the selected impairment (distortion); then to test its accuracy and estimate the impairment for the selected set of test images. The input data consisted of processed binary images in the form of two-dimensional matrices, with the position of the pixel. This article focuses only on the analysis of images containing chromatic dispersion.

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

    International Nuclear Information System (INIS)

    Barnes, R.M.

    2002-01-01

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

  14. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Urine Samples by Isotope Ratio Mass Spectrometry (French Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    The IAEA has fostered the more widespread use of a stable isotope technique to assess body composition in different population groups to address priority areas in public health nutrition in Member States. It has done this by supporting national and regional nutrition projects through its technical cooperation programme and coordinated research projects over many years. This publication was developed by an international group of experts to provide practical hands-on guidance in the use of this technique in settings where analysis of stable isotope ratios in biological samples is to be made by isotope ratio mass spectrometry. The publication is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical applications of state of the art methodologies to monitor changes in body composition can be found in IAEA Human Health Series No. 3, Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques

  15. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Urine Samples by Isotope Ratio Mass Spectrometry (Spanish Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    The IAEA has fostered the more widespread use of a stable isotope technique to assess body composition in different population groups to address priority areas in public health nutrition in Member States. It has done this by supporting national and regional nutrition projects through its technical cooperation programme and coordinated research projects over many years. This publication was developed by an international group of experts to provide practical hands-on guidance in the use of this technique in settings where analysis of stable isotope ratios in biological samples is to be made by isotope ratio mass spectrometry. The publication is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical applications of state of the art methodologies to monitor changes in body composition can be found in IAEA Human Health Series No. 3, Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques

  16. Modern Trends in Neutron Activation Analysis. Applications to some African Environmental Samples

    International Nuclear Information System (INIS)

    Hassan, A.M.

    2009-01-01

    This review covers the results of several published articles which deal with the modern trends in neutron activation analysis techniques using some of African research reactors for some environmental samples. The samples used have been collected from different areas in Egypt, South Africa, Ghana, Morocco, Nigeria, and Algeria. The neutron irradiation facilities and the advanced detection systems in each country are outlined. The prompt and delayed gamma-rays emitted due to neutron capture have been applied for investigation of the elemental constituents of such samples. Covered applications include exploration, mining, industrial environment, pollution of air, foodstuffs, soils and irrigation water samples. Some of the developed software programmes as well as the modern methods of data analysis are presented. The thermal and epithermal neutron activation analysis techniques have been applied for estimation of major, minor and trace elements in each material. Some of these data are presented with several comments.

  17. Direct analysis of biological samples by total reflection X-ray fluorescence

    International Nuclear Information System (INIS)

    Lue M, Marco P.; Hernandez-Caraballo, Edwin A.

    2004-01-01

    The technique of total reflection X-ray fluorescence (TXRF) is well suited for the direct analysis of biological samples due to the low matrix interferences and simultaneous multi-element nature. Nevertheless, biological organic samples are frequently analysed after digestion procedures. The direct determination of analytes requires shorter analysis time, low reactive consumption and simplifies the whole analysis process. On the other hand, the biological/clinical samples are often available in minimal amounts and routine studies require the analysis of large number of samples. To overcome the difficulties associated with the analysis of organic samples, particularly of solid ones, different procedures of sample preparation and calibration to approach the direct analysis have been evaluated: (1) slurry sampling, (2) Compton peak standardization, (3) in situ microwave digestion, (4) in situ chemical modification and (5) direct analysis with internal standardization. Examples of analytical methods developed by our research group are discussed. Some of them have not been previously published, illustrating alternative strategies for coping with various problems that may be encountered in the direct analysis by total reflection X-ray fluorescence spectrometry

  18. The electron transport problem sampling by Monte Carlo individual collision technique

    International Nuclear Information System (INIS)

    Androsenko, P.A.; Belousov, V.I.

    2005-01-01

    The problem of electron transport is of most interest in all fields of the modern science. To solve this problem the Monte Carlo sampling has to be used. The electron transport is characterized by a large number of individual interactions. To simulate electron transport the 'condensed history' technique may be used where a large number of collisions are grouped into a single step to be sampled randomly. Another kind of Monte Carlo sampling is the individual collision technique. In comparison with condensed history technique researcher has the incontestable advantages. For example one does not need to give parameters altered by condensed history technique like upper limit for electron energy, resolution, number of sub-steps etc. Also the condensed history technique may lose some very important tracks of electrons because of its limited nature by step parameters of particle movement and due to weakness of algorithms for example energy indexing algorithm. There are no these disadvantages in the individual collision technique. This report presents some sampling algorithms of new version BRAND code where above mentioned technique is used. All information on electrons was taken from Endf-6 files. They are the important part of BRAND. These files have not been processed but directly taken from electron information source. Four kinds of interaction like the elastic interaction, the Bremsstrahlung, the atomic excitation and the atomic electro-ionization were considered. In this report some results of sampling are presented after comparison with analogs. For example the endovascular radiotherapy problem (P2) of QUADOS2002 was presented in comparison with another techniques that are usually used. (authors)

  19. Recent trends in sorption-based sample preparation and liquid chromatography techniques for food analysis.

    Science.gov (United States)

    V Soares Maciel, Edvaldo; de Toffoli, Ana Lúcia; Lanças, Fernando Mauro

    2018-04-20

    The accelerated rising of the world's population increased the consumption of food, thus demanding more rigors in the control of residue and contaminants in food-based products marketed for human consumption. In view of the complexity of most food matrices, including fruits, vegetables, different types of meat, beverages, among others, a sample preparation step is important to provide more reliable results when combined with HPLC separations. An adequate sample preparation step before the chromatographic analysis is mandatory in obtaining higher precision and accuracy in order to improve the extraction of the target analytes, one of the priorities in analytical chemistry. The recent discovery of new materials such as ionic liquids, graphene-derived materials, molecularly imprinted polymers, restricted access media, magnetic nanoparticles, and carbonaceous nanomaterials, provided high sensitivity and selectivity results in an extensive variety of applications. These materials, as well as their several possible combinations, have been demonstrated to be highly appropriate for the extraction of different analytes in complex samples such as food products. The main characteristics and application of these new materials in food analysis will be presented and discussed in this paper. Another topic discussed in this review covers the main advantages and limitations of sample preparation microtechniques, as well as their off-line and on-line combination with HPLC for food analysis. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Proton induced x-ray emission analysis of trace elements in thick bread samples

    International Nuclear Information System (INIS)

    Mohamed Baker Al-bedri; Ikram Jameel Abdul Ghani; Ibrahim Abdul Rahman Al-aghil

    2009-01-01

    Proton induced X-ray emission (PIXE) technique has been used for identification and quantitative analysis of the elemental concentration in thick bread samples. Bread samples were air-oven dried at 60degC and milled in a clean agate mortar to homogenize the sample and pressed into a pellet. PIXE technique relies on the analysis of the energy spectra of the characteristic X-ray emitted from the thick bread sample and the orchard leaf standard (NIST-SRM-1571) bombarded with 2.0 MeV protons. The concentration of the elements (Cl, K, Ca, Mn, Fe, Cu, and Zn) in the bread samples was determined by comparison with NIST orchard leaf standard. The accuracy of the measurements ranged between ±2% and ±10% for the most elements detected in this method. The aim of this study is to establish the reference concentration of trace elements in the Iraqi bread using PIXE technique. (author)

  1. Metabolomic analysis using porcine skin: a pilot study of analytical techniques

    OpenAIRE

    Wu, Julie; Fiehn, Oliver; Armstrong, April W

    2014-01-01

    Background: Metabolic byproducts serve as indicators of the chemical processes and can provide valuable information on pathogenesis by measuring the amplified output. Standardized techniques for metabolome extraction of skin samples serve as a critical foundation to this field but have not been developed. Objectives: We sought to determine the optimal cell lysage techniques for skin sample preparation and to compare GC-TOF-MS and UHPLC-QTOF-MS for metabolomic analysis. ...

  2. Analysis of soil samples from OMRE decommissioning project

    International Nuclear Information System (INIS)

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

    1979-01-01

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

  3. Solid Phase Microextraction and Related Techniques for Drugs in Biological Samples

    OpenAIRE

    Moein, Mohammad Mahdi; Said, Rana; Bassyouni, Fatma; Abdel-Rehim, Mohamed

    2014-01-01

    In drug discovery and development, the quantification of drugs in biological samples is an important task for the determination of the physiological performance of the investigated drugs. After sampling, the next step in the analytical process is sample preparation. Because of the low concentration levels of drug in plasma and the variety of the metabolites, the selected extraction technique should be virtually exhaustive. Recent developments of sample handling techniques are directed, from o...

  4. Air pollution studies in Tianjing city using neutron activation analysis techniques

    International Nuclear Information System (INIS)

    Ni Bangfa; Tian Weizhi; Nie Nuiling; Wang Pingsheng

    1999-01-01

    Two sites of airborne sampling from industrial and residential areas were made in Tianjing city during February and June using PM-10 sampler and analyzed by NAA techniques; Comparison of air pollution between urban and rural area in Tianjing city was made using neutron activation analysis techniques and some other data analyzing techniques. (author)

  5. Analysis of Cell Phone Usage Using Correlation Techniques

    OpenAIRE

    T S R MURTHY; D. SIVA RAMA KRISHNA

    2011-01-01

    The present paper is a sample survey analysis, examined based on correlation techniques. The usage ofmobile phones is clearly almost un-avoidable these days and as such the authors have made a systematicsurvey through a well prepared questionnaire on making use of mobile phones to the maximum extent.These samples are various economical groups across a population of over one-lakh people. The resultsare scientifically categorized and interpreted to match the ground reality.

  6. Manipulation of biological samples using micro and nano techniques.

    Science.gov (United States)

    Castillo, Jaime; Dimaki, Maria; Svendsen, Winnie Edith

    2009-01-01

    The constant interest in handling, integrating and understanding biological systems of interest for the biomedical field, the pharmaceutical industry and the biomaterial researchers demand the use of techniques that allow the manipulation of biological samples causing minimal or no damage to their natural structure. Thanks to the advances in micro- and nanofabrication during the last decades several manipulation techniques offer us the possibility to image, characterize and manipulate biological material in a controlled way. Using these techniques the integration of biomaterials with remarkable properties with physical transducers has been possible, giving rise to new and highly sensitive biosensing devices. This article reviews the different techniques available to manipulate and integrate biological materials in a controlled manner either by sliding them along a surface (2-D manipulation), by grapping them and moving them to a new position (3-D manipulation), or by manipulating and relocating them applying external forces. The advantages and drawbacks are mentioned together with examples that reflect the state of the art of manipulation techniques for biological samples (171 references).

  7. The electron transport problem sampling by Monte Carlo individual collision technique

    Energy Technology Data Exchange (ETDEWEB)

    Androsenko, P.A.; Belousov, V.I. [Obninsk State Technical Univ. of Nuclear Power Engineering, Kaluga region (Russian Federation)

    2005-07-01

    The problem of electron transport is of most interest in all fields of the modern science. To solve this problem the Monte Carlo sampling has to be used. The electron transport is characterized by a large number of individual interactions. To simulate electron transport the 'condensed history' technique may be used where a large number of collisions are grouped into a single step to be sampled randomly. Another kind of Monte Carlo sampling is the individual collision technique. In comparison with condensed history technique researcher has the incontestable advantages. For example one does not need to give parameters altered by condensed history technique like upper limit for electron energy, resolution, number of sub-steps etc. Also the condensed history technique may lose some very important tracks of electrons because of its limited nature by step parameters of particle movement and due to weakness of algorithms for example energy indexing algorithm. There are no these disadvantages in the individual collision technique. This report presents some sampling algorithms of new version BRAND code where above mentioned technique is used. All information on electrons was taken from Endf-6 files. They are the important part of BRAND. These files have not been processed but directly taken from electron information source. Four kinds of interaction like the elastic interaction, the Bremsstrahlung, the atomic excitation and the atomic electro-ionization were considered. In this report some results of sampling are presented after comparison with analogs. For example the endovascular radiotherapy problem (P2) of QUADOS2002 was presented in comparison with another techniques that are usually used. (authors)

  8. Sampling and examination methods used for TMI-2 samples

    International Nuclear Information System (INIS)

    Marley, A.W.; Akers, D.W.; McIsaac, C.V.

    1988-01-01

    The purpose of this paper is to summarize the sampling and examination techniques that were used in the collection and analysis of TMI-2 samples. Samples ranging from auxiliary building air to core debris were collected and analyzed. Handling of the larger samples and many of the smaller samples had to be done remotely and many standard laboratory analytical techniques were modified to accommodate the extremely high radiation fields associated with these samples. The TMI-2 samples presented unique problems with sampling and the laboratory analysis of prior molten fuel debris. 14 refs., 8 figs

  9. NAIL SAMPLING TECHNIQUE AND ITS INTERPRETATION

    OpenAIRE

    TZAR MN; LEELAVATHI M

    2011-01-01

    The clinical suspicion of onychomyosis based on appearance of the nails, requires culture for confirmation. This is because treatment requires prolonged use of systemic agents which may cause side effects. One of the common problems encountered is improper nail sampling technique which results in loss of essential information. The unfamiliar terminologies used in reporting culture results may intimidate physicians resulting in misinterpretation and hamper treatment decision. This article prov...

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

    International Nuclear Information System (INIS)

    Whitehead, N.E.

    1985-01-01

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

  11. Collection and preparation of bottom sediment samples for analysis of radionuclides and trace elements

    International Nuclear Information System (INIS)

    2003-07-01

    The publication is the first in a series of TECDOCs on sampling and sample handling as part of the IAEA support to improve reliability of nuclear analytical techniques (NATs) in Member State laboratories. The purpose of the document is to provide information on the methods for collecting sediments, the equipment used, and the sample preparation techniques for radionuclide and elemental analysis. The most appropriate procedures for defining the strategies and criteria for selecting sampling locations, for sample storage and transportation are also given. Elements of QA/QC and documentation needs for sampling and sediment analysis are discussed. Collection and preparation of stream and river bottom sediments, lake bottom sediments, estuary bottom sediments, and marine (shallow) bottom sediments are covered. The document is intended to be a comprehensive manual for the collection and preparation of bottom sediments as a prerequisite to obtain representative and meaningful results using NATs. Quality assurance and quality control (QA/QC) is emphasized as an important aspect to ensure proper collection, transportation, preservation, and analysis since it forms the basis for interpretation and legislation. Although there are many approaches and methods available for sediment analyses, the scope of the report is limited to sample preparation for (1) analysis of radionuclides (including sediment dating using radionuclides such as Pb-210 and Cs-137) and (2) analysis of trace, minor and major elements using nuclear and related analytical techniques such as NAA, XRF and PIXE

  12. Collection and preparation of bottom sediment samples for analysis of radionuclides and trace elements

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2003-07-01

    The publication is the first in a series of TECDOCs on sampling and sample handling as part of the IAEA support to improve reliability of nuclear analytical techniques (NATs) in Member State laboratories. The purpose of the document is to provide information on the methods for collecting sediments, the equipment used, and the sample preparation techniques for radionuclide and elemental analysis. The most appropriate procedures for defining the strategies and criteria for selecting sampling locations, for sample storage and transportation are also given. Elements of QA/QC and documentation needs for sampling and sediment analysis are discussed. Collection and preparation of stream and river bottom sediments, lake bottom sediments, estuary bottom sediments, and marine (shallow) bottom sediments are covered. The document is intended to be a comprehensive manual for the collection and preparation of bottom sediments as a prerequisite to obtain representative and meaningful results using NATs. Quality assurance and quality control (QA/QC) is emphasized as an important aspect to ensure proper collection, transportation, preservation, and analysis since it forms the basis for interpretation and legislation. Although there are many approaches and methods available for sediment analyses, the scope of the report is limited to sample preparation for (1) analysis of radionuclides (including sediment dating using radionuclides such as Pb-210 and Cs-137) and (2) analysis of trace, minor and major elements using nuclear and related analytical techniques such as NAA, XRF and PIXE.

  13. Analysis of fresh fallout from Chinese tests by beta counting technique

    International Nuclear Information System (INIS)

    Mishra, U.C.; Lalit, B.Y.; Shukla, V.K.; Ramachandran, T.V.

    1979-01-01

    The paper describes beta counting techniques used in the analysis of fresh radioactive fallout samples from nuclear weapon tests. Fresh fallout samples have been collected by swiping the exposed portion of the engine covers of commercial aircrafts arriving at Bombay from New York after Chinese tests on September 26, 1976 and September 17, 1977. Activities of short-lived radionuclides such as Ag 111, Sr 89, Mo 99, U 237 and Np 239 were determined using these techniques. The results obtained from this analysis is discussed in brief in relation to the kind of fissile material, the extent of thermonuclear reaction in the weapon and the mode of detonation. (orig.) [de

  14. Trends and applications of integrated automated ultra-trace sample handling and analysis (T9)

    International Nuclear Information System (INIS)

    Kingston, H.M.S.; Ye Han; Stewart, L.; Link, D.

    2002-01-01

    Full text: Automated analysis, sub-ppt detection limits, and the trend toward speciated analysis (rather than just elemental analysis) force the innovation of sophisticated and integrated sample preparation and analysis techniques. Traditionally, the ability to handle samples at ppt and sub-ppt levels has been limited to clean laboratories and special sample handling techniques and equipment. The world of sample handling has passed a threshold where older or 'old fashioned' traditional techniques no longer provide the ability to see the sample due to the influence of the analytical blank and the fragile nature of the analyte. When samples require decomposition, extraction, separation and manipulation, application of newer more sophisticated sample handling systems are emerging that enable ultra-trace analysis and species manipulation. In addition, new instrumentation has emerged which integrate sample preparation and analysis to enable on-line near real-time analysis. Examples of those newer sample-handling methods will be discussed and current examples provided as alternatives to traditional sample handling. Two new techniques applying ultra-trace microwave energy enhanced sample handling have been developed that permit sample separation and refinement while performing species manipulation during decomposition. A demonstration, that applies to semiconductor materials, will be presented. Next, a new approach to the old problem of sample evaporation without losses will be demonstrated that is capable of retaining all elements and species tested. Both of those methods require microwave energy manipulation in specialized systems and are not accessible through convection, conduction, or other traditional energy applications. A new automated integrated method for handling samples for ultra-trace analysis has been developed. An on-line near real-time measurement system will be described that enables many new automated sample handling and measurement capabilities. This

  15. Characterization of Some Iraqi Archaeological Samples Using IBA, Analytical X-ray and Other Complementary Techniques

    International Nuclear Information System (INIS)

    Al-Sarraj, Ziyad Shihab; Damboos, Hassan I; Roumie, Mohamad

    2012-01-01

    The present work aimed at investigating the compositions and microstructures of some archaeological samples which dated back to various periods of the ancient Iraqi civilizations using PIXE, XRF, XRD, and SEM techniques. The models selected for the study (ceramics, glaze, etc.) were diverse in size and nature, therefore a limited number of samples were then butted from them by a small diamond wheel. Conventional powder metallurgy method was then used to prepare the samples. Dried samples were then coated with a thin layer of carbon, and analyzed using the ion beam accelerator of the LAEC. Three other groups of samples were also prepared for the purpose of analysis by X-ray fluorescence (XRF), X-ray diffraction (XRD), and scanning electron microscope (SEM). Analysis results of the chemical composition showed good agreement between the various techniques as well as for phases, while the fine structure analysis obtained by optical and scanning microscopy exhibited features of a structure where it got an intensified densification in the final stage of sintering and accompanied by quasi-homogeneous distribution of the closed pores. This will lead to the conclusion that the temperature used for sintering by ancient Iraqi was sufficient and it may fall in the range between 950-1200°C, also the mixes and the forming methods used by them, were both suitable to obtain good sintered bodies with even distribution of pores. A ring-shaped trace noticed in SEM micrographs need more work and study to explain what it is?

  16. Preparation of quality control samples for thyroid hormones T3 and T4 in radioimmunoassay techniques

    International Nuclear Information System (INIS)

    Ahmed, F.O.A.

    2006-03-01

    Today, the radioimmunoassay becomes one of the best techniques for quantitative analysis of very low concentration of different substances. RIA is being widely used in medical and research laboratories. To maintain high specificity and accuracy in RIA and other related techniques the quality controls must be introduced. In this dissertation quality control samples for thyroid hormones (Triiodothyronine T3 and Thyroxin T4), using RIA techniques. Ready made chinese T4, T3 RIA kits were used. IAEA statistical package were selected.(Author)

  17. Sensitivity analysis techniques applied to a system of hyperbolic conservation laws

    International Nuclear Information System (INIS)

    Weirs, V. Gregory; Kamm, James R.; Swiler, Laura P.; Tarantola, Stefano; Ratto, Marco; Adams, Brian M.; Rider, William J.; Eldred, Michael S.

    2012-01-01

    Sensitivity analysis is comprised of techniques to quantify the effects of the input variables on a set of outputs. In particular, sensitivity indices can be used to infer which input parameters most significantly affect the results of a computational model. With continually increasing computing power, sensitivity analysis has become an important technique by which to understand the behavior of large-scale computer simulations. Many sensitivity analysis methods rely on sampling from distributions of the inputs. Such sampling-based methods can be computationally expensive, requiring many evaluations of the simulation; in this case, the Sobol' method provides an easy and accurate way to compute variance-based measures, provided a sufficient number of model evaluations are available. As an alternative, meta-modeling approaches have been devised to approximate the response surface and estimate various measures of sensitivity. In this work, we consider a variety of sensitivity analysis methods, including different sampling strategies, different meta-models, and different ways of evaluating variance-based sensitivity indices. The problem we consider is the 1-D Riemann problem. By a careful choice of inputs, discontinuous solutions are obtained, leading to discontinuous response surfaces; such surfaces can be particularly problematic for meta-modeling approaches. The goal of this study is to compare the estimated sensitivity indices with exact values and to evaluate the convergence of these estimates with increasing samples sizes and under an increasing number of meta-model evaluations. - Highlights: ► Sensitivity analysis techniques for a model shock physics problem are compared. ► The model problem and the sensitivity analysis problem have exact solutions. ► Subtle details of the method for computing sensitivity indices can affect the results.

  18. Elemental analyses of goundwater: demonstrated advantage of low-flow sampling and trace-metal clean techniques over standard techniques

    Science.gov (United States)

    Creasey, C. L.; Flegal, A. R.

    The combined use of both (1) low-flow purging and sampling and (2) trace-metal clean techniques provides more representative measurements of trace-element concentrations in groundwater than results derived with standard techniques. The use of low-flow purging and sampling provides relatively undisturbed groundwater samples that are more representative of in situ conditions, and the use of trace-element clean techniques limits the inadvertent introduction of contaminants during sampling, storage, and analysis. When these techniques are applied, resultant trace-element concentrations are likely to be markedly lower than results based on standard sampling techniques. In a comparison of data derived from contaminated and control groundwater wells at a site in California, USA, trace-element concentrations from this study were 2-1000 times lower than those determined by the conventional techniques used in sampling of the same wells prior to (5months) and subsequent to (1month) the collections for this study. Specifically, the cadmium and chromium concentrations derived using standard sampling techniques exceed the California Maximum Contaminant Levels (MCL), whereas in this investigation concentrations of both of those elements are substantially below their MCLs. Consequently, the combined use of low-flow and trace-metal clean techniques may preclude erroneous reports of trace-element contamination in groundwater. Résumé L'utilisation simultanée de la purge et de l'échantillonnage à faible débit et des techniques sans traces de métaux permet d'obtenir des mesures de concentrations en éléments en traces dans les eaux souterraines plus représentatives que les résultats fournis par les techniques classiques. L'utilisation de la purge et de l'échantillonnage à faible débit donne des échantillons d'eau souterraine relativement peu perturbés qui sont plus représentatifs des conditions in situ, et le recours aux techniques sans éléments en traces limite l

  19. Multielemental neutron activation analysis of some egyptian cement samples

    International Nuclear Information System (INIS)

    Eissa, E.A.; Rofail, N.B.; Abdel-Basset, N.; Soroor, A.; Hassan, A.M.

    1996-01-01

    Multielemental analysis of normal, Karnak and sea-water cement samples were performed by neutron activation analysis technique using the (ET-R R-1) reactor for sample irradiation. The Data were collected and analysed by means of the (HPGe) detection system and a Pca computer. A total of 23 elements namely, Na, A1, C 1, K, Ca, Sc, Cr, Mn, Fe, Co, Zn, Sr, Ba, La, Sm, Eu, Yb, Lu, Ta, Au, Th and U were identified and analysed with concentrations ranging from 1 ppm upto 62% a comparison between the elemental concentrations of the three cement types is given. 2 tabs

  20. Metabolomic analysis using porcine skin: a pilot study of analytical techniques.

    Science.gov (United States)

    Wu, Julie; Fiehn, Oliver; Armstrong, April W

    2014-06-15

    Metabolic byproducts serve as indicators of the chemical processes and can provide valuable information on pathogenesis by measuring the amplified output. Standardized techniques for metabolome extraction of skin samples serve as a critical foundation to this field but have not been developed. We sought to determine the optimal cell lysage techniques for skin sample preparation and to compare GC-TOF-MS and UHPLC-QTOF-MS for metabolomic analysis. Using porcine skin samples, we pulverized the skin via various combinations of mechanical techniques for cell lysage. After extraction, the samples were subjected to GC-TOF-MS and/or UHPLC-QTOF-MS. Signal intensities from GC-TOF-MS analysis showed that ultrasonication (2.7x107) was most effective for cell lysage when compared to mortar-and-pestle (2.6x107), ball mill followed by ultrasonication (1.6x107), mortar-and-pestle followed by ultrasonication (1.4x107), and homogenization (trial 1: 8.4x106; trial 2: 1.6x107). Due to the similar signal intensities, ultrasonication and mortar-and-pestle were applied to additional samples and subjected to GC-TOF-MS and UHPLC-QTOF-MS. Ultrasonication yielded greater signal intensities than mortar-and-pestle for 92% of detected metabolites following GC-TOF-MS and for 68% of detected metabolites following UHPLC-QTOF-MS. Overall, ultrasonication is the preferred method for efficient cell lysage of skin tissue for both metabolomic platforms. With standardized sample preparation, metabolomic analysis of skin can serve as a powerful tool in elucidating underlying biological processes in dermatological conditions.

  1. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Saliva Samples by Fourier Transform Infrared Spectrometry (Spanish Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    For many years, the IAEA has fostered the more widespread use of stable isotope techniques to assess body composition in different population groups to address priority areas in public health nutrition in Member States. The objective is to support national and regional nutrition projects through both the IAEA's technical cooperation programme and its coordinated research projects. In particular, during the last few years, the increased access to analyses of deuterium enrichment by Fourier transform infrared (FTIR) spectrometry has increased the application of this technique in Africa, Asia and Latin America. This publication was developed by an international group of experts to provide practical, hands-on guidance in the use of this technique in settings where the analysis of deuterium enrichment in saliva samples will be made by FTIR. It is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical application of state of the art methodologies to monitor changes in body composition can be found in an IAEA publication entitled Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques (IAEA Human Health Series No. 3)

  2. Introduction to Body Composition Assessment Using the Deuterium Dilution Technique with Analysis of Saliva Samples by Fourier Transform Infrared Spectrometry (French Edition)

    International Nuclear Information System (INIS)

    2013-01-01

    For many years, the IAEA has fostered the more widespread use of stable isotope techniques to assess body composition in different population groups to address priority areas in public health nutrition in Member States. The objective is to support national and regional nutrition projects through both the IAEA's technical cooperation programme and its coordinated research projects. In particular, during the last few years, the increased access to analyses of deuterium enrichment by Fourier transform infrared (FTIR) spectrometry has increased the application of this technique in Africa, Asia and Latin America. This publication was developed by an international group of experts to provide practical, hands-on guidance in the use of this technique in settings where the analysis of deuterium enrichment in saliva samples will be made by FTIR. It is targeted at new users of this technique, for example nutritionists, analytical chemists and other professionals. More detailed information on the theoretical background and the practical application of state of the art methodologies to monitor changes in body composition can be found in an IAEA publication entitled Assessment of Body Composition and Total Energy Expenditure in Humans by Stable Isotope Techniques (IAEA Human Health Series No. 3)

  3. PANDA-A novel instrument for non-destructive sample analysis

    International Nuclear Information System (INIS)

    Turunen, Jani; Peraejaervi, Kari; Poellaenen, Roy; Toivonen, Harri

    2010-01-01

    An instrument known as PANDA (Particles And Non-Destructive Analysis) for non-destructive sample analysis has been designed and built at the Finnish Radiation and Nuclear Safety Authority (STUK). In PANDA the measurement techniques and instruments designed for the basic research are applied to the analysis of environmental samples. PANDA has two vacuum chambers, one for loading samples and the other for measurements. In the measurement chamber there are two individual measurement positions. Currently the first one hosts an HPGe gamma detector and a position-sensitive alpha detector. The second measurement position is intended for precise characterization of found particles. PANDA's data are recorded in event mode and events are timestamped. In the present article the technical design of PANDA is presented in detail. In addition, its performance using depleted uranium particles and an air filter is demonstrated.

  4. Heating and thermal control of brazing technique to break contamination path for potential Mars sample return

    Science.gov (United States)

    Bao, Xiaoqi; Badescu, Mircea; Sherrit, Stewart; Bar-Cohen, Yoseph; Campos, Sergio

    2017-04-01

    The potential return of Mars sample material is of great interest to the planetary science community, as it would enable extensive analysis of samples with highly sensitive laboratory instruments. It is important to make sure such a mission concept would not bring any living microbes, which may possibly exist on Mars, back to Earth's environment. In order to ensure the isolation of Mars microbes from Earth's Atmosphere, a brazing sealing and sterilizing technique was proposed to break the Mars-to-Earth contamination path. Effectively, heating the brazing zone in high vacuum space and controlling the sample temperature for integrity are key challenges to the implementation of this technique. The break-thechain procedures for container configurations, which are being considered, were simulated by multi-physics finite element models. Different heating methods including induction and resistive/radiation were evaluated. The temperature profiles of Martian samples in a proposed container structure were predicted. The results show that the sealing and sterilizing process can be controlled such that the samples temperature is maintained below the level that may cause damage, and that the brazing technique is a feasible approach to breaking the contamination path.

  5. Activation analysis of gold in geological samples (Paper No. RA-24)

    International Nuclear Information System (INIS)

    Das, N.R.; Bhattacharyya, S.N.

    1990-02-01

    The technique of neutron activation analysis (NAA) has been applied to study the distribution of gold in some geological samples. Traces of gold in the samples were preconcentrated in a solid matrix through a chemical procedure involving solvent extraction using MIBK and coprecipitation with PbS. Gold contents in the samples as determined by NAA vary from ppb to ppm levels. (author)

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

    Science.gov (United States)

    Van Eeckhaut, Ann; Mangelings, Debby

    2015-09-10

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

  7. Analysis of Atorvastatin in Commercial Solid Drugs using the TT-PIGE Technique

    International Nuclear Information System (INIS)

    Younes, G; Zahraman, K; Nsouli, B; Bejjani, A; Mahmoud, R; El-Yazbi, F

    2008-01-01

    The quantification of the active ingredient (Al) in drugs is a crucial and important step in the drug quality control process. This is usually performed by using wet chemical techniques like LC-MS, UV spectrophotometry and other appropriate organic analytical methods. In the case of an active ingredient contains specific heteroatoms (F, S, Cl), elemental IBA techniques can be explored for molecular quantification. IBA techniques permit the analysis of the sample under solid form, without any laborious sample preparations. This is an advantage when the number of sample is relatively large. In this work, we demonstrate the ability of the Thick Target PIGE technique for rapid and accurate quantification of low concentration AtorvastatinTM in three commercial anti-hyperlipidemic drugs (Lipitor, Liponorm and Storvas). (author)

  8. Analysis of Atorvastatin in Commercial Solid Drugs using the TT-PIGE Technique

    Energy Technology Data Exchange (ETDEWEB)

    Younes, G [Beirut Arab University, Faculty of Science, Chemistry Department Beirut (Lebanon); Zahraman, K; Nsouli, B; Bejjani, A [Lebanese Atomic Energy Commission, National Council for Scientific Research, Beirut (Lebanon); Mahmoud, R; El-Yazbi, F [Beirut Arab University, Faculty of Pharmacy, Department of Pharmaceutical and Analytical Chemistry, Beirut (Lebanon)

    2008-07-01

    The quantification of the active ingredient (Al) in drugs is a crucial and important step in the drug quality control process. This is usually performed by using wet chemical techniques like LC-MS, UV spectrophotometry and other appropriate organic analytical methods. In the case of an active ingredient contains specific heteroatoms (F, S, Cl), elemental IBA techniques can be explored for molecular quantification. IBA techniques permit the analysis of the sample under solid form, without any laborious sample preparations. This is an advantage when the number of sample is relatively large. In this work, we demonstrate the ability of the Thick Target PIGE technique for rapid and accurate quantification of low concentration AtorvastatinTM in three commercial anti-hyperlipidemic drugs (Lipitor, Liponorm and Storvas). (author)

  9. Introduction of Flame Atomic Absorption Spectrometry (FAAS) For River Water Samples Analysis

    International Nuclear Information System (INIS)

    Shakirah Abd Shukor; Mohd Suhaimi Hamzah; Shamsiah Abdul Rahman

    2015-01-01

    Metal contamination in water is a major component in the determination of water quality monitoring. In spite of the viability of several other metal ion analysis techniques for river water, atomic absorption spectroscopy (AAS) method is most commonly used due to the reproducibility results, short analysis time, cost effective, lower level detection and robust. Therefore, this article gives an overview on the principles, instrumentation techniques, sample preparations, instrument calibration and data analysis in a simple manner for beginner. (author)

  10. [Mass spectrometry technology and its application in analysis of biological samples].

    Science.gov (United States)

    Zhao, Long-Shan; Li, Qing; Guo, Chao-Wei; Chen, Xiao-Hui; Bi, Kai-Shun

    2012-02-01

    With the excellent merits of wide analytical range, high sensitivity, small sample size, fast analysis speed, good repeatability, simple operation, low mobile phase consumption, as well as its capability of simultaneous isolation and identification, etc, mass spectrometry techniques have become widely used in the area of environmental science, energy chemical industry, biological medicine, and so on. This article reviews the application of mass spectrometry technology in biological sample analysis in the latest three years with the focus on the new applications in pharmacokinetics and bioequivalence, toxicokinetics, pharmacokinetic-pharmacodynamic, population pharmacokinetics, identification and fragmentation pathways of drugs and their metabolites and metabonomics to provide references for further study of biological sample analysis.

  11. Advances in modern sample preparation techniques using microwaves assisted chemistry for metal species determination (W1)

    International Nuclear Information System (INIS)

    Ponard, O.F.X.

    2002-01-01

    Full text: Sample preparation has long been the bottleneck of environmental analysis for both total and species specific analysis. Digestion, extraction and preparation of the analytes are relying on a series of chemical reactions. The introduction of microwave assisted sample preparation has first been viewed as a mean to accelerate the kinetics of digestion of the matrix for total elements and fast samples preparation procedures. However, the extensive development and success of microwave digestion procedures in total elemental analysis has now allowed to have a larger insight of the perspectives offered by this technique. Microwave technologies now offer to have a precise control of the temperature and indirectly control the reaction kinetics taking place during the sample preparation procedures. Microwave assisted chemistry permits to perform simultaneously the fundamental steps required for metal species extraction and derivatization. The number of sample preparation steps used for organotin or organomercury species have been reduced to one and the total time of sample preparation brought down for a few hours to some minutes. Further, the developments of GC/ICP/MS techniques allow to routinely use speciated isotopic dilution methods has internal probe of the chemical reactions. These new approaches allow us to use the addition of the labeled species for isotopic dilution as a mean to evaluate and follow the chemical processes taking place during the extraction procedure. These procedures will help us to understand and check for the stability of the analytes during the chemistry of the sample preparation procedure and bring some insights of the chemistry taking place during the extraction. Understanding the different mechanisms involved in the sample preparation steps will allow us in return to further improve all theses procedures and bring us to the horizon of 'on-line sample preparation and detection'. (author)

  12. Analysis of boron utilization in sample preparation for microorganisms detection by neutron radiography technique

    International Nuclear Information System (INIS)

    Wacha, Reinaldo; Crispim, Verginia R.

    2000-01-01

    The neutron radiography technique applied to the microorganisms detection is the study of a new and faster alternative for diagnosis of infectious means. This work presents the parameters and the effects involved in the use of the boron as a conversion agent, that convert neutrons in a particles, capable ones of generating latent tracks in a solid state nuclear tracks detector, CR-39. The collected samples are doped with the boron by the incubation method, propitiating an interaction microorganisms/boron, that will guarantee the identification of the images of those microorganisms, through your morphology. (author)

  13. Elemental analysis of soil and plant samples at El-Manzala lake neutron activation analysis technique. Vol. 4

    Energy Technology Data Exchange (ETDEWEB)

    Eissa, E A; Rofail, N B; Hassan, A M [Reactor and Neutron Physics Department, Nuclear Research Center, Atomic Energy Authority, Cairo (Egypt); Abd El-Haleem, A S [Radiactive Environment Pollution Department, Hot Laboratories Center, Nuclear Research Center, Atomic Energy Authority, Cairo (Egypt); El-Abbady, W H [Phsics Department, Faculty of Science , Al-Azhar University, (Egypt)

    1996-03-01

    Soil and plant samples were collected from from two locations, Bahr El-Baker, and Bahr kados at the manzala lake, where, where high pollution is expected. The samples were especially treated and prepared for investigation by thermal neutron activation analysis (NAA). The irradiation facilities of the first egyptian research reactor (ET-R R-1), and the hyper pure germanium (HPGe) detection system were used for analysis. Among the 34 identified Fe, Co, As, Cd, Te, La, Sm, Rb, Hg, Th, and U are of a special significance because of the their toxic deleterious impact on living organisms. This work is part of a research project concerning pollution studies on the river Nile and some lakes of egypt. The data obtained in the present work stands as a reference basic record for any future follow up of contamination level. 1 tab.

  14. Elemental analysis of soil and plant samples at El-Manzala lake neutron activation analysis technique. Vol. 4

    International Nuclear Information System (INIS)

    Eissa, E.A.; Rofail, N.B.; Hassan, A.M.; Abd El-Haleem, A.S.; El-Abbady, W.H.

    1996-01-01

    Soil and plant samples were collected from from two locations, Bahr El-Baker, and Bahr kados at the manzala lake, where, where high pollution is expected. The samples were especially treated and prepared for investigation by thermal neutron activation analysis (NAA). The irradiation facilities of the first egyptian research reactor (ET-R R-1), and the hyper pure germanium (HPGe) detection system were used for analysis. Among the 34 identified Fe, Co, As, Cd, Te, La, Sm, Rb, Hg, Th, and U are of a special significance because of the their toxic deleterious impact on living organisms. This work is part of a research project concerning pollution studies on the river Nile and some lakes of egypt. The data obtained in the present work stands as a reference basic record for any future follow up of contamination level. 1 tab

  15. Neutron activation analysis of bulk samples from Chinese ancient porcelain to provenance research

    International Nuclear Information System (INIS)

    Jian Zhu; Wentao Hao; Jianming Zhen; Tongxiu Zhen; Glascock, M.D.

    2013-01-01

    Neutron activation analysis (NAA) is an important technique to determine the provenance of ancient ceramics. The most common technique used for preparing ancient samples for NAA is to grind them into a powder and then encapsulate them before neutron irradiation. Unfortunately, ceramic materials are typically very hard making it a challenge to grind them into a powder. In this study we utilize bulk porcelain samples cut from ancient shards. The bulk samples are irradiated by neutrons alongside samples that have been conventionally ground into a powder. The NAA for both the bulk samples and powders are compared and shown to provide equivalent information regarding their chemical composition. Also, the multivariate statistical have been employed to the analysis data for check the consistency. The findings suggest that NAA results are less dependent on the state of the porcelain sample, and thus bulk samples cut from shards may be used to effectively determine their provenance. (author)

  16. Sampling of Atmospheric Precipitation and Deposits for Analysis of Atmospheric Pollution

    OpenAIRE

    Skarżyńska, K.; Polkowska, Ż; Namieśnik, J.

    2006-01-01

    This paper reviews techniques and equipment for collecting precipitation samples from the atmosphere (fog and cloud water) and from atmospheric deposits (dew, hoarfrost, and rime) that are suitable for the evaluation of atmospheric pollution. It discusses the storage and preparation of samples for analysis and also presents bibliographic information on the concentration ranges of inorganic and organic compounds in the precipitation and atmospheric deposit samples.

  17. Elemental investigation of (Al-Cu) alloys and some geological samples using neutron activation and XRF analysis techniques

    International Nuclear Information System (INIS)

    Hammad, E.A.M.

    2012-01-01

    Neutron activation analysis (NAA) using k 0 - standardization (k 0 -NAA) is well known method for multi-elemental analysis. The method is used to analyze different samples belonging to different fields. In addition, X- ray fluorescence (XRF) is also used for multi-elemental analysis. XRF complements NAA methods. Both methods were used for investigation of some iron ores and aluminum- cupper alloy (Al-Cu) samples. Elemental concentration of Iron ores and Al-Cu alloy samples were determined by k 0 - NAA and XRF methods. The iron ore samples were collected from Wadi Kareim and Umm Nar sites (the Eastern desert of Egypt). Six and two samples representing the ores of Wadi Kareim and Umm Nar, respectively altogether with the standard samples consisting of Fe, Au , Zr and W and the certified reference sample IAEA Soil-7 were irradiated in one of the irradiated boxes at the Second Egyptian Research Reactor (ETRR- 2). The induced activities were counted using an efficiency calibrated HPGe detector systems. The neutron spectrum parameters α and f characterizing the neutron irradiation position that are needed in applying k 0 -NAA method were determined using the activation product of Zr , Au, Fe and W and found α≅ - 0.048 ±0.002 and f ≅ 38± k 0 -NAA method was applied to determine the elemental concentrations in the two iron ore samples. The concentrations determined were found to vary erratically form one sample to another. The results were discussed and compared with similar results in literature. The accuracy of the k 0 - NAA method was checked by determining the elemental concentration in the IAEA-Soil 7 reference sample. The obtained results are compared with the recommended values. Good agreements were found within 10 %. Short time neutron activation analysis (STNAA) was carried out to determine concentration of major elements in Al-Cu alloy samples. Three (Al-Cu) alloys samples with different concentrations of Cu (2, 3.5 and 5 %) altogether. Au standard sample

  18. Development of flow injection analysis technique for uranium estimation

    International Nuclear Information System (INIS)

    Paranjape, A.H.; Pandit, S.S.; Shinde, S.S.; Ramanujam, A.; Dhumwad, R.K.

    1991-01-01

    Flow injection analysis is increasingly used as a process control analytical technique in many industries. It involves injection of the sample at a constant rate into a steady flowing stream of reagent and passing this mixture through a suitable detector. This paper describes the development of such a system for the analysis of uranium (VI) and (IV) and its gross gamma activity. It is amenable for on-line or automated off-line monitoring of uranium and its activity in process streams. The sample injection port is suitable for automated injection of radioactive samples. The performance of the system has been tested for the colorimetric response of U(VI) samples at 410 nm in the range of 35 to 360mg/ml in nitric acid medium using Metrohm 662 Photometer and a recorder as detector assembly. The precision of the method is found to be better than +/- 0.5%. This technique with certain modifications is used for the analysis of U(VI) in the range 0.1-3mg/ailq. by alcoholic thiocynate procedure within +/- 1.5% precision. Similarly the precision for the determination of U(IV) in the range 15-120 mg at 650 nm is found to be better than 5%. With NaI well-type detector in the flow line, the gross gamma counting of the solution under flow is found to be within a precision of +/- 5%. (author). 4 refs., 2 figs., 1 tab

  19. Lutz's spontaneous sedimentation technique and the paleoparasitological analysis of sambaqui (shell mound sediments

    Directory of Open Access Journals (Sweden)

    Morgana Camacho

    2013-04-01

    Full Text Available Parasite findings in sambaquis (shell mounds are scarce. Although the 121 shell mound samples were previously analysed in our laboratory, we only recently obtained the first positive results. In the sambaqui of Guapi, Rio de Janeiro, Brazil, paleoparasitological analysis was performed on sediment samples collected from various archaeological layers, including the superficial layer as a control. Eggs of Acanthocephala, Ascaridoidea and Heterakoidea were found in the archaeological layers. We applied various techniques and concluded that Lutz's spontaneous sedimentation technique is effective for concentrating parasite eggs in sambaqui soil for microscopic analysis.

  20. Lutz's spontaneous sedimentation technique and the paleoparasitological analysis of sambaqui (shell mound) sediments

    Science.gov (United States)

    Camacho, Morgana; Pessanha, Thaíla; Leles, Daniela; Dutra, Juliana MF; Silva, Rosângela; de Souza, Sheila Mendonça; Araujo, Adauto

    2013-01-01

    Parasite findings in sambaquis (shell mounds) are scarce. Although the 121 shell mound samples were previously analysed in our laboratory, we only recently obtained the first positive results. In the sambaqui of Guapi, Rio de Janeiro, Brazil, paleoparasitological analysis was performed on sediment samples collected from various archaeological layers, including the superficial layer as a control. Eggs of Acanthocephala, Ascaridoidea and Heterakoidea were found in the archaeological layers. We applied various techniques and concluded that Lutz's spontaneous sedimentation technique is effective for concentrating parasite eggs in sambaqui soil for microscopic analysis. PMID:23579793

  1. Determination of toxic and trace elements in human hair and sediment samples by reactor neutron activation analysis technique based-on the k-zero method

    International Nuclear Information System (INIS)

    Ho Manh Dung; Nguyen Mong Sinh; Nguyen Thanh Binh; Cao Dong Vu; Nguyen Thi Si

    2004-01-01

    The analysis of human hair can evaluate the degree of environmental pollutants exposure to human body, intakes of food and metabolism. Also, the analysis of sediment can aid in reconstructing the history of changes, understanding human impact on the ecosystem, and suggesting possible remedial strategies. The k o -standardization method of neutron activation analysis (k o -NAA) on research reactor is capable to play an important role as a main analytical technique with the advantages of sensitivity, precision, accuracy, multielement and routine for the sample object. Therefore, the project's aim is to build the k o -NAA procedures on the Dalat research reactor for the analysis of human hair and sediment samples. The K o -NAA procedure on the Dalat research reactor is able to determine of multielement: Ag, Al, As, Br, Ca, Cl, Co, Cr, Cu, Fe, Hg, I, K Mg, Mn, Na, S, Sb, Se, Sr, Ti, V and Zn in The human hair; and of multielement: As, Co, Cr, Cs, Fe, Hf, K, La, Mn, Na Rb, Sb, Sc, Yb and Zn in the sediment. (author)

  2. Neutron activation analysis - an old technique but is it still useful?

    International Nuclear Information System (INIS)

    McOrist, G.D.

    1998-01-01

    Neutron activation analysis (NAA) is a non-destructive technique of analysis making it particularly suitable to analyse certain types of samples or particular elements, such as diamonds, black precious opal and ancient fish fossil bones. It is particularly suited to analysing solid samples since no sample dissolution, with its associated problems, prior to analysis is necessary. NAA is remarkably free of matrix effects essentially eliminating complex pre analysis procedures. It is uniquely suited to determining low levels of certain elements such as Cl, Br and I, particularly in organic samples. Its ability to determine sub-ppm levels of Cl in transformer oils has greatly assisted in the development of a patented method for the destruction of PCB ' s. It is possible to analyse large samples in order to overcome homogeneity problems, which is particularly useful in the precious metals industry. Radiochemical NAA enables the determination of very low levels of particular elements (eg Ta) in samples traditionally difficult to dissolve (author)

  3. Determination of multi-element in marine sediment samples collected in Angola by the k0-NAA technique

    International Nuclear Information System (INIS)

    Teixeira, M.C.P.; Ho Manh Dung; Cao Dong Vu; Nguyen Thi Sy; Nguyen Thanh Binh; Vuong Huu Tan

    2006-01-01

    The marine sediment samples were designed to collect in Angola for marine environmental pollution study. The k 0 -standardization method of neutron activation analysis (k 0 -NAA) on Dalat research reactor has been developed to determine of multi-element in the Angola marine sediment samples. The samples were irradiated in cell 7-1 for short- and middle-lived nuclides and rotary specimen rack for long-lived nuclides. The irradiation facilities were characterized for neutron spectrum parameters and post-activated samples were measured on the calibrated gamma-ray spectrometers using HPGe detectors. The analytical results for 9 marine sediment samples with 27 elements: Al, As, Br, Ca, Ce,Cl, Co, Cs, Dy, Fe, Hf, I, K, Mg, Mn, Na, Rb, Sb, Sc, Se, Sm, Th, Ti, U, V and Zn in term of mean concentration, standard deviation and their content range are shown in the report. The analytical quality assurance was done by analysis of a Japan's certified reference material namely marine sediment NMIJ-CRM-7302a. These preliminary results revealed that the k 0 -NAA technique on the Dalat research reactor is a good analytical technique for determination of multi-element in the marine sediment samples. Some heavy metals and trace elements determined in this work possibly connected to the human activities at the sampling region. (author)

  4. Analysis of marine samples by neutron-induced prompt gamma-ray technique and ICP-MS

    International Nuclear Information System (INIS)

    Yonezawa, C.; Matsue, H.; McKay, K.; Povinec, P.

    2001-01-01

    Multi-element and isotopic analyses of oils and marine environmental samples were carried out to estimate a contamination source using a 'finger printing' method. Elemental analyses were carried out using neutron-induced prompt gamma-ray analysis (PGA), instrumental neutron activation analysis (INAA) at the Japan Atomic Institute, Tokai-mura, Japan (JAERI) and ICP-MS in the IAEA Marine Environment Laboratory, Monaco (MEL). Fifteen elements including light elements, H, B, N, Si and Ca, which cannot be determined by INAA and ICP-MS, were determined by PGA. A total of 47 elements were determined in the present study. The potential of PGA for the determination of isotopic ratios was tested by measuring 34 S/ 32 S ratios in oils. The evaluation of historical records of marine environmental conditions using annual bands in coral samples was also investigated. (author)

  5. XRF analysis of mineralised samples

    International Nuclear Information System (INIS)

    Ahmedali, T.

    2002-01-01

    Full text: Software now supplied by instrument manufacturers has made it practical and convenient for users to analyse unusual samples routinely. Semiquantitative scanning software can be used for rapid preliminary screening of elements ranging from Carbon to Uranium, prior to assigning mineralised samples to an appropriate quantitative analysis routine. The general quality and precision of analytical results obtained from modern XRF spectrometers can be significantly enhanced by several means: a. Modifications in preliminary sample preparation can result in less contamination from crushing and grinding equipment. Optimised techniques of actual sample preparation can significantly increase precision of results. b. Employment of automatic data recording balances and the use of catch weights during sample preparation reduces technician time as well as weighing errors. * c. Consistency of results can be improved significantly by the use of appropriate stable drift monitors with a statistically significant content of the analyte d. A judicious selection of kV/mA combinations, analysing crystals, primary beam filters, collimators, peak positions, accurate background correction and peak overlap corrections, followed by the use of appropriate matrix correction procedures. e. Preventative maintenance procedures for XRF spectrometers and ancillary equipment, which can also contribute significantly to reducing instrument down times, are described. Examples of various facets of sample processing routines are given from the XRF spectrometer component of a multi-instrument analytical university facility, which provides XRF data to 17 Canadian universities. Copyright (2002) Australian X-ray Analytical Association Inc

  6. Estimation of trace levels of plutonium in urine samples by fission track technique

    International Nuclear Information System (INIS)

    Sawant, P.D.; Prabhu, S.; Pendharkar, K.A.; Kalsi, P.C.

    2009-01-01

    Individual monitoring of radiation workers handling Pu in various nuclear installations requires the detection of trace levels of plutonium in bioassay samples. It is necessary to develop methods that can detect urinary excretion of Pu in fraction of mBq range. Therefore, a sensitive method such as fission track analysis has been developed for the measurement of trace levels of Pu in bioassay samples. In this technique, chemically separated plutonium from the sample and a Pu standard were electrodeposited on planchettes and covered with Lexan solid state nuclear track detector (SSNTD) and irradiated with thermal neutrons in APSARA reactor of Bhabha Atomic Research Centre, India. The fission track densities in the Lexan films of the sample and the standard were used to calculate the amount of Pu in the sample. The minimum amount of Pu that can be analyzed by this method using doubly distilled electronic grade (E. G.) reagents is about 12 μBq/L. (author)

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

    Science.gov (United States)

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

    2015-12-01

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

  8. Utilization of neutrons in nuclear data measurements and bulk sample analysis

    International Nuclear Information System (INIS)

    Jonah, S. A.

    1995-01-01

    Experimental investigations were carried out with neutrons in the fields of neutron data measurements and bulk sample analysis based on the interactions of neutron interactions required in the investigations together with some salient features of the sources employed are enumerated. Excitation cross section curves and isomeric cross section ratio of 58 Ni(n,p) 58 Co m , g reaction over the neutron energy range of between 5 and 15 MeV were determined using the activation analysis technique in combination with high-resolution gamma spectroscopy. Characteristics of the incident neutrons produced via the D-T reaction of a neutron generator and D-D reaction of a cyclotron were determined experimentally to account for the contributing effects of background neutrons especially in the 5-13 MeV neutron energy range where existing data are scanty and rather discrepant. The measured data agree well with calculated data using nuclear models but deviate significantly from the recommended data based on existing literature data. The measured δ act and δ m /δ g data made it possible to determine the cross section curve for 58 Ni(n,p) 58 Co m reaction. Furthermore the flux density distributions of thermal and primary fast neutrons in different configurations of bulk samples consisting of water, graphite and coal together with the attenuation characteristics were determined by the activation analysis and pulse height response spectrometry techniques. From the results obtained, an experimental geometry has been proposed for on-line elemental analysis of coal and other minerals. Similarly the total hydrogen content and 0+C/H atomic ratio in household and motor oils as well as crude oil samples of different origins were measured by an improved experimental arrangement based on the thermal neutron reflection technique. A detection limit of 0.12 w % was obtained for hydrogen indicating the possible adaptation of this technique for quality control of petroleum products

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

    Science.gov (United States)

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

    2006-10-01

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

  10. Monitoring of persistent organic pollutants in seawater of the Pearl River Estuary with rapid on-site active SPME sampling technique

    International Nuclear Information System (INIS)

    Huang, Siming; He, Shuming; Xu, Hao; Wu, Peiyan; Jiang, Ruifen; Zhu, Fang; Luan, Tiangang; Ouyang, Gangfeng

    2015-01-01

    An on-site active solid-phase microextraction (SPME) sampling technique coupled with gas chromatography-mass spectrometry (GC–MS) for sampling and monitoring 16 polycyclic aromatic hydrocarbons (PAHs) and 8 organochlorine pesticides (OCPs) in seawater was developed. Laboratory experiments demonstrated that the sampling-rate calibration method was practical and could be used for the quantification of on-site sampling. The proposed method was employed for field tests which covered large amounts of water samples in the Pearl River Estuary in rainy and dry seasons. The on-site SPME sampling method can avoid the contamination of sample, the losses of analytes during sample transportation, as well as the usage of solvent and time-consuming sample preparation process. Results indicated that the technique with the designed device can address the requirement of modern environment water analysis. In addition, the sources, bioaccumulation and potential risk to human of the PAHs and OCPs in seawater of the Pearl River Estuary were discussed. - Highlights: • SPME on-site active sampling technique was developed and validated. • The technique was employed for field tests in the Pearl River Estuary. • 16 PAHs and 8 OCPs in the seawater of Pearl River Estuary were monitored. • The potential risk of the PAHs and OCPs in Pearl River Estuary were discussed. - An on-site active SPME sampling technique was developed and successfully applied for sampling and monitoring 16 PAHs and 8 OCPs in the Pearl River Estuary

  11. Decomposition techniques

    Science.gov (United States)

    Chao, T.T.; Sanzolone, R.F.

    1992-01-01

    Sample decomposition is a fundamental and integral step in the procedure of geochemical analysis. It is often the limiting factor to sample throughput, especially with the recent application of the fast and modern multi-element measurement instrumentation. The complexity of geological materials makes it necessary to choose the sample decomposition technique that is compatible with the specific objective of the analysis. When selecting a decomposition technique, consideration should be given to the chemical and mineralogical characteristics of the sample, elements to be determined, precision and accuracy requirements, sample throughput, technical capability of personnel, and time constraints. This paper addresses these concerns and discusses the attributes and limitations of many techniques of sample decomposition along with examples of their application to geochemical analysis. The chemical properties of reagents as to their function as decomposition agents are also reviewed. The section on acid dissolution techniques addresses the various inorganic acids that are used individually or in combination in both open and closed systems. Fluxes used in sample fusion are discussed. The promising microwave-oven technology and the emerging field of automation are also examined. A section on applications highlights the use of decomposition techniques for the determination of Au, platinum group elements (PGEs), Hg, U, hydride-forming elements, rare earth elements (REEs), and multi-elements in geological materials. Partial dissolution techniques used for geochemical exploration which have been treated in detail elsewhere are not discussed here; nor are fire-assaying for noble metals and decomposition techniques for X-ray fluorescence or nuclear methods be discussed. ?? 1992.

  12. Micro and Nano Techniques for the Handling of Biological Samples

    DEFF Research Database (Denmark)

    Micro and Nano Techniques for the Handling of Biological Samples reviews the different techniques available to manipulate and integrate biological materials in a controlled manner, either by sliding them along a surface (2-D manipulation), or by gripping and moving them to a new position (3-D...

  13. MUP, CEC-DES, STRADE. Codes for uncertainty propagation, experimental design and stratified random sampling techniques

    International Nuclear Information System (INIS)

    Amendola, A.; Astolfi, M.; Lisanti, B.

    1983-01-01

    The report describes the how-to-use of the codes: MUP (Monte Carlo Uncertainty Propagation) for uncertainty analysis by Monte Carlo simulation, including correlation analysis, extreme value identification and study of selected ranges of the variable space; CEC-DES (Central Composite Design) for building experimental matrices according to the requirements of Central Composite and Factorial Experimental Designs; and, STRADE (Stratified Random Design) for experimental designs based on the Latin Hypercube Sampling Techniques. Application fields, of the codes are probabilistic risk assessment, experimental design, sensitivity analysis and system identification problems

  14. Analysis of obsydians and films of silicon carbide by RBS technique

    International Nuclear Information System (INIS)

    Franco S, F.

    1998-01-01

    Motivated by archaeological interest this work is presented, which consist in the characterization of obsydian samples from different mineral sites in Mexico and films of silicon carbide, undertaken by an Ion Beam Analysis: RBS (Rutherford Back Scattering). As part of an intensive investigation of obsydian in Mesoamerica by anthropologists from Mexico National Institute of Anthropology and History, 818 samples were collected from different volcanic sources in Central Mexico for the purpose of establishing a data bank of element concentrations of each source. Part of this collection was analyzed by Neutron activation analysis and most of the important elements concentrations reported. In the first part of this work, the non-destructive IBA technique, RBS are used to analyze obsydian samples. The last part is an analysis of thin films of silicon carbide as a part of a research program of the Universidad Nacional Autonoma de Mexico and ININ. The application of this technique were carried out at the IF-UNAM, and the analysis was performed at laboratories of the ININ Nuclear Centre facilities. The samples considered in this work were mounted on a sample holder designed for the purpose of exposing each sample to the alpha particles beam. This RBS analysis was carried out with an ET Tandem accelerator at the IF UNAM. The spectrometry was carried out with employing a Si(Li) detector set at 15 degrees in relation to the target normal. The mean projectile energy was 2.00 MeV, and the beam profile was about 4 mm in diameter. As results were founded elemental concentrations of a set of samples from ten different sources: Altotonga (Veracruz), Penjamo (Guanajuato), Otumba (Mexico), Zinapecuaro (MIchoacan), Ucareo (Michoacan), Tres Cabezas (Puebla), Sierra Navajas (Hidalgo), Zaragoza (Puebla), Guadalupe Victoria (Puebla) and Oyameles (Puebla). The mean values are accompanied by errors expressed as one standard devistion of the mean for each element

  15. Methodological integrative review of the work sampling technique used in nursing workload research.

    Science.gov (United States)

    Blay, Nicole; Duffield, Christine M; Gallagher, Robyn; Roche, Michael

    2014-11-01

    To critically review the work sampling technique used in nursing workload research. Work sampling is a technique frequently used by researchers and managers to explore and measure nursing activities. However, work sampling methods used are diverse making comparisons of results between studies difficult. Methodological integrative review. Four electronic databases were systematically searched for peer-reviewed articles published between 2002-2012. Manual scanning of reference lists and Rich Site Summary feeds from contemporary nursing journals were other sources of data. Articles published in the English language between 2002-2012 reporting on research which used work sampling to examine nursing workload. Eighteen articles were reviewed. The review identified that the work sampling technique lacks a standardized approach, which may have an impact on the sharing or comparison of results. Specific areas needing a shared understanding included the training of observers and subjects who self-report, standardization of the techniques used to assess observer inter-rater reliability, sampling methods and reporting of outcomes. Work sampling is a technique that can be used to explore the many facets of nursing work. Standardized reporting measures would enable greater comparison between studies and contribute to knowledge more effectively. Author suggestions for the reporting of results may act as guidelines for researchers considering work sampling as a research method. © 2014 John Wiley & Sons Ltd.

  16. Selective parathyroid venous sampling in primary hyperparathyroidism: A systematic review and meta-analysis.

    Science.gov (United States)

    Ibraheem, Kareem; Toraih, Eman A; Haddad, Antoine B; Farag, Mahmoud; Randolph, Gregory W; Kandil, Emad

    2018-05-14

    Minimally invasive parathyroidectomy requires accurate preoperative localization techniques. There is considerable controversy about the effectiveness of selective parathyroid venous sampling (sPVS) in primary hyperparathyroidism (PHPT) patients. The aim of this meta-analysis is to examine the diagnostic accuracy of sPVS as a preoperative localization modality in PHPT. Studies evaluating the diagnostic accuracy of sPVS for PHPT were electronically searched in the PubMed, EMBASE, Web of Science, and Cochrane Controlled Trials Register databases. Two independent authors reviewed the studies, and revised quality assessment of diagnostic accuracy study tool was used for the quality assessment. Study heterogeneity and pooled estimates were calculated. Two hundred and two unique studies were identified. Of those, 12 studies were included in the meta-analysis. Pooled sensitivity, specificity, and positive likelihood ratio (PLR) of sPVS were 74%, 41%, and 1.55, respectively. The area-under-the-receiver operating characteristic curve was 0.684, indicating an average discriminatory ability of sPVS. On comparison between sPVS and noninvasive imaging modalities, sensitivity, PLR, and positive posttest probability were significantly higher in sPVS compared to noninvasive imaging modalities. Interestingly, super-selective venous sampling had the highest sensitivity, accuracy, and positive posttest probability compared to other parathyroid venous sampling techniques. This is the first meta-analysis to examine the accuracy of sPVS in PHPT. sPVS had higher pooled sensitivity when compared to noninvasive modalities in revision parathyroid surgery. However, the invasiveness of this technique does not favor its routine use for preoperative localization. Super-selective venous sampling was the most accurate among all other parathyroid venous sampling techniques. Laryngoscope, 2018. © 2018 The American Laryngological, Rhinological and Otological Society, Inc.

  17. Analysis of submicrogram samples by INAA

    Energy Technology Data Exchange (ETDEWEB)

    Lindstrom, D J [National Aeronautics and Space Administration, Houston, TX (USA). Lyndon B. Johnson Space Center

    1990-12-20

    Procedure have been developed to increase the sensitivity of instrumental neutron activation analysis (INAA) so that cosmic-dust samples weighing only 10{sup -9}-10{sup -7} g are routinely analyzed for a sizable number of elements. The primary differences from standard techniques are: (1) irradiation of the samples is much more intense, (2) gamma ray assay of the samples is done using long counting times and large Ge detectors that are operated in an excellent low-background facility, (3) specially prepared glass standards are used, (4) samples are too small to be weighed routinely and concentrations must be obtained indirectly, (5) sample handling is much more difficult, and contamination of small samples with normally insignificant amounts of contaminants is difficult to prevent. In spite of the difficulties, INAA analyses have been done on 15 cosmic-dust particles and a large number of other stratospheric particles. Two-sigma detection limits for some elements are in the range of femtograms (10{sup -15} g), e.g. Co=11, Sc=0.9, Sm=0.2 A particle weighing just 0.2 ng was analyzed, obtaining abundances with relative analytical uncertainties of less than 10% for four elements (Fe, Co, Ni and Sc), which were sufficient to allow identification of the particle as chondritic interplanetary dust. Larger samples allow abundances of twenty or more elements to be obtained. (orig.).

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

    Science.gov (United States)

    Filippou, Olga; Bitas, Dimitrios; Samanidou, Victoria

    2017-02-01

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

  19. Recent Improvements at CEA on Trace Analysis of Actinides in Environmental Samples

    International Nuclear Information System (INIS)

    Pointurier, F.; Hubert, A.; Faure, A.L.; Pottin, A.C.; Mourier, W.; Marie, O.

    2010-01-01

    In this paper, we present some results of R and D works conducted at CEA to improve on the one side the performance of the techniques already in use for detection of undeclared activities, and on the other side to develop new capabilities, either as alternative to the existing techniques or new methods that bring new information, complementary to the isotopic composition. For the trace analysis of plutonium in swipe samples by ICP-MS, we demonstrate that a thorough knowledge of the background in the actinide mass range is highly desirable. In order to avoid false plutonium detection in the femtogram range, correction from polyatomic interferences including mercury, lead or iridium atoms are in some case necessary. Efforts must be put on improving the purification procedure. Micro-Raman spectrometry allows determining the chemical composition of uranium compound at the scale of the microscopic object using a pre-location of the particles thanks to SEM and a relocation of these particles thanks to mathematical calculations. However, particles below 5 μm are hardly relocated and a coupling device between the SEM and the micro-Raman spectrometer for direct Raman analysis after location of a particle of interest is currently under testing. Lastly, laser ablation - ICP-MS is an interesting technique for direct isotopic or elemental analysis of various solid samples and proves to be a suitable alternative technique for particle analysis, although precision over isotopic ratio measurement is strongly limited by the short duration and irregularity of the signals. However, sensitivity and sample throughput are high and more developments are in progress to validate and improve this method. (author)

  20. Analysis of metal samples

    International Nuclear Information System (INIS)

    Ramirez T, J.J.; Lopez M, J.; Sandoval J, A.R.; Villasenor S, P.; Aspiazu F, J.A.

    2001-01-01

    An elemental analysis, metallographic and of phases was realized in order to determine the oxidation states of Fe contained in three metallic pieces: block, plate and cylinder of unknown material. Results are presented from the elemental analysis which was carried out in the Tandem Accelerator of ININ by Proton induced X-ray emission (PIXE). The phase analysis was carried out by X-ray diffraction which allowed to know the type of alloy or alloys formed. The combined application of nuclear techniques with metallographic techniques allows the integral characterization of industrial metals. (Author)

  1. RF Sub-sampling Receiver Architecture based on Milieu Adapting Techniques

    DEFF Research Database (Denmark)

    Behjou, Nastaran; Larsen, Torben; Jensen, Ole Kiel

    2012-01-01

    A novel sub-sampling based architecture is proposed which has the ability of reducing the problem of image distortion and improving the signal to noise ratio significantly. The technique is based on sensing the environment and adapting the sampling rate of the receiver to the best possible...

  2. Determination of metals in air samples using X-Ray fluorescence associated the APDC preconcentration technique

    Energy Technology Data Exchange (ETDEWEB)

    Nardes, Raysa C.; Santos, Ramon S.; Sanches, Francis A.C.R.A.; Gama Filho, Hamilton S.; Oliveira, Davi F.; Anjos, Marcelino J., E-mail: rc.nardes@gmail.com, E-mail: ramonziosp@yahoo.com.br, E-mail: francissanches@gmail.com, E-mail: hamiltongamafilho@hotmail.com, E-mail: davi.oliveira@uerj.br, E-mail: marcelin@uerj.br [Universidade do Estado do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil). Instituto de Fisica. Departamento de Fisica Aplicada e Termodinamica

    2015-07-01

    Air pollution has become one of the leading quality degradation factors of life for people in large urban centers. Studies indicate that the suspended particulate matter in the atmosphere is directly associated with risks to public health, in addition, it can cause damage to fauna, flora and public / cultural patrimonies. The inhalable particulate materials can cause the emergence and / or worsening of chronic diseases related to respiratory system and other diseases, such as reduced physical strength. In this study, we propose a new method to measure the concentration of total suspended particulate matter (TSP) in the air using an impinger as an air cleaning apparatus, preconcentration with APDC and Total Reflection X-ray Fluorescence technique (TXRF) to analyze the heavy metals present in the air. The samples were collected from five random points in the city of Rio de Janeiro/Brazil. Analyses of TXRF were performed at the Brazilian Synchrotron Light Laboratory (LNLS). The technique proved viable because it was able to detect five important metallic elements to environmental studies: Cr, Fe, Ni, Cu and Zn. This technique presented substantial efficiency in determining the elementary concentration of air pollutants, in addition to low cost. It can be concluded that the metals analysis technique in air samples using an impinger as sample collection instrument associated with a complexing agent (APDC) was viable because it is a low-cost technique, moreover, it was possible the detection of five important metal elements in environmental studies associated with industrial emissions and urban traffic. (author)

  3. Determination of metals in air samples using X-Ray fluorescence associated the APDC preconcentration technique

    International Nuclear Information System (INIS)

    Nardes, Raysa C.; Santos, Ramon S.; Sanches, Francis A.C.R.A.; Gama Filho, Hamilton S.; Oliveira, Davi F.; Anjos, Marcelino J.

    2015-01-01

    Air pollution has become one of the leading quality degradation factors of life for people in large urban centers. Studies indicate that the suspended particulate matter in the atmosphere is directly associated with risks to public health, in addition, it can cause damage to fauna, flora and public / cultural patrimonies. The inhalable particulate materials can cause the emergence and / or worsening of chronic diseases related to respiratory system and other diseases, such as reduced physical strength. In this study, we propose a new method to measure the concentration of total suspended particulate matter (TSP) in the air using an impinger as an air cleaning apparatus, preconcentration with APDC and Total Reflection X-ray Fluorescence technique (TXRF) to analyze the heavy metals present in the air. The samples were collected from five random points in the city of Rio de Janeiro/Brazil. Analyses of TXRF were performed at the Brazilian Synchrotron Light Laboratory (LNLS). The technique proved viable because it was able to detect five important metallic elements to environmental studies: Cr, Fe, Ni, Cu and Zn. This technique presented substantial efficiency in determining the elementary concentration of air pollutants, in addition to low cost. It can be concluded that the metals analysis technique in air samples using an impinger as sample collection instrument associated with a complexing agent (APDC) was viable because it is a low-cost technique, moreover, it was possible the detection of five important metal elements in environmental studies associated with industrial emissions and urban traffic. (author)

  4. Improved importance sampling technique for efficient simulation of digital communication systems

    Science.gov (United States)

    Lu, Dingqing; Yao, Kung

    1988-01-01

    A new, improved importance sampling (IIS) approach to simulation is considered. Some basic concepts of IS are introduced, and detailed evolutions of simulation estimation variances for Monte Carlo (MC) and IS simulations are given. The general results obtained from these evolutions are applied to the specific previously known conventional importance sampling (CIS) technique and the new IIS technique. The derivation for a linear system with no signal random memory is considered in some detail. For the CIS technique, the optimum input scaling parameter is found, while for the IIS technique, the optimum translation parameter is found. The results are generalized to a linear system with memory and signals. Specific numerical and simulation results are given which show the advantages of CIS over MC and IIS over CIS for simulations of digital communications systems.

  5. Cone penetrometer tests and HydroPunch sampling: A screening technique for plume definition

    International Nuclear Information System (INIS)

    Smolley, M.; Kappmeyer, J.C.

    1991-01-01

    Cone penetrometer tests and HydroPunch sampling were used to define the extent of volatile organic compounds in ground water. The investigation indicated that the combination of the these techniques is effective for obtaining ground water samples for preliminary plume definition. HydroPunch samples can be collected in unconsolidated sediments and the analytical results obtained from these samples are comparable to those obtained from adjacent monitoring wells. This sampling method is a rapid and cost-effective screening technique for characterizing the extent of contaminant plumes in soft sediment environments. Use of this screening technique allowed monitoring wells to be located at the plume boundary, thereby reducing the number of wells installed and the overall cost of the plume definition program

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  7. A Comparative Analysis of Uranium Ore using Laser Fluorimetric and gamma Spectrometry Techniques

    International Nuclear Information System (INIS)

    Madbouly, M.; Nassef, M. H.; El-Mongy, S.A.; Diab, A.M.

    2009-01-01

    A developed chemical separation method was used for the analysis of uranium in a standard U-ore (IAEA-RGU-1) by LASER fluorimetric technique. The non-destructive gamma assay technique was also applied to verify and compare the uranium content analyzed using laser technique. The results of the uranium analysis obtained by laser fluorimetry were found to be in the range of 360 - 420 μg/g with an average value of 390 μg/g. The bias between the measured and the certified value does not exceed 9.9%. For gamma-ray spectrometric analysis, the results of the measured uranium content were found to be in the range of 393.8 - 399.4 μg/g with an average value of 396.3 μg/g. The % difference in the case of γ- assay was 1.6 %. In general, the methods of analysis used in this study are applicable for a precise determination of uranium. It can be concluded that, laser analysis is preferred for assay of uranium ore due to the required small sample weight, the low time of sample preparation and cost of analysis.

  8. Chance constrained problems: penalty reformulation and performance of sample approximation technique

    Czech Academy of Sciences Publication Activity Database

    Branda, Martin

    2012-01-01

    Roč. 48, č. 1 (2012), s. 105-122 ISSN 0023-5954 R&D Projects: GA ČR(CZ) GBP402/12/G097 Institutional research plan: CEZ:AV0Z10750506 Keywords : chance constrained problems * penalty functions * asymptotic equivalence * sample approximation technique * investment problem Subject RIV: BB - Applied Statistics, Operational Research Impact factor: 0.619, year: 2012 http://library.utia.cas.cz/separaty/2012/E/branda-chance constrained problems penalty reformulation and performance of sample approximation technique.pdf

  9. Use of X-ray diffraction technique and chemometrics to aid soil sampling strategies in traceability studies.

    Science.gov (United States)

    Bertacchini, Lucia; Durante, Caterina; Marchetti, Andrea; Sighinolfi, Simona; Silvestri, Michele; Cocchi, Marina

    2012-08-30

    Aim of this work is to assess the potentialities of the X-ray powder diffraction technique as fingerprinting technique, i.e. as a preliminary tool to assess soil samples variability, in terms of geochemical features, in the context of food geographical traceability. A correct approach to sampling procedure is always a critical issue in scientific investigation. In particular, in food geographical traceability studies, where the cause-effect relations between the soil of origin and the final foodstuff is sought, a representative sampling of the territory under investigation is certainly an imperative. This research concerns a pilot study to investigate the field homogeneity with respect to both field extension and sampling depth, taking also into account the seasonal variability. Four Lambrusco production sites of the Modena district were considered. The X-Ray diffraction spectra, collected on the powder of each soil sample, were treated as fingerprint profiles to be deciphered by multivariate and multi-way data analysis, namely PCA and PARAFAC. The differentiation pattern observed in soil samples, as obtained by this fast and non-destructive analytical approach, well matches with the results obtained by characterization with other costly analytical techniques, such as ICP/MS, GFAAS, FAAS, etc. Thus, the proposed approach furnishes a rational basis to reduce the number of soil samples to be collected for further analytical characterization, i.e. metals content, isotopic ratio of radiogenic element, etc., while maintaining an exhaustive description of the investigated production areas. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Sampling methods and non-destructive examination techniques for large radioactive waste packages

    International Nuclear Information System (INIS)

    Green, T.H.; Smith, D.L.; Burgoyne, K.E.; Maxwell, D.J.; Norris, G.H.; Billington, D.M.; Pipe, R.G.; Smith, J.E.; Inman, C.M.

    1992-01-01

    Progress is reported on work undertaken to evaluate quality checking methods for radioactive wastes. A sampling rig was designed, fabricated and used to develop techniques for the destructive sampling of cemented simulant waste using remotely operated equipment. An engineered system for the containment of cooling water was designed and manufactured and successfully demonstrated with the drum and coring equipment mounted in both vertical and horizontal orientations. The preferred in-cell orientation was found to be with the drum and coring machinery mounted in a horizontal position. Small powdered samples can be taken from cemented homogeneous waste cores using a hollow drill/vacuum section technique with the preferred subsampling technique being to discard the outer 10 mm layer to obtain a representative sample of the cement core. Cement blends can be dissolved using fusion techniques and the resulting solutions are stable to gelling for periods in excess of one year. Although hydrochloric acid and nitric acid are promising solvents for dissolution of cement blends, the resultant solutions tend to form silicic acid gels. An estimate of the beta-emitter content of cemented waste packages can be obtained by a combination of non-destructive and destructive techniques. The errors will probably be in excess of +/-60 % at the 95 % confidence level. Real-time X-ray video-imaging techniques have been used to analyse drums of uncompressed, hand-compressed, in-drum compacted and high-force compacted (i.e. supercompacted) simulant waste. The results have confirmed the applicability of this technique for NDT of low-level waste. 8 refs., 12 figs., 3 tabs

  11. Quantitative chemical analysis of lead in canned chillis by spectrophotometric and nuclear techniques

    International Nuclear Information System (INIS)

    Sanchez Paz, L.A.

    1991-01-01

    The objectives of this work are the quantification of lead contents in two types of canned chilli of three trademarks, determining its inside of maximum permissible level (2 ppm), comparing moreover two trademarks that have flask and canned presentation for to determine the filling effect in the final content of lead, moreover make a comparative study of the techniques using on base to exactitude, linearity and sensibility. The techniques used were atomic absorption spectrophotometry, plasma emission spectrometry and x-ray fluorescence. The preliminary treatment of the samples was by calcination, continued of the ashes dissolution in acid medium, for later gauge a determinate volume for analyze by atomic absorption and plasma emission. For the analysis by x-ray fluorescence, after solubilyzing ashes, its precipitate the lead with PCDA (Pyrrolidine carbodithioic ammonium acid) then its filtered, filter paper is dried and counted directly. The standards preparation is made following the same procedure as in samples using lead titrisol solution. For each technique the recovery percent is determined by the addition of enough know amount. For each technique calibration curves are plotted been determined that the three are lineal in the established range of work. The recovery percent in three cases is superior to ninety five percent. By means of a variance analysis it was determined that lead contain in samples do not exceed two ppm., and the lead content in canned chillis is superior to contained in glass containers (1.7, 0.4 ppm respectively). X-ray fluorescence analysis is different to the attained results by the other two techniques due to its sensibility is less. The most advisable techniques for this kind of analysis are atomic absorption spectrophotometry and plasma emission. (Author)

  12. Practical applications of activation analysis and other nuclear techniques

    International Nuclear Information System (INIS)

    Lyon, W.S.

    1982-01-01

    Neeutron activation analysis (NAA) is a versatile, sensitive multielement, usually nondestructive analytical technique used to determine elemental concentrations in a variety of materials. Samples are irradiated with neutrons in a nuclear reactor, removed, and for the nondestructive technique, the induced radioactivity measured. This measurement of γ rays emitted from specific radionuclides makes possible the quantitative determination of elements present. The method is described, advantages and disadvantages listed and a number of examples of its use given. Two other nuclear methods, particle induced x-ray emission and synchrotron produced x-ray fluorescence are also briefly discussed

  13. LC-MS analysis of the plasma metabolome–a novel sample preparation strategy

    DEFF Research Database (Denmark)

    Skov, Kasper; Hadrup, Niels; Smedsgaard, Jørn

    2015-01-01

    Blood plasma is a well-known body fluid often analyzed in studies on the effects of toxic compounds as physiological or chemical induced changes in the mammalian body are reflected in the plasma metabolome. Sample preparation prior to LC-MS based analysis of the plasma metabolome is a challenge...... as plasma contains compounds with very different properties. Besides, proteins, which usually are precipitated with organic solvent, phospholipids, are known to cause ion suppression in electrospray mass spectrometry. We have compared two different sample preparation techniques prior to LC-qTOF analysis...... of plasma samples: The first is protein precipitation; the second is protein precipitation followed by solid phase extraction with sub-fractionation into three sub-samples; a phospholipid, a lipid and a polar sub-fraction. Molecular feature extraction of the data files from LC-qTOF analysis of the samples...

  14. Combined neutron activation analysis techniques for multiple purposes at Portuguese research reactor

    International Nuclear Information System (INIS)

    Dung, H.M.; Freitas, M.C.; Beasley, D.; Almeida, S.M.; Dionisio, I; Canha, N.H.; Galinha, C.; Marques, J.G.

    2010-01-01

    Full text: Developments of the neutron activation analysis (NAA) techniques using Compton suppression system (CSS), fast pneumatic irradiation facility (SIPRA), epithermal neutron and automatic sample changers (ASCs) associated with the traditional NAA for trace element determination in various sample types are described with reference to specific conditions at the 1 MW Portuguese research reactor (RPI). Experiences in application of k o -IAEA software for data processing in order to deduce the results are also discussed. A selected number of sample types which are intended to the application in biological and environmental areas as well as industrial and material samples are demonstrated which provide challenges in the irradiation, measurement and the interpretation of data to which in most cases a combined solution should be made. The role that each NAA technique can play in the combined scheme along with their optimized characteristics has been studied and shown. The combined NAA techniques at RPI established for on-going and potential projects as well as analysis service with respect to the element scope (48), typically Ag, Al, As, Au, Ba, Br, Ca, Cd, Ce, CI, Co, Cr, Cs, Cu, Dy, Er, Eu, F, Fe, Ga, Hf, Hg, I, In, K, La, Mg, Mn, Mo, Na, Rb, Sb, Sc, Se, Si, Sm, Sn, Sr, Ta, Tb, Th, Ti, U, V, W, Vb, Zn and Zr along with detection limits, accuracies and precision's have been evaluated as a trace analysis method meeting the requirements of the intended applications

  15. Experiences in the ICP-MS analysis of geological and environmental samples

    International Nuclear Information System (INIS)

    Kallio, E.

    1994-01-01

    Inductively coupled plasma mass spectrometry (ICP-MS) has been used at the Geological Survey of Finland since 1991. Applied to determination of trace and ultra trace elements in water, sediments, biological samples and rocks. The strength of the technique lies in the ability to determine isotope ratios, and elements that are difficult or expensive to determine by other techniques, e.g. platinum group elements (PGEs), rare earths elements (REEs) and toxic metals (As, Be, Cd, Hg, Pb, Tl, U). An important part of the analysis is the pretreatment of the samples before the measurement. This paper gives an overview of the methods used at the Geological Survey. (orig.). (5 refs.)

  16. A Comparison of Soil-Water Sampling Techniques

    Science.gov (United States)

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

    2007-12-01

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

  17. Use of alpha spectrometry for analysis of U-isotopes in some granite samples

    International Nuclear Information System (INIS)

    El-Galy, M.M.; Desouky, O.A.; Khattab, M.R.; Issa, F.A.

    2011-01-01

    The present study aims to use the α-spectrometry, at NMA. A radiochemical technique for analysis of U-isotopes was carried out for some granite samples from Gabal Gattar and El Missikat localities and also for some reference soil samples of IAEA. Several steps of sample preparation, radiochemical separation, and source preparation were performed before analysis. The concerned sample was leached by HNO 3 , HF and H 2 O 2 acids after ashing. The ashed sample was spiked with uranium tracer ( 232 U) for chemical yield and activity calculation. Then uranium was extracted from the matrix elements with trioctylphosphine oxide (TOPO) and stripped with 1 M NH 4 F/0.1 M HCl solution. The uranium fraction was purified by co-precipitation with LaF 3 to ensure complete removal of thorium and traces of resolution degrading elements. This was followed by a final clean-up step using an anion exchange. The pure uranium fraction was electrodeposited on a stainless steel disc from HCl/oxalate solution. The obtained results from the soil reference samples indicate general similarities between the techniques of α-spectrometers of NMA, EAEA and IAEA for analysis of U-isotopes. The U-isotopes in the granite samples of high radioactivity levels need more attempts after dilution process to be in the limit detection of α-spectrometry. (author)

  18. Can groundwater sampling techniques used in monitoring wells influence methane concentrations and isotopes?

    Science.gov (United States)

    Rivard, Christine; Bordeleau, Geneviève; Lavoie, Denis; Lefebvre, René; Malet, Xavier

    2018-03-06

    Methane concentrations and isotopic composition in groundwater are the focus of a growing number of studies. However, concerns are often expressed regarding the integrity of samples, as methane is very volatile and may partially exsolve during sample lifting in the well and transfer to sampling containers. While issues concerning bottle-filling techniques have already been documented, this paper documents a comparison of methane concentration and isotopic composition obtained with three devices commonly used to retrieve water samples from dedicated observation wells. This work lies within the framework of a larger project carried out in the Saint-Édouard area (southern Québec, Canada), whose objective was to assess the risk to shallow groundwater quality related to potential shale gas exploitation. The selected sampling devices, which were tested on ten wells during three sampling campaigns, consist of an impeller pump, a bladder pump, and disposable sampling bags (HydraSleeve). The sampling bags were used both before and after pumping, to verify the appropriateness of a no-purge approach, compared to the low-flow approach involving pumping until stabilization of field physicochemical parameters. Results show that methane concentrations obtained with the selected sampling techniques are usually similar and that there is no systematic bias related to a specific technique. Nonetheless, concentrations can sometimes vary quite significantly (up to 3.5 times) for a given well and sampling event. Methane isotopic composition obtained with all sampling techniques is very similar, except in some cases where sampling bags were used before pumping (no-purge approach), in wells where multiple groundwater sources enter the borehole.

  19. Investigation of CPD and HMDS Sample Preparation Techniques for Cervical Cells in Developing Computer-Aided Screening System Based on FE-SEM/EDX

    Science.gov (United States)

    Ng, Siew Cheok; Abu Osman, Noor Azuan

    2014-01-01

    This paper investigated the effects of critical-point drying (CPD) and hexamethyldisilazane (HMDS) sample preparation techniques for cervical cells on field emission scanning electron microscopy and energy dispersive X-ray (FE-SEM/EDX). We investigated the visualization of cervical cell image and elemental distribution on the cervical cell for two techniques of sample preparation. Using FE-SEM/EDX, the cervical cell images are captured and the cell element compositions are extracted for both sample preparation techniques. Cervical cell image quality, elemental composition, and processing time are considered for comparison of performances. Qualitatively, FE-SEM image based on HMDS preparation technique has better image quality than CPD technique in terms of degree of spread cell on the specimen and morphologic signs of cell deteriorations (i.e., existence of plate and pellet drying artifacts and membrane blebs). Quantitatively, with mapping and line scanning EDX analysis, carbon and oxygen element compositions in HMDS technique were higher than the CPD technique in terms of weight percentages. The HMDS technique has shorter processing time than the CPD technique. The results indicate that FE-SEM imaging, elemental composition, and processing time for sample preparation with the HMDS technique were better than CPD technique for cervical cell preparation technique for developing computer-aided screening system. PMID:25610902

  20. Single-particle characterization of ice-nucleating particles and ice particles residuals sampled by three different techniques

    Science.gov (United States)

    Kandler, Konrad; Worringen, Annette; Benker, Nathalie; Dirsch, Thomas; Mertes, Stephan; Schenk, Ludwig; Kästner, Udo; Frank, Fabian; Nillius, Björn; Bundke, Ulrich; Rose, Diana; Curtius, Joachim; Kupiszewski, Piotr; Weingartner, Ernest; Vochezer, Paul; Schneider, Johannes; Schmidt, Susan; Weinbruch, Stephan; Ebert, Martin

    2015-04-01

    During January/February 2013, at the High Alpine Research Station Jungfraujoch a measurement campaign was carried out, which was centered on atmospheric ice-nucleating particles (INP) and ice particle residuals (IPR). Three different techniques for separation of INP and IPR from the non-ice-active particles are compared. The Ice Selective Inlet (ISI) and the Ice Counterflow Virtual Impactor (Ice-CVI) sample ice particles from mixed phase clouds and allow for the analysis of the residuals. The combination of the Fast Ice Nucleus Chamber (FINCH) and the Ice Nuclei Pumped Counterflow Virtual Impactor (IN-PCVI) provides ice-activating conditions to aerosol particles and extracts the activated INP for analysis. Collected particles were analyzed by scanning electron microscopy and energy-dispersive X-ray microanalysis to determine size, chemical composition and mixing state. All INP/IPR-separating techniques had considerable abundances (median 20 - 70 %) of instrumental contamination artifacts (ISI: Si-O spheres, probably calibration aerosol; Ice-CVI: Al-O particles; FINCH+IN-PCVI: steel particles). Also, potential sampling artifacts (e.g., pure soluble material) occurred with a median abundance of separated by all three techniques. Soot was a minor contributor. Lead was detected in less than 10 % of the particles, of which the majority were internal mixtures with other particle types. Sea-salt and sulfates were identified by all three methods as INP/IPR. Most samples showed a maximum of the INP/IPR size distribution at 400 nm geometric diameter. In a few cases, a second super-micron maximum was identified. Soot/carbonaceous material and metal oxides were present mainly in the submicron range. ISI and FINCH yielded silicates and Ca-rich particles mainly with diameters above 1 µm, while the Ice-CVI also separated many submicron IPR. As strictly parallel sampling could not be performed, a part of the discrepancies between the different techniques may result from

  1. XRF and TXRF techniques for multi-element determination of trace elements in whole blood and human hair samples

    International Nuclear Information System (INIS)

    Khuder, A.; Karjou, J.; Sawan, M.Kh.; Bakir, M.A.

    2007-01-01

    XRF and TXRF were established as useful techniques for multi-element analysis of whole blood and human head hair samples. Direct-XRF with different collimation units and different X-ray excitation modes was successfully used for the determination of S, P, K, Ca, Fe, and Br elements in blood samples and K, Ca, Mn, Fe elements in human hair samples. Direct analysis by TXRF was used for the determination of Rb and Sr in digested blood and human hair samples, respectively, while, the co-precipitation method using APDC for TXRF analysis was used for the determination of Ni, Cu, Zn, and Pb elements in both matrices. As a result, the improved XRF and TXRF methods were applied for multi-element determination of elements in whole blood and human hair samples in non-occupational exposed population living in Damascus city. The mean concentrations of analyzed elements in both matrices were on the reported range values for non-occupational population in other countries. (author)

  2. XRF and TXRF techniques for multi-element determination of trace elements in whole blood and human hair samples

    International Nuclear Information System (INIS)

    Khuder, A.; Karjou, J.; Sawan, M.Kh.; Bakir, M.A.

    2008-01-01

    XRF and TXRF were established as useful techniques for multi-element analysis of whole blood and human head hair samples. Direct-XRF with different collimation units and different X-ray excitation modes was successfully used for the determination of S, P, K, Ca, Fe, and Br elements in blood samples and K, Ca, Mn, Fe elements in human hair samples. Direct analysis by TXRF was used for the determination of Rb and Sr in digested blood and human hair samples, respectively, while, the co-precipitation method using APDC for TXRF analysis was used for the determination of Ni, Cu, Zn, and Pb elements in both matrices. As a result, the improved XRF and TXRF methods were applied for multi-element determination of elements in whole blood and human hair samples in non-occupational exposed population living in Damascus city. The mean concentrations of analyzed elements in both matrices were on the reported range values for non-occupational population in other countries. (author)

  3. Performance evaluation of an importance sampling technique in a Jackson network

    Science.gov (United States)

    brahim Mahdipour, E.; Masoud Rahmani, Amir; Setayeshi, Saeed

    2014-03-01

    Importance sampling is a technique that is commonly used to speed up Monte Carlo simulation of rare events. However, little is known regarding the design of efficient importance sampling algorithms in the context of queueing networks. The standard approach, which simulates the system using an a priori fixed change of measure suggested by large deviation analysis, has been shown to fail in even the simplest network settings. Estimating probabilities associated with rare events has been a topic of great importance in queueing theory, and in applied probability at large. In this article, we analyse the performance of an importance sampling estimator for a rare event probability in a Jackson network. This article carries out strict deadlines to a two-node Jackson network with feedback whose arrival and service rates are modulated by an exogenous finite state Markov process. We have estimated the probability of network blocking for various sets of parameters, and also the probability of missing the deadline of customers for different loads and deadlines. We have finally shown that the probability of total population overflow may be affected by various deadline values, service rates and arrival rates.

  4. Small area analysis using micro-diffraction techniques

    International Nuclear Information System (INIS)

    Goehner, Raymond P.; Tissot, Ralph G. Jr.; Michael, Joseph R.

    2000-01-01

    An overall trend toward smaller electronic packages and devices makes it increasingly important and difficult to obtain meaningful diffraction information from small areas. X-ray micro-diffraction, electron back-scattered diffraction (EBSD) and Kossel are micro-diffraction techniques used for crystallographic analysis including texture, phase identification and strain measurements. X-ray micro-diffraction primarily is used for phase analysis and residual strain measurements. X-ray micro-diffraction primarily is used for phase analysis and residual strain measurements of areas between 10 microm to 100 microm. For areas this small glass capillary optics are used for producing a usable collimated x-ray beam. These optics are designed to reflect x-rays below the critical angle therefore allowing for larger solid acceptance angle at the x-ray source resulting in brighter smaller x-ray beams. The determination of residual strain using micro-diffraction techniques is very important to the semiconductor industry. Residual stresses have caused voiding of the interconnect metal which then destroys electrical continuity. Being able to determine the residual stress helps industry to predict failures from the aging effects of interconnects due to this stress voiding. Stress measurements would be impossible using a conventional x-ray diffractometer; however, utilizing a 30 microm glass capillary these small areas are readily assessable for analysis. Kossel produces a wide angle diffraction pattern from fluorescent x-rays generated in the sample by an e-beam in a SEM. This technique can yield very precise lattice parameters for determining strain. Fig. 2 shows a Kossel pattern from a Ni specimen. Phase analysis on small areas is also possible using an energy dispersive spectrometer (EBSD) and x-ray micro-diffraction techniques. EBSD has the advantage of allowing the user to observe the area of interest using the excellent imaging capabilities of the SEM. An EDS detector has been

  5. Nanoliter hemolymph sampling and analysis of individual adult Drosophila melanogaster.

    Science.gov (United States)

    Piyankarage, Sujeewa C; Featherstone, David E; Shippy, Scott A

    2012-05-15

    The fruit fly (Drosophila melanogaster) is an extensively used and powerful, genetic model organism. However, chemical studies using individual flies have been limited by the animal's small size. Introduced here is a method to sample nanoliter hemolymph volumes from individual adult fruit-flies for chemical analysis. The technique results in an ability to distinguish hemolymph chemical variations with developmental stage, fly sex, and sampling conditions. Also presented is the means for two-point monitoring of hemolymph composition for individual flies.

  6. Single-particle characterization of ice-nucleating particles and ice particle residuals sampled by three different techniques

    Science.gov (United States)

    Worringen, A.; Kandler, K.; Benker, N.; Dirsch, T.; Mertes, S.; Schenk, L.; Kästner, U.; Frank, F.; Nillius, B.; Bundke, U.; Rose, D.; Curtius, J.; Kupiszewski, P.; Weingartner, E.; Vochezer, P.; Schneider, J.; Schmidt, S.; Weinbruch, S.; Ebert, M.

    2015-04-01

    In the present work, three different techniques to separate ice-nucleating particles (INPs) as well as ice particle residuals (IPRs) from non-ice-active particles are compared. The Ice Selective Inlet (ISI) and the Ice Counterflow Virtual Impactor (Ice-CVI) sample ice particles from mixed-phase clouds and allow after evaporation in the instrument for the analysis of the residuals. The Fast Ice Nucleus Chamber (FINCH) coupled with the Ice Nuclei Pumped Counterflow Virtual Impactor (IN-PCVI) provides ice-activating conditions to aerosol particles and extracts the activated particles for analysis. The instruments were run during a joint field campaign which took place in January and February 2013 at the High Alpine Research Station Jungfraujoch (Switzerland). INPs and IPRs were analyzed offline by scanning electron microscopy and energy-dispersive X-ray microanalysis to determine their size, chemical composition and mixing state. Online analysis of the size and chemical composition of INP activated in FINCH was performed by laser ablation mass spectrometry. With all three INP/IPR separation techniques high abundances (median 20-70%) of instrumental contamination artifacts were observed (ISI: Si-O spheres, probably calibration aerosol; Ice-CVI: Al-O particles; FINCH + IN-PCVI: steel particles). After removal of the instrumental contamination particles, silicates, Ca-rich particles, carbonaceous material and metal oxides were the major INP/IPR particle types obtained by all three techniques. In addition, considerable amounts (median abundance mostly a few percent) of soluble material (e.g., sea salt, sulfates) were observed. As these soluble particles are often not expected to act as INP/IPR, we consider them as potential measurement artifacts. Minor types of INP/IPR include soot and Pb-bearing particles. The Pb-bearing particles are mainly present as an internal mixture with other particle types. Most samples showed a maximum of the INP/IPR size distribution at 200

  7. PIXE analysis of thin samples

    International Nuclear Information System (INIS)

    Kiss, Ildiko; Koltay, Ede; Szabo, Gyula; Laszlo, S.; Meszaros, A.

    1985-01-01

    Particle-induced X-ray emission (PIXE) multielemental analysis of thin film samples are reported. Calibration methods of K and L X-lines are discussed. Application of PIXE analysis to aerosol monitoring, multielement aerosol analysis is described. Results of PIXE analysis of samples from two locations in Hungary are compared with the results of aerosol samples from Scandinavia and the USA. (D.Gy.)

  8. Microfabricated Devices for Sample Extraction, Concentrations, and Related Sample Processing Technologies

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Gang; Lin, Yuehe

    2006-12-01

    This is an invited book chapter. As with other analytical techniques, sample pretreatments, sample extraction, sample introduction, and related techniques are of extreme importance for micro-electro-mechanical systems (MEMS). Bio-MEMS devices and systems start with a sampling step. The biological sample then usually undergoes some kinds of sample preparation steps before the actual analysis. These steps may involve extracting the target sample from its matrix, removing interferences from the sample, derivatizing the sample to detectable species, or performing a sample preconcentration step. The integration of the components for sample pretreatment into microfluidic devices represents one of the remaining the bottle-neck towards achieving true miniaturized total analysis systems (?TAS). This chapter provides a thorough state-of-art of the developments in this field to date.

  9. A rapid method of radium-226 analysis in water samples using an alpha spectroscopic technique

    International Nuclear Information System (INIS)

    Lim, T.P.

    1981-01-01

    A fast, reliable and accurate method for radium-226 determination in environmental water samples has been devised, using an alpha spectroscopic technique. The correlation between barium-133 and radium-226 in the barium-radium sulphate precipitation mechanism was studied and in the limited experimental recovery range, the coefficient of correlation was r = 0.986. A self-absorption study for various barium carrier concentrations was also undertaken to obtain the least broadening of alpha energy line widths. An optimum value of 0.3 mg barium carrier was obtained for chemical recovery in the range of 85 percent. (auth)

  10. An introduction to the technique of combined ion mobility spectrometry-mass spectrometry for the analysis of complex biological samples

    International Nuclear Information System (INIS)

    McDowall, Mark A.; Bateman, Robert H.; Bajic, Steve; Giles, Kevin; Langridge, Jim; McKenna, Therese; Pringle, Steven D.; Wildgoose, Jason L.

    2008-01-01

    Full Text: Ultra Performance Liquid Chromatography (UPLC) offers several advantages compared with conventional High Performance Liquid Chromatography (HPLC) as an 'inlet system' for mass spectrometry. UPLC provides improved chromatographic resolution, increased sensitivity and reduced analysis time. This is achieved through the use of sub 2μm particles (stationary phase) combined with high-pressure solvent delivery (up to 15,000 psi). When coupled with orthogonal acceleration time-of-flight (oa-TOF) mass spectrometry (MS), UPLC presents a means to achieve high sample throughput with reduced spectral overlap, increased sensitivity, and exact mass measurement capabilities with high mass spectral resolution (Ca 20,000 FWHM). Dispersive ion mobility spectrometry (IMS) implemented within a traveling-wave ion guide provides an orthogonal separation strategy for ions in the gas phase that can resolve isobaric ions formed by either Electrospray of MALDI ionization typically in Ca 20 mille seconds. All three techniques have the potential to be combined on-line (e.g. UPLC-IMS-MS/MS) in real time to maximize peak capacity and resolving power for the analysis of complex biological mixtures including; intact proteins, modified peptides and endogenous/exogenous metabolites

  11. Laboratory techniques for safe encapsulation of α-emitting powder samples

    International Nuclear Information System (INIS)

    Chamberlain, H.E.; Pottinger, J.S.

    1984-01-01

    Plutonium oxide powder samples can be encapsulated in thin plastic film to prevent spread of contamination in counting and X-ray diffraction equipment. The film has to be thin enough to transmit X-rays and α-particles. Techniques are described for the wrapping process and the precautions necessary to keep the sample processing line free of significant contamination. (author)

  12. Radio-analysis of hydrogenous material using neutron back-scattering technique

    International Nuclear Information System (INIS)

    Holly, Wiam Ahmed Alteghany

    2014-10-01

    In this work, we have explored the possibility of using neutron back-scattering technique in performing radio analysis for samples of hydrogenous materials such as explosives, drugs, crude oil and water, looking for different signals that may be used to discriminate these samples. Monte Carlo simulations were carried out to model the detection system and select the optimal geometry as well. The results were determined in terms of the energy spectra of the back-scattered neutrons.(Author)

  13. Use of fission track analysis technique for the determination of MicroBequerel level of {sup 239}Pu in urine samples from radiation workers handling MOX fuel

    Energy Technology Data Exchange (ETDEWEB)

    Yadav, J.R., E-mail: yadav_jogendra@rediffmail.co [Health Physics Laboratory, Health Physics Division, BARC, Tarapur 401502 (India); Rao, D.D.; Kumar, Ranjeet [Health Physics Laboratory, Health Physics Division, BARC, Tarapur 401502 (India); Aggarwal, S.K. [Fuel chemistry Division, BARC, Trombay, Mumbai 400085 (India)

    2011-07-15

    Fission track analysis (FTA) technique for the determination of {sup 239}Pu excreted through urine has been standardized using blank samples, tracer and {sup 239}Pu spikes. Double stage anion exchange separation protocol has been applied and an average radiochemical recovery of {sup 239}Pu of 18% was obtained. An average track registration efficiency of 11 tracks per {mu}Bq of {sup 239}Pu, irradiated to 0.35x10{sup 17} neutron fluence was established. Reagent blank urine samples from 11 controlled subjects were analyzed by FTA and an average of 149{+-}14 tracks was obtained. Minimum detectable activity of 34 {mu}Bq L{sup -1} of urine sample was obtained and will be useful for monitoring chronic exposure cases handling MOX fuel.

  14. A cost-saving statistically based screening technique for focused sampling of a lead-contaminated site

    International Nuclear Information System (INIS)

    Moscati, A.F. Jr.; Hediger, E.M.; Rupp, M.J.

    1986-01-01

    High concentrations of lead in soils along an abandoned railroad line prompted a remedial investigation to characterize the extent of contamination across a 7-acre site. Contamination was thought to be spotty across the site reflecting its past use in battery recycling operations at discrete locations. A screening technique was employed to delineate the more highly contaminated areas by testing a statistically determined minimum number of random samples from each of seven discrete site areas. The approach not only quickly identified those site areas which would require more extensive grid sampling, but also provided a statistically defensible basis for excluding other site areas from further consideration, thus saving the cost of additional sample collection and analysis. The reduction in the number of samples collected in ''clean'' areas of the site ranged from 45 to 60%

  15. Uncertainty Estimation of Neutron Activation Analysis in Zinc Elemental Determination in Food Samples

    International Nuclear Information System (INIS)

    Endah Damastuti; Muhayatun; Diah Dwiana L

    2009-01-01

    Beside to complished the requirements of international standard of ISO/IEC 17025:2005, uncertainty estimation should be done to increase quality and confidence of analysis results and also to establish traceability of the analysis results to SI unit. Neutron activation analysis is a major technique used by Radiometry technique analysis laboratory and is included as scope of accreditation under ISO/IEC 17025:2005, therefore uncertainty estimation of neutron activation analysis is needed to be carried out. Sample and standard preparation as well as, irradiation and measurement using gamma spectrometry were the main activities which could give contribution to uncertainty. The components of uncertainty sources were specifically explained. The result of expanded uncertainty was 4,0 mg/kg with level of confidence 95% (coverage factor=2) and Zn concentration was 25,1 mg/kg. Counting statistic of cuplikan and standard were the major contribution of combined uncertainty. The uncertainty estimation was expected to increase the quality of the analysis results and could be applied further to other kind of samples. (author)

  16. Sampling phased array a new technique for signal processing and ultrasonic imaging

    OpenAIRE

    Bulavinov, A.; Joneit, D.; Kröning, M.; Bernus, L.; Dalichow, M.H.; Reddy, K.M.

    2006-01-01

    Different signal processing and image reconstruction techniques are applied in ultrasonic non-destructive material evaluation. In recent years, rapid development in the fields of microelectronics and computer engineering lead to wide application of phased array systems. A new phased array technique, called "Sampling Phased Array" has been developed in Fraunhofer Institute for non-destructive testing. It realizes unique approach of measurement and processing of ultrasonic signals. The sampling...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1998-12-01

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

  18. Sampling and Analysis for Assessment of Body Burdens

    International Nuclear Information System (INIS)

    Harley, J.H.

    1964-01-01

    A review of sampling criteria and techniques and of sample processing methods for indirect assessment of body burdens is presented. The text is limited to the more recent developments in the field of bioassay and to the nuclides which cannot be readily determined in the body directly. A selected bibliography is included. The planning of a bioassay programme should emphasize the detection of high or unusual exposures and the concentrated study of these cases when detected. This procedure gives the maximum amount of data for the dosimetry of individuals at risk and also adds to our scientific background for an understanding of internal emitters. Only a minimum of effort should be spent on sampling individuals having had negligible exposure. The chemical separation procedures required for bioassay also fall into two categories. The first is the rapid method, possibly of low accuracy, used for detection. The second is the more accurate method required for study of the individual after detection of the exposure. Excretion, whether exponential or a power function, drops off rapidly. It is necessary to locate the exposure in time before any evaluation can be made, even before deciding if the exposure is significant. One approach is frequent sampling and analysis by a quick screening technique. More commonly, samples are collected at longer intervals and an arbitrary level of re-sampling is set to assist in the detection of real exposures. It is probable that too much bioassay effort has gone into measurements on individuals at low risk and not enough on those at higher risk. The development of bioassay procedures for overcoming this problem has begun, and this paper emphasizes this facet of sampling and sample processing. (author) [fr

  19. Retrospective analysis of dengue specific IgM reactive serum samples

    OpenAIRE

    Nemai Bhattacharya; Bhaswati Bandyopadhyay; Indranil Bhattacharjee; Hiranmoy Mukherjee; Srabani Talukdar; Ruby Mondal; Netai Pramanick; Goutam Chandra; Amiya K. Hati

    2013-01-01

    Objective: To conduct a retrospective analysis of dengue cases in Kolkata, on the basis of presence of anti-dengue IgM in their sera and presence or absence of anti-dengue IgG and dengue specific Non structural 1 (NS1) antigen in each of the serum sample. Methods: Sample was tested quantitatively employing ELISA technique, using Biorad test kits, with a view to get a more comprehensive picture of dengue in an urban endemic area and also to evaluate individual cases. Results: Th...

  20. Informational analysis for compressive sampling in radar imaging.

    Science.gov (United States)

    Zhang, Jingxiong; Yang, Ke

    2015-03-24

    Compressive sampling or compressed sensing (CS) works on the assumption of the sparsity or compressibility of the underlying signal, relies on the trans-informational capability of the measurement matrix employed and the resultant measurements, operates with optimization-based algorithms for signal reconstruction and is thus able to complete data compression, while acquiring data, leading to sub-Nyquist sampling strategies that promote efficiency in data acquisition, while ensuring certain accuracy criteria. Information theory provides a framework complementary to classic CS theory for analyzing information mechanisms and for determining the necessary number of measurements in a CS environment, such as CS-radar, a radar sensor conceptualized or designed with CS principles and techniques. Despite increasing awareness of information-theoretic perspectives on CS-radar, reported research has been rare. This paper seeks to bridge the gap in the interdisciplinary area of CS, radar and information theory by analyzing information flows in CS-radar from sparse scenes to measurements and determining sub-Nyquist sampling rates necessary for scene reconstruction within certain distortion thresholds, given differing scene sparsity and average per-sample signal-to-noise ratios (SNRs). Simulated studies were performed to complement and validate the information-theoretic analysis. The combined strategy proposed in this paper is valuable for information-theoretic orientated CS-radar system analysis and performance evaluation.

  1. The application of radiotracer technique for preconcentration neutron activation analysis

    International Nuclear Information System (INIS)

    Wang Xiaolin; Chen Yinliang; Sun Ying; Fu Yibei

    1995-01-01

    The application of radiotracer technique for preconcentration neutron activation analysis (Pre-NAA) are studied and the method for determination of chemical yield of Pre-NAA is developed. This method has been applied to determination of gold, iridium and rhenium in steel and rock samples and the contents of noble metal are in the range of 1-20 ng·g -1 (sample). In addition, the accuracy difference caused by determination of chemical yield between RNAA and Pre-NAA are also discussed

  2. Assessment of Natural Radioactivity in TENORM Samples Using Different Techniques

    International Nuclear Information System (INIS)

    Salman, Kh.A.; Shahein, A.Y.

    2009-01-01

    In petroleum oil industries, technologically-enhanced, naturally occurring radioactive materials are produced. The presence of TENORM constitutes a significant radiological human health hazard. In the present work, liquid scintillation counting technique was used to determine both 222 Rn and 226 Ra concentrations in TENORM samples, by measuring 222 Rn concentrations in the sample at different intervals of time after preparation. The radiation doses from the TENORM samples were estimated using thermoluminenscent detector (TLD-4000). The estimated radiation doses were found to be proportional to both the measured radiation doses in site and natural activity concentration in the samples that measured with LSC

  3. The application of x-ray fluorescence spectrometry for multielemental analysis of air particulate samples

    International Nuclear Information System (INIS)

    Mohamad Rashid Mohamad Yusoff

    1986-01-01

    The performance of XRF spectrometer as a tool for multielemental analysis of air pollution samples was discussed. The non-destructive couples with multielemental nature of the technique satisfactory sensitivity for most elements were the most important characteristics for its popularity as a method of analysis. Thus, the technique promises a significant reduction in cost and time of analysis. As a result, more extensive and revealing air particulates survey should be possible, with consequent improvements in the discovery and positive identification of particulate pollution sources. (author)

  4. Sampling and analytical methodologies for instrumental neutron activation analysis of airborne particulate matter

    International Nuclear Information System (INIS)

    1992-01-01

    The IAEA supports a number of projects having to do with the analysis of airborne particulate matter by nuclear techniques. Most of this work involves the use of activation analysis in its various forms, particularly instrumental neutron activation analysis (INAA). This technique has been widely used in many different countries for the analysis of airborne particulate matter, and there are already many publications in scientific journals, books and reports describing such work. The present document represents an attempt to summarize the most important features of INAA as applied to the analysis of airborne particulate matter. It is intended to serve as a set of guidelines for use by participants in the IAEA's own programmes, and other scientists, who are not yet fully experienced in the application of INAA to airborne particulate samples, and who wish either to make a start on using this technique or to improve their existing procedures. The methodologies for sampling described in this document are of rather general applicability, although they are presented here in a way that takes account of the particular requirements arising from the use of INAA as the analytical technique. The analytical part of the document, however, is presented in a form that is applicable only to INAA. (Subsequent publications in this series are expected to deal specifically with other nuclear related techniques such as energy dispersive X ray fluorescence (ED-XRF) and particle induced X ray emission (PIXE) analysis). Although the methods and procedures described here have been found through experience to yield acceptable results, they should not be considered mandatory. Any other procedure used should, however, be chosen to be capable of yielding results at least of equal quality to those described

  5. Sampling and analytical methodologies for instrumental neutron activation analysis of airborne particulate matter

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1992-12-01

    The IAEA supports a number of projects having to do with the analysis of airborne particulate matter by nuclear techniques. Most of this work involves the use of activation analysis in its various forms, particularly instrumental neutron activation analysis (INAA). This technique has been widely used in many different countries for the analysis of airborne particulate matter, and there are already many publications in scientific journals, books and reports describing such work. The present document represents an attempt to summarize the most important features of INAA as applied to the analysis of airborne particulate matter. It is intended to serve as a set of guidelines for use by participants in the IAEA's own programmes, and other scientists, who are not yet fully experienced in the application of INAA to airborne particulate samples, and who wish either to make a start on using this technique or to improve their existing procedures. The methodologies for sampling described in this document are of rather general applicability, although they are presented here in a way that takes account of the particular requirements arising from the use of INAA as the analytical technique. The analytical part of the document, however, is presented in a form that is applicable only to INAA. (Subsequent publications in this series are expected to deal specifically with other nuclear related techniques such as energy dispersive X ray fluorescence (ED-XRF) and particle induced X ray emission (PIXE) analysis). Although the methods and procedures described here have been found through experience to yield acceptable results, they should not be considered mandatory. Any other procedure used should, however, be chosen to be capable of yielding results at least of equal quality to those described.

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

    International Nuclear Information System (INIS)

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

    1975-01-01

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

  7. Review of online coupling of sample preparation techniques with liquid chromatography.

    Science.gov (United States)

    Pan, Jialiang; Zhang, Chengjiang; Zhang, Zhuomin; Li, Gongke

    2014-03-07

    Sample preparation is still considered as the bottleneck of the whole analytical procedure, and efforts has been conducted towards the automation, improvement of sensitivity and accuracy, and low comsuption of organic solvents. Development of online sample preparation techniques (SP) coupled with liquid chromatography (LC) is a promising way to achieve these goals, which has attracted great attention. This article reviews the recent advances on the online SP-LC techniques. Various online SP techniques have been described and summarized, including solid-phase-based extraction, liquid-phase-based extraction assisted with membrane, microwave assisted extraction, ultrasonic assisted extraction, accelerated solvent extraction and supercritical fluids extraction. Specially, the coupling approaches of online SP-LC systems and the corresponding interfaces have been discussed and reviewed in detail, such as online injector, autosampler combined with transport unit, desorption chamber and column switching. Typical applications of the online SP-LC techniques have been summarized. Then the problems and expected trends in this field are attempted to be discussed and proposed in order to encourage the further development of online SP-LC techniques. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Cleaning and Cleanliness Verification Techniques for Mars Returned Sample Handling

    Science.gov (United States)

    Mickelson, E. T.; Lindstrom, D. J.; Allton, J. H.; Hittle, J. D.

    2002-01-01

    Precision cleaning and cleanliness verification techniques are examined as a subset of a comprehensive contamination control strategy for a Mars sample return mission. Additional information is contained in the original extended abstract.

  9. Application of energy dispersive x-ray techniques for water analysis

    International Nuclear Information System (INIS)

    Funtua, I. I.

    2000-07-01

    Energy dispersive x-ray fluorescence (EDXRF) is a class of emission spectroscopic techniques that depends upon the emission of characteristic x-rays following excitation of the atomic electron energy levels by tube or isotopic source x-rays. The technique has found wide range of applications that include determination of chemical elements of water and water pollutants. Three EDXRF systems, the isotopic source, secondary target and total reflection (TXRF) are available at the Centre for Energy research and Training. These systems have been applied for the analysis of sediments, suspensions, ground water, river and rainwater. The isotopic source is based on 55 Fe, 109 Cd and 241 Am excitations while the secondary target and the total reflection are utilizing a Mo x-ray tube. Sample preparation requirements for water analysis range from physical and chemical pre-concentration steps to direct analysis and elements from Al to U can be determined with these systems. The EDXRF techniques, TXRF in particular with its multielement capability, low detection limit and possibility of direct analysis for water have competitive edge over the traditional methods of atomic absorption and flame photometry

  10. [A comparison of convenience sampling and purposive sampling].

    Science.gov (United States)

    Suen, Lee-Jen Wu; Huang, Hui-Man; Lee, Hao-Hsien

    2014-06-01

    Convenience sampling and purposive sampling are two different sampling methods. This article first explains sampling terms such as target population, accessible population, simple random sampling, intended sample, actual sample, and statistical power analysis. These terms are then used to explain the difference between "convenience sampling" and purposive sampling." Convenience sampling is a non-probabilistic sampling technique applicable to qualitative or quantitative studies, although it is most frequently used in quantitative studies. In convenience samples, subjects more readily accessible to the researcher are more likely to be included. Thus, in quantitative studies, opportunity to participate is not equal for all qualified individuals in the target population and study results are not necessarily generalizable to this population. As in all quantitative studies, increasing the sample size increases the statistical power of the convenience sample. In contrast, purposive sampling is typically used in qualitative studies. Researchers who use this technique carefully select subjects based on study purpose with the expectation that each participant will provide unique and rich information of value to the study. As a result, members of the accessible population are not interchangeable and sample size is determined by data saturation not by statistical power analysis.

  11. Research Progress on Pesticide Residue Analysis Techniques in Agro-products

    Directory of Open Access Journals (Sweden)

    HE Ze-ying

    2016-07-01

    Full Text Available There are constant occurrences of acute pesticide poisoning among consumers and pesticide residue violations in agro-products import/export trading. Pesticide residue analysis is the important way to protect the food safety and the interest of import/export enterprises. There has been a rapid development in pesticide residue analysis techniques in recent years. In this review, the research progress in the past five years were discussed in the respects of samples preparation and instrument determination. The application, modification and development of the QuEChERS method in samples preparation and the application of tandem mass spectrometry and high resolution mass spectrometry were reviewed. And the implications for the future of the field were discussed.

  12. APPLICATION OF NEUTRON ACTIVATION ANALYSIS IN CHARACTERIZATION OF ENVIRONMENTAL SRM SAMPLES

    Directory of Open Access Journals (Sweden)

    Diah Dwiana Lestiani

    2010-06-01

    Full Text Available Neutron activation analysis (NAA is a nuclear technique that is excellent, multi-elemental, sensitive and has limit detection up to nanogram level. The application of NAA in analysis of Standard Reference Material (SRM National Institute of Standard Technology (NIST 1633b Coal Fly Ash and SRM NIST 1646a Estuarine Sediment was carried out for NAA laboratory inter-comparison program. The samples were distributed by Technology Centre for Nuclear Industry Material, National Nuclear Energy Agency as a coordinator of the inter-comparison program. The samples were irradiated in rabbit facility of G.A. Siwabessy reactor with neutron flux ~ 1013 n.cm-2.s-1, and counted with HPGe spectrometry gamma detector. Several trace elements in these samples were detected. The concentration of Al, Mg, K, Na and Ti in SRM NIST 1633b were 15.11, 7.35, 2.09, 0.192 and 0.756% respectively and the concentration of As, Cr, Mn, Se, V, Sb, Co, Cs, La, Sc and Sm were 137.0, 195.6, 129.4, 9.61, 305.8, 5.45, 56.2, 11.18, 83.73, 41.1 and 19.13 mg/kg respectively. The analysis result in SRM NIST 1646a of the concentration of Al and Na were 2.15 and 0.70% and the concentration of As, Cr, Co, La and Sc were 5.75, 36.3, 4.58, 15.67 and 4.00 mg/kg respectively. These results analysis had relative bias and u-test ranged from 0.4-11.3% and 0.15-2.25. The accuracy and precision evaluation based on International Atomic Energy Agency (IAEA criteria was also applied. The result showed that NAA technique is applicable for the environmental samples analysis, and it also showed that the NAA laboratory in BATAN Bandung has a good performance.   Keywords: NAA, inter-comparison, estuarine sediment, coal fly ash, environmental samples

  13. Exploratory Factor Analysis With Small Samples and Missing Data.

    Science.gov (United States)

    McNeish, Daniel

    2017-01-01

    Exploratory factor analysis (EFA) is an extremely popular method for determining the underlying factor structure for a set of variables. Due to its exploratory nature, EFA is notorious for being conducted with small sample sizes, and recent reviews of psychological research have reported that between 40% and 60% of applied studies have 200 or fewer observations. Recent methodological studies have addressed small size requirements for EFA models; however, these models have only considered complete data, which are the exception rather than the rule in psychology. Furthermore, the extant literature on missing data techniques with small samples is scant, and nearly all existing studies focus on topics that are not of primary interest to EFA models. Therefore, this article presents a simulation to assess the performance of various missing data techniques for EFA models with both small samples and missing data. Results show that deletion methods do not extract the proper number of factors and estimate the factor loadings with severe bias, even when data are missing completely at random. Predictive mean matching is the best method overall when considering extracting the correct number of factors and estimating factor loadings without bias, although 2-stage estimation was a close second.

  14. Field-based detection of biological samples for forensic analysis: Established techniques, novel tools, and future innovations.

    Science.gov (United States)

    Morrison, Jack; Watts, Giles; Hobbs, Glyn; Dawnay, Nick

    2018-04-01

    Field based forensic tests commonly provide information on the presence and identity of biological stains and can also support the identification of species. Such information can support downstream processing of forensic samples and generate rapid intelligence. These approaches have traditionally used chemical and immunological techniques to elicit the result but some are known to suffer from a lack of specificity and sensitivity. The last 10 years has seen the development of field-based genetic profiling systems, with specific focus on moving the mainstay of forensic genetic analysis, namely STR profiling, out of the laboratory and into the hands of the non-laboratory user. In doing so it is now possible for enforcement officers to generate a crime scene DNA profile which can then be matched to a reference or database profile. The introduction of these novel genetic platforms also allows for further development of new molecular assays aimed at answering the more traditional questions relating to body fluid identity and species detection. The current drive for field-based molecular tools is in response to the needs of the criminal justice system and enforcement agencies, and promises a step-change in how forensic evidence is processed. However, the adoption of such systems by the law enforcement community does not represent a new strategy in the way forensic science has integrated previous novel approaches. Nor do they automatically represent a threat to the quality control and assurance practices that are central to the field. This review examines the historical need and subsequent research and developmental breakthroughs in field-based forensic analysis over the past two decades with particular focus on genetic methods Emerging technologies from a range of scientific fields that have potential applications in forensic analysis at the crime scene are identified and associated issues that arise from the shift from laboratory into operational field use are discussed

  15. Toxicological Analysis of Some Drugs of Abuse in Biological Samples

    Directory of Open Access Journals (Sweden)

    Anne Marie Ciobanu

    2015-10-01

    Full Text Available Consumption of drugs of abuse is a scourge of modern world. Abuse, drug addiction and their consequences are one of the major current problems of European society because of the significant repercussions in individual, family, social and economic level. In this context, toxicological analysis of the drugs of abuse in biological samples is a useful tool for: diagnosis of drug addiction, checking an auto-response, mandatory screening in some treatment programs, identification of a substance in the case of an overdose, determining compliance of the treatment. The present paper aims to address the needs of healthcare professionals involved in drugs addiction treatment through systematic presentation of information regarding their toxicological analysis. Basically, it is a tool that help you to select the suitable biological sample and the right collecting time, as well as the proper analysis technique, depending on the purpose of analysis, pharmacokinetic characteristics of the drugs of abuse, available equipment and staff expertise.

  16. Nondestructive neutron activation analysis of volcanic samples: Hawaii

    International Nuclear Information System (INIS)

    Zoller, W.H.; Finnegan, D.L.; Crowe, B.

    1986-01-01

    Samples of volcanic emissions have been collected between and during eruptions of both Kilauea and Mauna Loa volcanoes during the last three years. Airborne particles have been collected on Teflon filters and acidic gases on base-impregnated cellulose filters. Chemically neutral gas-phase species are collected on charcoal-coated cellulose filters. The primary analytical technique used is nondestructive neutron activation analysis, which has been used to determine the quantities of up to 35 elements on the different filters. The use of neutron activation analysis makes it possible to analyze for a wide range of elements in the different matrices used for the collection and to learn about the distribution between particles and gas phases for each of the elements

  17. Trace metals analysis in molybdenite mineral sample

    International Nuclear Information System (INIS)

    Tamrakar, Praveen Kumar; Pitre, K.S.

    2000-01-01

    DC polarography and other related techniques, viz., DPP and DPASV have been successfully used for the simultaneous determination of trace metals in molybdenite mineral sample. The polarograms and voltammograms of sample solution have been recorded in 0.1 M (NH 4 ) 2 tartrate supporting electrolyte at two different pH values i.e., 2.7±0.1 and 9.0±0.1. The results indicate the presence of Cu 2+ , Mo 6+ , Cd 2+ , Ni 2+ , In 3+ , Fe 3+ and W 6+ metal ions in the sample. For the determination of tungsten(VI), 11 M HCl has been used as supporting electrolyte. Tungsten(VI) produces a well defined wave/peak with E 1/2 /Ep=-0.42V/-0.48V vs SCE in 11 M HCl. The quantitative analysis by the method of standard addition shows the mineral sample to have the following composition, Cu 2+ ( 14.83), Mo 6+ (253.70), Cd 2+ (41.36), Ni 2+ (16.08), In 3+ (3.06), Fe 3+ (83.00)and W 6+ (4.14 )mg/g of the sample. Statistical treatment of the observed voltammetric data reveals high accuracy and good precision of determination. The observed voltammetric results are comparable with those obtained using AAS method. (author)

  18. Surface analysis the principal techniques

    CERN Document Server

    Vickerman, John C

    2009-01-01

    This completely updated and revised second edition of Surface Analysis: The Principal Techniques, deals with the characterisation and understanding of the outer layers of substrates, how they react, look and function which are all of interest to surface scientists. Within this comprehensive text, experts in each analysis area introduce the theory and practice of the principal techniques that have shown themselves to be effective in both basic research and in applied surface analysis. Examples of analysis are provided to facilitate the understanding of this topic and to show readers how they c

  19. THE STUDY OF HEAVY METAL FROM ENVIRONMENTAL SAMPLES BY ATOMIC TECHNIQUES

    Directory of Open Access Journals (Sweden)

    Ion V. POPESCU

    2011-05-01

    Full Text Available Using the Atomic Absorption Spectrometry (AAS and Energy Dispersive X-ray spectrometry (EDXRF techniques we analyzed the contents of heavy metals ( Cd, Cr, Ni, Pb, Ti, Sr, Co, Bi from eight wild mushrooms and soil substrate samples (48 samples of eight fungal species and 32 underlying soil samples, collected from ten forest sites of Dambovița County Romania. It was determined that the elements, especially heavy metals, in soil were characteristic of the acidic soils of the Romanian forest lands and are influenced by industrial pollution. Analytical possibilities of AAS and EDXRF analytical techniques have been compared and the heavy metal transfer from substrate to mushrooms has been studied. The coefficient of accumulation of essential and heavy metals has been calculated as well. Heavy metal contents of all analyzed mushrooms were generally higher than previously reported in literature.

  20. Comparison between correlated sampling and the perturbation technique of MCNP5 for fixed-source problems

    International Nuclear Information System (INIS)

    He Tao; Su Bingjing

    2011-01-01

    Highlights: → The performance of the MCNP differential operator perturbation technique is compared with that of the MCNP correlated sampling method for three types of fixed-source problems. → In terms of precision, the MCNP perturbation technique outperforms correlated sampling for one type of problem but performs comparably with or even under-performs correlated sampling for the other two types of problems. → In terms of accuracy, the MCNP perturbation calculations may predict inaccurate results for some of the test problems. However, the accuracy can be improved if the midpoint correction technique is used. - Abstract: Correlated sampling and the differential operator perturbation technique are two methods that enable MCNP (Monte Carlo N-Particle) to simulate small response change between an original system and a perturbed system. In this work the performance of the MCNP differential operator perturbation technique is compared with that of the MCNP correlated sampling method for three types of fixed-source problems. In terms of precision of predicted response changes, the MCNP perturbation technique outperforms correlated sampling for the problem involving variation of nuclide concentrations in the same direction but performs comparably with or even underperforms correlated sampling for the other two types of problems that involve void or variation of nuclide concentrations in opposite directions. In terms of accuracy, the MCNP differential operator perturbation calculations may predict inaccurate results that deviate from the benchmarks well beyond their uncertainty ranges for some of the test problems. However, the accuracy of the MCNP differential operator perturbation can be improved if the midpoint correction technique is used.

  1. Enhanced Sampling and Analysis, Selection of Technology for Testing

    Energy Technology Data Exchange (ETDEWEB)

    Svoboda, John; Meikrantz, David

    2010-02-01

    The focus of this study includes the investigation of sampling technologies used in industry and their potential application to nuclear fuel processing. The goal is to identify innovative sampling methods using state of the art techniques that could evolve into the next generation sampling and analysis system for metallic elements. This report details the progress made in the first half of FY 2010 and includes a further consideration of the research focus and goals for this year. Our sampling options and focus for the next generation sampling method are presented along with the criteria used for choosing our path forward. We have decided to pursue the option of evaluating the feasibility of microcapillary based chips to remotely collect, transfer, track and supply microliters of sample solutions to analytical equipment in support of aqueous processes for used nuclear fuel cycles. Microchip vendors have been screened and a choice made for the development of a suitable microchip design followed by production of samples for evaluation by ANL, LANL, and INL on an independent basis.

  2. A technique for extracting blood samples from mice in fire toxicity tests

    Science.gov (United States)

    Bucci, T. J.; Hilado, C. J.; Lopez, M. T.

    1976-01-01

    The extraction of adequate blood samples from moribund and dead mice has been a problem because of the small quantity of blood in each animal and the short time available between the animals' death and coagulation of the blood. These difficulties are particularly critical in fire toxicity tests because removal of the test animals while observing proper safety precautions for personnel is time-consuming. Techniques for extracting blood samples from mice were evaluated, and a technique was developed to obtain up to 0.8 ml of blood from a single mouse after death. The technique involves rapid exposure and cutting of the posterior vena cava and accumulation of blood in the peritoneal space. Blood samples of 0.5 ml or more from individual mice have been consistently obtained as much as 16 minutes after apparent death. Results of carboxyhemoglobin analyses of blood appeared reproducible and consistent with carbon monoxide concentrations in the exposure chamber.

  3. Amorphous and liquid samples structure and density measurements at high pressure - high temperature using diffraction and imaging techniques

    Science.gov (United States)

    Guignot, N.; King, A.; Clark, A. N.; Perrillat, J. P.; Boulard, E.; Morard, G.; Deslandes, J. P.; Itié, J. P.; Ritter, X.; Sanchez-Valle, C.

    2016-12-01

    Determination of the density and structure of liquids such as iron alloys, silicates and carbonates is a key to understand deep Earth structure and dynamics. X-ray diffraction provided by large synchrotron facilities gives excellent results as long as the signal scattered from the sample can be isolated from its environment. Different techniques already exist; we present here the implementation and the first results given by the combined angle- and energy-dispersive structural analysis and refinement (CAESAR) technique introduced by Wang et al. in 2004, that has never been used in this context. It has several advantages in the study of liquids: 1/ the standard energy-dispersive technique (EDX), fast and compatible with large multi-anvil presses frames, is used for fast analysis free of signal pollution from the sample environment 2/ some limitations of the EDX technique (homogeneity of the sample, low resolution) are irrelevant in the case of liquid signals, others (wrong intensities, escape peaks artifacts, background subtraction) are solved by the CAESAR technique 3/ high Q data (up to 15 A-1 and more) can be obtained in a few hours (usually less than 2). We present here the facilities available on the PSICHE beamline (SOLEIL synchrotron, France) and a few results obtained using a Paris-Edinburgh (PE) press and a 1200 tons load capacity multi-anvil press with a (100) DIA compression module. X-ray microtomography, used in conjunction with a PE press featuring rotating anvils (RotoPEc, Philippe et al., 2013) is also very effective, by simply measuring the 3D volume of glass or liquid spheres at HPHT, thus providing density. This can be done in conjunction with the CAESAR technique and we illustrate this point. Finally, absorption profiles can be obtained via imaging techniques, providing another independent way to measure the density of these materials. References Y. Wang et al., A new technique for angle-dispersive powder diffraction using an energy

  4. Sampling in forests for radionuclide analysis. General and practical guidance

    Energy Technology Data Exchange (ETDEWEB)

    Aro, Lasse (Finnish Forest Research Inst. (METLA) (Finland)); Plamboeck, Agneta H. (Swedish Defence Research Agency (FOI) (Sweden)); Rantavaara, Aino; Vetikko, Virve (Radiation and Nuclear Safety Authority (STUK) (Finland)); Straalberg, Elisabeth (Inst. Energy Technology (IFE) (Norway))

    2009-01-15

    The NKS project FOREST was established to prepare a guide for sampling in forest ecosystems for radionuclide analysis. The aim of this guide is to improve the reliability of datasets generated in future studies by promoting the use of consistent, recommended practices, thorough documentation of field sampling regimes and robust preparation of samples from the forest ecosystem. The guide covers general aims of sampling, the description of major compartments of the forest ecosystem and outlines key factors to consider when planning sampling campaigns for radioecological field studies in forests. Recommended and known sampling methods for various sample types are also compiled and presented. The guide focuses on sampling practices that are applicable in various types of boreal forests, robust descriptions of sampling sites, and documentation of the origin and details of individual samples. The guide is intended for scientists, students, forestry experts and technicians who appreciate the need to use sound sampling procedures in forest radioecological projects. The guide will hopefully encourage readers to participate in field studies and sampling campaigns, using robust techniques, thereby fostering competence in sampling. (au)

  5. Sampling in forests for radionuclide analysis. General and practical guidance

    International Nuclear Information System (INIS)

    Aro, Lasse; Plamboeck, Agneta H.; Rantavaara, Aino; Vetikko, Virve; Straelberg, Elisabeth

    2009-01-01

    The NKS project FOREST was established to prepare a guide for sampling in forest ecosystems for radionuclide analysis. The aim of this guide is to improve the reliability of datasets generated in future studies by promoting the use of consistent, recommended practices, thorough documentation of field sampling regimes and robust preparation of samples from the forest ecosystem. The guide covers general aims of sampling, the description of major compartments of the forest ecosystem and outlines key factors to consider when planning sampling campaigns for radioecological field studies in forests. Recommended and known sampling methods for various sample types are also compiled and presented. The guide focuses on sampling practices that are applicable in various types of boreal forests, robust descriptions of sampling sites, and documentation of the origin and details of individual samples. The guide is intended for scientists, students, forestry experts and technicians who appreciate the need to use sound sampling procedures in forest radioecological projects. The guide will hopefully encourage readers to participate in field studies and sampling campaigns, using robust techniques, thereby fostering competence in sampling. (au)

  6. Uncertainty analysis techniques

    International Nuclear Information System (INIS)

    Marivoet, J.; Saltelli, A.; Cadelli, N.

    1987-01-01

    The origin of the uncertainty affecting Performance Assessments, as well as their propagation to dose and risk results is discussed. The analysis is focused essentially on the uncertainties introduced by the input parameters, the values of which may range over some orders of magnitude and may be given as probability distribution function. The paper briefly reviews the existing sampling techniques used for Monte Carlo simulations and the methods for characterizing the output curves, determining their convergence and confidence limits. Annual doses, expectation values of the doses and risks are computed for a particular case of a possible repository in clay, in order to illustrate the significance of such output characteristics as the mean, the logarithmic mean and the median as well as their ratios. The report concludes that provisionally, due to its better robustness, such estimation as the 90th percentile may be substituted to the arithmetic mean for comparison of the estimated doses with acceptance criteria. In any case, the results obtained through Uncertainty Analyses must be interpreted with caution as long as input data distribution functions are not derived from experiments reasonably reproducing the situation in a well characterized repository and site

  7. Comparison of sampling techniques for Rift Valley Fever virus ...

    African Journals Online (AJOL)

    We investigated mosquito sampling techniques with two types of traps and attractants at different time for trapping potential vectors for Rift Valley Fever virus. The study was conducted in six villages in Ngorongoro district in Tanzania from September to October 2012. A total of 1814 mosquitoes were collected, of which 738 ...

  8. Regional and global atmospheric aerosol studies using the ''Gent'' stacked filter unit sampler and other aerosol collectors, with multi-elemental analysis of the samples by nuclear-related analytical techniques

    International Nuclear Information System (INIS)

    Maenhaut, W.; Francois, F.; Salma, I.; Cafmeyer, J.; Gilot, C.

    1994-01-01

    The ''Gent'' staked filter unit sampler and other collection devices are used in regional and global scale studies on the tropospheric atmospheric aerosols, its composition, sources and fate. The aerosol samples are analyzed by particle-induced X-ray emission analysis, instrumental neutron activation analysis, ion chromatography, a light reflectance technique (for determining black carbon), and gravimetry (for measuring the particular mass). In evaluating the data, use is made of receptor modelling techniques, transport models and wind sector analysis, and also of air mass trajectories and other meteorological information. Preliminary results from a long-term study in southern Norway are presented. It is suggested that the anthropogenic and soil dust aerosol components are mainly adverted to southern Norway by long-range transport and that the major fraction of the submicrometer particle mass is from anthropogenic origin. Preliminary results are also presented for an intensive study in southern Africa. On the basis of the data for two sites (about 40 km apart) in the Kruger National Park it was concluded that regionally representative aerosol samples were collected and that the biomass burning products account for more than 50% of the fine particle mass. Finally, our plans for future work are given. (author). 70 refs, 4 figs, 1 tab

  9. Analytical techniques for wine analysis: An African perspective; a review

    International Nuclear Information System (INIS)

    Villiers, André de; Alberts, Phillipus; Tredoux, Andreas G.J.; Nieuwoudt, Hélène H.

    2012-01-01

    Highlights: ► Analytical techniques developed for grape and wine analysis in Africa are reviewed. ► The utility of infrared spectroscopic methods is demonstrated. ► An overview of separation of wine constituents by GC, HPLC, CE is presented. ► Novel LC and GC sample preparation methods for LC and GC are presented. ► Emerging methods for grape and wine analysis in Africa are discussed. - Abstract: Analytical chemistry is playing an ever-increasingly important role in the global wine industry. Chemical analysis of wine is essential in ensuring product safety and conformity to regulatory laws governing the international market, as well as understanding the fundamental aspects of grape and wine production to improve manufacturing processes. Within this field, advanced instrumental analysis methods have been exploited more extensively in recent years. Important advances in instrumental analytical techniques have also found application in the wine industry. This review aims to highlight the most important developments in the field of instrumental wine and grape analysis in the African context. The focus of this overview is specifically on the application of advanced instrumental techniques, including spectroscopic and chromatographic methods. Recent developments in wine and grape analysis and their application in the African context are highlighted, and future trends are discussed in terms of their potential contribution to the industry.

  10. Analytical techniques for wine analysis: An African perspective; a review

    Energy Technology Data Exchange (ETDEWEB)

    Villiers, Andre de, E-mail: ajdevill@sun.ac.za [Department of Chemistry and Polymer Science, Stellenbosch University, Private Bag X1, Matieland 7602, Stellenbosch (South Africa); Alberts, Phillipus [Department of Chemistry and Polymer Science, Stellenbosch University, Private Bag X1, Matieland 7602, Stellenbosch (South Africa); Tredoux, Andreas G.J.; Nieuwoudt, Helene H. [Institute for Wine Biotechnology, Department of Viticulture and Oenology, Stellenbosch University, Private Bag X1, Matieland 7602, Stellenbosch (South Africa)

    2012-06-12

    Highlights: Black-Right-Pointing-Pointer Analytical techniques developed for grape and wine analysis in Africa are reviewed. Black-Right-Pointing-Pointer The utility of infrared spectroscopic methods is demonstrated. Black-Right-Pointing-Pointer An overview of separation of wine constituents by GC, HPLC, CE is presented. Black-Right-Pointing-Pointer Novel LC and GC sample preparation methods for LC and GC are presented. Black-Right-Pointing-Pointer Emerging methods for grape and wine analysis in Africa are discussed. - Abstract: Analytical chemistry is playing an ever-increasingly important role in the global wine industry. Chemical analysis of wine is essential in ensuring product safety and conformity to regulatory laws governing the international market, as well as understanding the fundamental aspects of grape and wine production to improve manufacturing processes. Within this field, advanced instrumental analysis methods have been exploited more extensively in recent years. Important advances in instrumental analytical techniques have also found application in the wine industry. This review aims to highlight the most important developments in the field of instrumental wine and grape analysis in the African context. The focus of this overview is specifically on the application of advanced instrumental techniques, including spectroscopic and chromatographic methods. Recent developments in wine and grape analysis and their application in the African context are highlighted, and future trends are discussed in terms of their potential contribution to the industry.

  11. Multiple predictor smoothing methods for sensitivity analysis: Description of techniques

    International Nuclear Information System (INIS)

    Storlie, Curtis B.; Helton, Jon C.

    2008-01-01

    The use of multiple predictor smoothing methods in sampling-based sensitivity analyses of complex models is investigated. Specifically, sensitivity analysis procedures based on smoothing methods employing the stepwise application of the following nonparametric regression techniques are described: (i) locally weighted regression (LOESS), (ii) additive models, (iii) projection pursuit regression, and (iv) recursive partitioning regression. Then, in the second and concluding part of this presentation, the indicated procedures are illustrated with both simple test problems and results from a performance assessment for a radioactive waste disposal facility (i.e., the Waste Isolation Pilot Plant). As shown by the example illustrations, the use of smoothing procedures based on nonparametric regression techniques can yield more informative sensitivity analysis results than can be obtained with more traditional sensitivity analysis procedures based on linear regression, rank regression or quadratic regression when nonlinear relationships between model inputs and model predictions are present

  12. Quality assurance and reference material requirements and considerations for environmental sample analysis in nuclear forensics

    International Nuclear Information System (INIS)

    Swindle, D.W. Jr.; Perrin, R.E.; Goldberg, S.A.; Cappis, J.

    2002-01-01

    Full text: High-sensitivity nuclear environmental sampling and analysis techniques have been proven in their ability to verify declared nuclear activities, as well as to assist in the detection of undeclared nuclear activities and facilities. Following the Gulf War, the capability and revealing power of environmental sampling and analysis techniques to support international safeguards was demonstrated and subsequently adopted by the International Atomic Energy Agency (IAEA) as routine safeguards measures in safeguards inspections and verifications. In addition to having been proved useful in international safeguards, environmental sampling and analysis techniques have demonstrated their utility in identifying the origins of 'orphaned' nuclear material, as well as the origin of intercepted smuggled nuclear material. Today, environmental sampling and analysis techniques are now being applied in six broad areas to support nonproliferation, disarmament treaty verification, national and international nuclear security, and environmental stewardship of weapons production activities. Consequently, more and more laboratories around the world are establishing capabilities or expanding capabilities to meet these growing applications, and as such requirements for quality assurance and control are increasing. The six areas are: 1) Nuclear safeguards; 2) Nuclear forensics/illicit trafficking; 3) Ongoing monitoring and verification (OMV); 4) Comprehensive Test Ban Treaty (CTBT); 5) Weapons dismantlement/materials disposition; and 6) Research and development (R and D)/environmental stewardship/safety. Application of environmental sampling and analysis techniques and resources to illicit nuclear material trafficking, while embodying the same basic techniques and resources, does have unique requirements for sample management, handling, protocols, chain of custody, archiving, and data interpretation. These requirements are derived from needs of how data from nuclear forensics

  13. A line-based vegetation sampling technique and its application in ...

    African Journals Online (AJOL)

    percentage cover, density and intercept frequency) and also provides plant size distributions, yet requires no more sampling effort than the line-intercept method.. A field test of the three techniques in succulent karoo, showed that the discriminating ...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2002-12-15

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

  15. Proposal for Analysis of the Safeguarded Nuclear Materials 235U and 239Pu by Delayed Neutrons Technique

    International Nuclear Information System (INIS)

    El-Mongy, S.A.

    2000-01-01

    This paper introduces, describes and initiates a very sensitive and rapid non-destructive technique to be used for analysis of the safeguarded nuclear materials 235 U and 239 Pu. The technique is based on fission of the nuclear material by neutrons and then measuring the delayed neutrons produced from the neutron rich fission products. By this technique, fissile isotope content ( 235 U) can be determined in the presence of the other fissile (e.g. 239 Pu) or fertile isotopes (e.g. 238 U) in fresh and spent fuel. The time consumed for analysis of bulk materials by this technique is only 4 minutes. The method is also used for analysis of uranium in rock, sediment, soil, meteorites, lunar, biological, urine, archaeological, zircon sand and seawater samples. The method enables uranium in a sample to be measured without respect to its oxidation state, organic and inorganic elements

  16. A new sampling technique for surface exposure dating using a portable electric rock cutter

    Directory of Open Access Journals (Sweden)

    Yusuke Suganuma

    2012-07-01

    Full Text Available Surface exposure dating using in situ cosmogenic nuclides has contributed to our understanding of Earth-surface processes. The precision of the ages estimated by this method is affected by the sample geometry; therefore, high accuracy measurements of the thickness and shape of the rock sample (thickness and shape is crucial. However, it is sometimes diffi cult to meet these requirements by conventional sampling methods with a hammer and chisel. Here, we propose a new sampling technique using a portable electric rock cutter. This sampling technique is faster, produces more precisely shaped samples, and allows for a more precise age interpretation. A simple theoretical modeldemonstrates that the age error due to defective sample geometry increases as the total sample thickness increases, indicating the importance of precise sampling for surface exposure dating.

  17. Mantle biopsy: a technique for nondestructive tissue-sampling of freshwater mussels

    Science.gov (United States)

    David J. Berg; Wendell R. Haag; Sheldon I. Guttman; James B. Sickel

    1995-01-01

    Mantle biopsy is a means of obtaining tissue samples for genetic, physiological, and contaminant studies of bivalves; but the effects of this biopsy on survival have not been determined. We describe a simple technique for obtaining such samples from unionacean bivalves and how we compared survival among biopsied and control organisms in field experiments. Survival was...

  18. A Monte Carlo Sampling Technique for Multi-phonon Processes

    Energy Technology Data Exchange (ETDEWEB)

    Hoegberg, Thure

    1961-12-15

    A sampling technique for selecting scattering angle and energy gain in Monte Carlo calculations of neutron thermalization is described. It is supposed that the scattering is separated into processes involving different numbers of phonons. The number of phonons involved is first determined. Scattering angle and energy gain are then chosen by using special properties of the multi-phonon term.

  19. Evaluation of primary immunization coverage of infants under universal immunization programme in an urban area of bangalore city using cluster sampling and lot quality assurance sampling techniques.

    Science.gov (United States)

    K, Punith; K, Lalitha; G, Suman; Bs, Pradeep; Kumar K, Jayanth

    2008-07-01

    Is LQAS technique better than cluster sampling technique in terms of resources to evaluate the immunization coverage in an urban area? To assess and compare the lot quality assurance sampling against cluster sampling in the evaluation of primary immunization coverage. Population-based cross-sectional study. Areas under Mathikere Urban Health Center. Children aged 12 months to 23 months. 220 in cluster sampling, 76 in lot quality assurance sampling. Percentages and Proportions, Chi square Test. (1) Using cluster sampling, the percentage of completely immunized, partially immunized and unimmunized children were 84.09%, 14.09% and 1.82%, respectively. With lot quality assurance sampling, it was 92.11%, 6.58% and 1.31%, respectively. (2) Immunization coverage levels as evaluated by cluster sampling technique were not statistically different from the coverage value as obtained by lot quality assurance sampling techniques. Considering the time and resources required, it was found that lot quality assurance sampling is a better technique in evaluating the primary immunization coverage in urban area.

  20. A novel quantitative approach for eliminating sample-to-sample variation using a hue saturation value analysis program.

    Science.gov (United States)

    Yabusaki, Katsumi; Faits, Tyler; McMullen, Eri; Figueiredo, Jose Luiz; Aikawa, Masanori; Aikawa, Elena

    2014-01-01

    As computing technology and image analysis techniques have advanced, the practice of histology has grown from a purely qualitative method to one that is highly quantified. Current image analysis software is imprecise and prone to wide variation due to common artifacts and histological limitations. In order to minimize the impact of these artifacts, a more robust method for quantitative image analysis is required. Here we present a novel image analysis software, based on the hue saturation value color space, to be applied to a wide variety of histological stains and tissue types. By using hue, saturation, and value variables instead of the more common red, green, and blue variables, our software offers some distinct advantages over other commercially available programs. We tested the program by analyzing several common histological stains, performed on tissue sections that ranged from 4 µm to 10 µm in thickness, using both a red green blue color space and a hue saturation value color space. We demonstrated that our new software is a simple method for quantitative analysis of histological sections, which is highly robust to variations in section thickness, sectioning artifacts, and stain quality, eliminating sample-to-sample variation.

  1. On-line hydrogen-isotope measurements of organic samples using elemental chromium: An extension for high temperature elemental-analyzer techniques

    Science.gov (United States)

    Gehre, Matthias; Renpenning, Julian; Gilevska, Tetyana; Qi, Haiping; Coplen, Tyler B.; Meijer, Harro A.J.; Brand, Willi A.; Schimmelmann, Arndt

    2015-01-01

    The high temperature conversion (HTC) technique using an elemental analyzer with a glassy carbon tube and filling (temperature conversion/elemental analysis, TC/EA) is a widely used method for hydrogen isotopic analysis of water and many solid and liquid organic samples with analysis by isotope-ratio mass spectrometry (IRMS). However, the TC/EA IRMS method may produce inaccurate δ2H results, with values deviating by more than 20 mUr (milliurey = 0.001 = 1‰) from the true value for some materials. We show that a single-oven, chromium-filled elemental analyzer coupled to an IRMS substantially improves the measurement quality and reliability for hydrogen isotopic compositions of organic substances (Cr-EA method). Hot chromium maximizes the yield of molecular hydrogen in a helium carrier gas by irreversibly and quantitatively scavenging all reactive elements except hydrogen. In contrast, under TC/EA conditions, heteroelements like nitrogen or chlorine (and other halogens) can form hydrogen cyanide (HCN) or hydrogen chloride (HCl) and this can cause isotopic fractionation. The Cr-EA technique thus expands the analytical possibilities for on-line hydrogen-isotope measurements of organic samples significantly. This method yielded reproducibility values (1-sigma) for δ2H measurements on water and caffeine samples of better than 1.0 and 0.5 mUr, respectively. To overcome handling problems with water as the principal calibration anchor for hydrogen isotopic measurements, we have employed an effective and simple strategy using reference waters or other liquids sealed in silver-tube segments. These crimped silver tubes can be employed in both the Cr-EA and TC/EA techniques. They simplify considerably the normalization of hydrogen-isotope measurement data to the VSMOW-SLAP (Vienna Standard Mean Ocean Water-Standard Light Antarctic Precipitation) scale, and their use improves accuracy of the data by eliminating evaporative loss and associated isotopic fractionation while

  2. On-line hydrogen-isotope measurements of organic samples using elemental chromium: an extension for high temperature elemental-analyzer techniques.

    Science.gov (United States)

    Gehre, Matthias; Renpenning, Julian; Gilevska, Tetyana; Qi, Haiping; Coplen, Tyler B; Meijer, Harro A J; Brand, Willi A; Schimmelmann, Arndt

    2015-01-01

    The high temperature conversion (HTC) technique using an elemental analyzer with a glassy carbon tube and filling (temperature conversion/elemental analysis, TC/EA) is a widely used method for hydrogen isotopic analysis of water and many solid and liquid organic samples with analysis by isotope-ratio mass spectrometry (IRMS). However, the TC/EA IRMS method may produce inaccurate δ(2)H results, with values deviating by more than 20 mUr (milliurey = 0.001 = 1‰) from the true value for some materials. We show that a single-oven, chromium-filled elemental analyzer coupled to an IRMS substantially improves the measurement quality and reliability for hydrogen isotopic compositions of organic substances (Cr-EA method). Hot chromium maximizes the yield of molecular hydrogen in a helium carrier gas by irreversibly and quantitatively scavenging all reactive elements except hydrogen. In contrast, under TC/EA conditions, heteroelements like nitrogen or chlorine (and other halogens) can form hydrogen cyanide (HCN) or hydrogen chloride (HCl) and this can cause isotopic fractionation. The Cr-EA technique thus expands the analytical possibilities for on-line hydrogen-isotope measurements of organic samples significantly. This method yielded reproducibility values (1-sigma) for δ(2)H measurements on water and caffeine samples of better than 1.0 and 0.5 mUr, respectively. To overcome handling problems with water as the principal calibration anchor for hydrogen isotopic measurements, we have employed an effective and simple strategy using reference waters or other liquids sealed in silver-tube segments. These crimped silver tubes can be employed in both the Cr-EA and TC/EA techniques. They simplify considerably the normalization of hydrogen-isotope measurement data to the VSMOW-SLAP (Vienna Standard Mean Ocean Water-Standard Light Antarctic Precipitation) scale, and their use improves accuracy of the data by eliminating evaporative loss and associated isotopic fractionation while

  3. Nanomechanical IR Spectroscopy for the fast analysis of picogram samples of engineered nanomaterials

    DEFF Research Database (Denmark)

    Andersen, Alina Joukainen; Ek, Pramod Kumar; Andresen, Thomas Lars

    2014-01-01

    The proliferation of engineered nanomaterials (ENMs), e.g. in nanomedicine, demands for novel sensitive techniques allowing for the analysis of minute samples. We present nanoelectromechanical system-based IR spectroscopy (NEMS-IR) of picograms of polymeric micelles. The micelles are nebulized...

  4. Trace element analysis at the Livermore pool-type reactor using neutron activation techniques

    International Nuclear Information System (INIS)

    Ragaini, R.C.; Ralston, R.; Garvis, D.

    1975-01-01

    The capabilities of trace element analysis at the Livermore Pool-Type Reactor (LPTR) using instrumental neutron activation analysis (INAA) are discussed. A description is given of the technology and the methods employed, including sample preparation, irradiation, and analysis. Applications of the INAA technique in past and current projects are described. A computer program, GAMANAL, has been used for nuclide identification and quantification. (U.S.)

  5. Laser-induced breakdown spectroscopy for the real-time analysis of mixed waste samples containing Sr

    International Nuclear Information System (INIS)

    Barefield, J.E. II; Koskelo, A.C.; Multari, R.A.; Cremers, D.A.; Gamble, T.K.; Han, C.Y.

    1995-01-01

    In this report, the use of Laser-induced breakdown spectroscopy to analyze mixed waste samples containing Sr is discussed. The mixed waste samples investigated include vitrified waste glass and contaminated soil. Compared to traditional analysis techniques, the laser-based method is fast (i.e., analysis times on the order of minutes) and essentially waste free since little or no sample preparation is required. Detection limits on the order of pmm Sr were determined. Detection limits obtained using a fiber optic cable to deliver laser pulses to soil samples containing Cr, Zr, Pb, Be, Cu, and Ni will also be discussed

  6. TRAN-STAT: statistics for environmental studies, Number 22. Comparison of soil-sampling techniques for plutonium at Rocky Flats

    International Nuclear Information System (INIS)

    Gilbert, R.O.; Bernhardt, D.E.; Hahn, P.B.

    1983-01-01

    A summary of a field soil sampling study conducted around the Rocky Flats Colorado plant in May 1977 is preseted. Several different soil sampling techniques that had been used in the area were applied at four different sites. One objective was to comparethe average 239 - 240 Pu concentration values obtained by the various soil sampling techniques used. There was also interest in determining whether there are differences in the reproducibility of the various techniques and how the techniques compared with the proposed EPA technique of sampling to 1 cm depth. Statistically significant differences in average concentrations between the techniques were found. The differences could be largely related to the differences in sampling depth-the primary physical variable between the techniques. The reproducibility of the techniques was evaluated by comparing coefficients of variation. Differences between coefficients of variation were not statistically significant. Average (median) coefficients ranged from 21 to 42 percent for the five sampling techniques. A laboratory study indicated that various sample treatment and particle sizing techniques could increase the concentration of plutonium in the less than 10 micrometer size fraction by up to a factor of about 4 compared to the 2 mm size fraction

  7. An Electromagnetic Gauge Technique for Measuring Shocked Particle Velocity in Electrically Conductive Samples

    Science.gov (United States)

    Cheng, David; Yoshinaka, Akio

    2014-11-01

    Electromagnetic velocity (EMV) gauges are a class of film gauges which permit the direct in-situ measurement of shocked material flow velocity. The active sensing element, typically a metallic foil, requires exposure to a known external magnetic field in order to produce motional electromotive force (emf). Due to signal distortion caused by mutual inductance between sample and EMV gauge, this technique is typically limited to shock waves in non-conductive materials. In conductive samples, motional emf generated in the EMV gauge has to be extracted from the measured signal which results from the combined effects of both motional emf and voltage changes from induced currents. An electromagnetic technique is presented which analytically models the dynamics of induced current between a copper disk moving as a rigid body with constant 1D translational velocity toward an EMV gauge, where both disk and gauge are exposed to a uniform external static magnetic field. The disk is modelled as a magnetic dipole loop where its Foucault current is evaluated from the characteristics of the fields, whereas the EMV gauge is modelled as a circuit loop immersed in the field of the magnetic dipole loop, the intensity of which is calculated as a function of space and, implicitly, time. Equations of mutual induction are derived and the current induced in the EMV gauge loop is solved, allowing discrimination of the motional emf. Numerical analysis is provided for the step response of the induced EMV gauge current with respect to the Foucault current in the moving copper sample.

  8. Heavy metal analysis in groundwater samples by SR-TXRF

    International Nuclear Information System (INIS)

    Moreira, Silvana; Ficaris, Maria; Vives, Ana Elisa S. de; Zucchi, Orgheda L.A.D.; Nascimento Filho, Virgilio Franco do Centro de Energia Nuclear na Agricultura , Piracicaba, SP . Lab. Instrumentacao Nuclear.; Brazil)

    2005-01-01

    In order to obtain information about levels of heavy metals in groundwater, analysis were carried out on samples from monitoring and supplying wells located in Campinas, Sao Paulo State, Southeastern Brazil. The analytical technique used was Synchrotron Radiation Total Reflection X-Ray Fluorescence (SR-TXRF) and all the measurements were performed at Synchrotron Light Source Laboratory, using a white beam and a Si(Li) detector in total reflection condition. The determined elements were Al, Cr, Mn, Fe, Ni, Cu, Zn, Ba and Pb. The results were compared with the maximum allowed values (MPV) established by the Brazilian Health Department. The detection limits obtained varying from 0.10 up to 8 μg.L -1 were in agreement with the values presented by others analytical techniques. (author)

  9. Heavy metal analysis in groundwater samples by SR-TXRF

    Energy Technology Data Exchange (ETDEWEB)

    Moreira, Silvana; Ficaris, Maria [Universidade Estadual de Campinas, SP (Brazil). Faculdade de Engenharia Civil, Arquitetura e Urbanismo. Dept. de Recursos Hidricos]. E-mail: silvana@fec.unicamp.br; Vives, Ana Elisa S. de [Universidade Metodista de Piracicaba (UNIMEP), Santa Barbara D' Oeste, SP (Brazil). Faculdade de Engenharia, Arquitetura e Urbanismo]. E-mail: aesvives@unimep.br; Zucchi, Orgheda L.A.D. [Sao Paulo Univ., Ribeirao Preto, SP (Brazil). Faculdade de Ciencias Farmaceuticas]. E-mail: olzucchi@fcfrp.usp.br; Nascimento Filho, Virgilio Franco do [Centro de Energia Nuclear na Agricultura (CENA), Piracicaba, SP (Brazil). Lab. Instrumentacao Nuclear]. E-mail: virgilio@cena.usp.br

    2005-07-01

    In order to obtain information about levels of heavy metals in groundwater, analysis were carried out on samples from monitoring and supplying wells located in Campinas, Sao Paulo State, Southeastern Brazil. The analytical technique used was Synchrotron Radiation Total Reflection X-Ray Fluorescence (SR-TXRF) and all the measurements were performed at Synchrotron Light Source Laboratory, using a white beam and a Si(Li) detector in total reflection condition. The determined elements were Al, Cr, Mn, Fe, Ni, Cu, Zn, Ba and Pb. The results were compared with the maximum allowed values (MPV) established by the Brazilian Health Department. The detection limits obtained varying from 0.10 up to 8 {mu}g.L{sup -1} were in agreement with the values presented by others analytical techniques. (author)

  10. Comparison of analysis techniques by liquid scintillation and Cerenkov Effect for 40K quantification in aqueous samples

    International Nuclear Information System (INIS)

    Miranda C, L.; Davila R, J. I.; Lopez del R, H.; Mireles G, F.

    2015-09-01

    In this work the counting by liquid scintillation and Cerenkov Effect to quantify 40 K in aqueous samples was used. The performance of both techniques was studied by comparing the response of three commercial liquid scintillation OptiPhase HiSafe 3, Ultima Gold Ab and OptiPhase TriSafe, the vial type and presentation conditions of the sample for counting. In liquid scintillation, the ability to form homogeneous mixtures depended on the ionic strength of the aqueous solutions. The scintillator OptiPhase HiSafe 3 showed a greater charge capacity for solutions with high ionic strength (<3.4), while the scintillator OptiSafe TriSafe no form homogeneous mixtures for solutions of ionic strength higher than 0.3. Counting efficiencies for different proportions of sample and scintillator near 100% for the scintillators OptiSafe HiSafe 3 and Ultima Gold Ab were obtained. In the counting by Cerenkov Effect, the efficiency and sensitivity depended of the vial type; polyethylene vials were more suitable for counting that the glass vials. The sample volume had not significant effect on counting efficiency, obtaining an average value of 44.8% for polyethylene vials and 37.3% for glass vials. Therefore, the liquid scintillation was more efficient and sensitive for the measurement of 40 K in aqueous solutions. (Author)

  11. Elemental analysis of biological materials. Current problems and techniques with special reference to trace elements

    International Nuclear Information System (INIS)

    1980-01-01

    Selected techniques were reviewed for the assay of trace and minor elements in biological materials. Other relevant information is also presented on the need for such analyses, sampling, sample preparation and analytical quality control. In order to evaluate and compare the applicability of the various analytical techniques on a meaningful and objective basis, the materials chosen for consideration were intended to be typical of a wide range of biological matrics of different elemental compositions, namely Bowen's kale, representing a plant material, and NBS bovine liver, IAEA animal muscle, and blood serum, representing animal tissues. The subject is reviewed under the following headings: on the need for trace element analyses in the life sciences (4 papers); sampling and sample preparation for trace element analysis (2 papers); analytical techniques for trace and minor elements in biological materials (7 papers); analytical quality control (2 papers)

  12. Direct analysis of radionuclides-96 samples simultaneously

    International Nuclear Information System (INIS)

    Kessler, M.J.

    1991-01-01

    Recently, there has been a tremendous interest in two areas of concern in nuclear counting and radioactivity waste disposal. The first is the reduction of radioactive waste, in particular the reduction in the amount of or the development of environmentally safe scintillation cocktails. The second is the development of a simple method of quantitating large numbers of samples (thousands/day) in a short period of time (minutes). These two areas of concern have been addressed with the development of the Matrix 96 direct beta counter. This new instrumental technique is capable of quantitating 96 samples simultaneously in the microplate format (8 x 12, 96 sample) on a solid support WITHOUT the use of any cocktails, vials, and is non-destructive to the sample. The use of this technique for the following biomedical applications, DNA dot blots, cell proliferation (3H thymidine), receptor binding, chromium cytotoxicity assays, and protein assays will be discussed in detail. The data from both the conventional beta and gamma counter will be correlated and compared to the new Matrix 96 direct beta counter. This new technique provides a convenient method of addressing the concerns of reducing radioactive waste and provides a method of quantitating a large number of samples, accurately in a short period of time (96 at a time)

  13. Analysis of monazite samples

    International Nuclear Information System (INIS)

    Kartiwa Sumadi; Yayah Rohayati

    1996-01-01

    The 'monazit' analytical program has been set up for routine work of Rare Earth Elements analysis in the monazite and xenotime minerals samples. Total relative error of the analysis is very low, less than 2.50%, and the reproducibility of counting statistic and stability of the instrument were very excellent. The precision and accuracy of the analytical program are very good with the maximum percentage relative are 5.22% and 1.61%, respectively. The mineral compositions of the 30 monazite samples have been also calculated using their chemical constituents, and the results were compared to the grain counting microscopic analysis

  14. Data analysis for steam generator tubing samples

    International Nuclear Information System (INIS)

    Dodd, C.V.

    1996-07-01

    The objective of the Improved Eddy-Current ISI for Steam Generators program is to upgrade and validate eddy-current inspections, including probes, instrumentation, and data processing techniques for inservice inspection of new, used, and repaired steam generator tubes; to improve defect detection, classification and characterization as affected by diameter and thickness variations, denting, probe wobble, tube sheet, tube supports, copper and sludge deposits, even when defect types and other variables occur in combination; to transfer this advanced technology to NRC's mobile NDE laboratory and staff. This report provides a description of the application of advanced eddy-current neural network analysis methods for the detection and evaluation of common steam generator tubing flaws including axial and circumferential outer-diameter stress-corrosion cracking and intergranular attack. The report describes the training of the neural networks on tubing samples with known defects and the subsequent evaluation results for unknown samples. Evaluations were done in the presence of artifacts. Computer programs are given in the appendix

  15. Fingerprint elements scatter analysis on ancient chinese Ru porcelains samples

    International Nuclear Information System (INIS)

    Gao Zhengyao; Wang Jie; Chen Xiande

    1997-01-01

    Altogether 28 samples, mainly including glazes and bodies of ancient Chinese Ru porcelain, were analyzed by NAA technique and the contents of 36 elements were compared. The scatter analysis for nine fingerprint-elements indicates that almost all ancient Chinese Ru porcelain samples had nearly identical and long-term stable source of raw materials although they were fired in different kilns, at varying time and with distinct colors, and moreover, the source of raw materials for modern Ru porcelain seems to approach that for ancient one. The close provenance relation between ancient Jun porcelain and ancient Ru porcelain is also preliminarily verified. The glaze material of Jingdezhen white porcelain is totally different from all other samples. It shows that the former came from a separate source

  16. Recent advances in sample preparation techniques and methods of sulfonamides detection - A review.

    Science.gov (United States)

    Dmitrienko, Stanislava G; Kochuk, Elena V; Apyari, Vladimir V; Tolmacheva, Veronika V; Zolotov, Yury A

    2014-11-19

    Sulfonamides (SAs) have been the most widely used antimicrobial drugs for more than 70 years, and their residues in foodstuffs and environmental samples pose serious health hazards. For this reason, sensitive and specific methods for the quantification of these compounds in numerous matrices have been developed. This review intends to provide an updated overview of the recent trends over the past five years in sample preparation techniques and methods for detecting SAs. Examples of the sample preparation techniques, including liquid-liquid and solid-phase extraction, dispersive liquid-liquid microextraction and QuEChERS, are given. Different methods of detecting the SAs present in food and feed and in environmental, pharmaceutical and biological samples are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Biomonitoring of air pollution in Jamaica through trace-element analysis of epiphytic plants using nuclear and related analytical techniques

    International Nuclear Information System (INIS)

    Vutchkov, Mitko

    2001-01-01

    The main goal of the Coordinated Research Project (No:9937/R0), entitled 'Biomonitoring of Air Pollution in Jamaica Through Trace-Element Analysis of Epiphytic Plants Using Nuclear and Related Analytical Techniques', is to identify and validate site specific epiphytic plants for biomonitoring the atmospheric pollution in Jamaica using nuclear analytical techniques at the International Centre for Environmental and Nuclear Sciences (ICENS). The specific objectives for the second year of the project were: Development of HOP for sampling epiphytic plants in Jamaica; Sampling design and sample collection; Sample preparation and analysis; Development of an in-house SRM and participation in the NAT-5 inter-laboratory study; Data analysis and interpretation of the results; Development of a work plan of the third year of the project

  18. PIXE analysis of Nigerian flour and bread samples

    Energy Technology Data Exchange (ETDEWEB)

    Olise, Felix S., E-mail: felix_olise@rushpost.com [Department of Physics, Obafemi Awolowo University, Ile-Ife 220005 (Nigeria); Fernandes, Adriana M.; Cristina Chaves, P. [CFA: Centro de Física Atómica da Universidade de Lisboa, Av. Prof. Gama Pinto 2, 1649-003 Lisboa (Portugal); Taborda, Ana; Reis, Miguel A. [IST/CTN: Instituto Superior Técnico, Universidade Técnica de Lisboa, Campus Tecnológico e Nuclear (CTN), EN10, 2686-953 Sacavém (Portugal); CFA: Centro de Física Atómica da Universidade de Lisboa, Av. Prof. Gama Pinto 2, 1649-003 Lisboa (Portugal)

    2014-01-01

    Highlights: • The PIXE technique has been used to determine K and Br in a major Nigerian food item. • Samples were analysed using two proton beam energies, namely 1.25 MeV and 2.15 MeV. • Mismatched Ca results reflect its nature and accuracy/precision of the procedure. • Explanations for the presence of the contaminant in the samples are presented. • Other sources originating from erroneous burning of dangerous products suspected. -- Abstract: The alleged use of potassium bromate (KBrO{sub 3}) in bread baking led a few authors to report on the chemical methods for the determination of KBrO{sub 3} levels in bread. In order to examine the potentials of a non chemical particle induced X-ray emission (PIXE) method for this purpose, six sets of samples, each composed of flour, dough and bread from a production batch were analysed. The samples were obtained from six different bakers of bread at Ile-Ife, Nigeria. The flour samples were air-dried while others were freeze dried at about −16 °C. The samples were homogenised in an agate mortar and then pelletised. Samples were analysed at the CTN standard PIXE setup and standard procedures for thick target samples analysis were followed. In some samples significant concentrations of bromine were found. In the present work we present possible explanations for the presence of this potentially dangerous contaminant in the samples.

  19. PIXE analysis of Nigerian flour and bread samples

    International Nuclear Information System (INIS)

    Olise, Felix S.; Fernandes, Adriana M.; Cristina Chaves, P.; Taborda, Ana; Reis, Miguel A.

    2014-01-01

    Highlights: • The PIXE technique has been used to determine K and Br in a major Nigerian food item. • Samples were analysed using two proton beam energies, namely 1.25 MeV and 2.15 MeV. • Mismatched Ca results reflect its nature and accuracy/precision of the procedure. • Explanations for the presence of the contaminant in the samples are presented. • Other sources originating from erroneous burning of dangerous products suspected. -- Abstract: The alleged use of potassium bromate (KBrO 3 ) in bread baking led a few authors to report on the chemical methods for the determination of KBrO 3 levels in bread. In order to examine the potentials of a non chemical particle induced X-ray emission (PIXE) method for this purpose, six sets of samples, each composed of flour, dough and bread from a production batch were analysed. The samples were obtained from six different bakers of bread at Ile-Ife, Nigeria. The flour samples were air-dried while others were freeze dried at about −16 °C. The samples were homogenised in an agate mortar and then pelletised. Samples were analysed at the CTN standard PIXE setup and standard procedures for thick target samples analysis were followed. In some samples significant concentrations of bromine were found. In the present work we present possible explanations for the presence of this potentially dangerous contaminant in the samples

  20. Comparison of Two Surface Contamination Sampling Techniques Conducted for the Characterization of Two Pajarito Site Manhattan Project National Historic Park Properties

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, Tammy Ann [Montana Tech of the Univ. of Montana, Butte, MT (United States); Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2016-07-29

    Technical Area-18 (TA-18), also known as Pajarito Site, is located on Los Alamos National Laboratory property and has historic buildings that will be included in the Manhattan Project National Historic Park. Characterization studies of metal contamination were needed in two of the four buildings that are on the historic registry in this area, a “battleship” bunker building (TA-18-0002) and the Pond cabin (TA-18-0029). However, these two buildings have been exposed to the elements, are decades old, and have porous and rough surfaces (wood and concrete). Due to these conditions, it was questioned whether standard wipe sampling would be adequate to detect surface dust metal contamination in these buildings. Thus, micro-vacuum and surface wet wipe sampling techniques were performed side-by-side at both buildings and results were compared statistically. A two-tail paired t-test revealed that the micro-vacuum and wet wipe techniques were statistically different for both buildings. Further mathematical analysis revealed that the wet wipe technique picked up more metals from the surface than the microvacuum technique. Wet wipes revealed concentrations of beryllium and lead above internal housekeeping limits; however, using an yttrium normalization method with linear regression analysis between beryllium and yttrium revealed a correlation indicating that the beryllium levels were likely due to background and not operational contamination. PPE and administrative controls were implemented for National Park Service (NPS) and Department of Energy (DOE) tours as a result of this study. Overall, this study indicates that the micro-vacuum technique may not be an efficient technique to sample for metal dust contamination.

  1. Analysis of Cultural Heritage by Accelerator Techniques and Analytical Imaging

    Science.gov (United States)

    Ide-Ektessabi, Ari; Toque, Jay Arre; Murayama, Yusuke

    2011-12-01

    In this paper we present the result of experimental investigation using two very important accelerator techniques: (1) synchrotron radiation XRF and XAFS; and (2) accelerator mass spectrometry and multispectral analytical imaging for the investigation of cultural heritage. We also want to introduce a complementary approach to the investigation of artworks which is noninvasive and nondestructive that can be applied in situ. Four major projects will be discussed to illustrate the potential applications of these accelerator and analytical imaging techniques: (1) investigation of Mongolian Textile (Genghis Khan and Kublai Khan Period) using XRF, AMS and electron microscopy; (2) XRF studies of pigments collected from Korean Buddhist paintings; (3) creating a database of elemental composition and spectral reflectance of more than 1000 Japanese pigments which have been used for traditional Japanese paintings; and (4) visible light-near infrared spectroscopy and multispectral imaging of degraded malachite and azurite. The XRF measurements of the Japanese and Korean pigments could be used to complement the results of pigment identification by analytical imaging through spectral reflectance reconstruction. On the other hand, analysis of the Mongolian textiles revealed that they were produced between 12th and 13th century. Elemental analysis of the samples showed that they contained traces of gold, copper, iron and titanium. Based on the age and trace elements in the samples, it was concluded that the textiles were produced during the height of power of the Mongol empire, which makes them a valuable cultural heritage. Finally, the analysis of the degraded and discolored malachite and azurite demonstrates how multispectral analytical imaging could be used to complement the results of high energy-based techniques.

  2. Symbol synchronization and sampling frequency synchronization techniques in real-time DDO-OFDM systems

    Science.gov (United States)

    Chen, Ming; He, Jing; Cao, Zizheng; Tang, Jin; Chen, Lin; Wu, Xian

    2014-09-01

    In this paper, we propose and experimentally demonstrate a symbol synchronization and sampling frequency synchronization techniques in real-time direct-detection optical orthogonal frequency division multiplexing (DDO-OFDM) system, over 100-km standard single mode fiber (SSMF) using a cost-effective directly modulated distributed feedback (DFB) laser. The experiment results show that the proposed symbol synchronization based on training sequence (TS) has a low complexity and high accuracy even at a sampling frequency offset (SFO) of 5000-ppm. Meanwhile, the proposed pilot-assisted sampling frequency synchronization between digital-to-analog converter (DAC) and analog-to-digital converter (ADC) is capable of estimating SFOs with an accuracy of technique can also compensate SFO effects within a small residual SFO caused by deviation of SFO estimation and low-precision or unstable clock source. The two synchronization techniques are suitable for high-speed DDO-OFDM transmission systems.

  3. Quantitative mineralogical analysis of sandstones using x-ray diffraction techniques

    International Nuclear Information System (INIS)

    Ward, C.R.; Taylor, J.C.

    1999-01-01

    Full text: X-ray diffraction has long been used as a definitive technique for mineral identification based on the measuring the internal atomic or crystal structures present in powdered rocks; soils and other mineral mixtures. Recent developments in data gathering and processing, however, have provided an improved basis for its use as a quantitative tool, determining not only the nature of the minerals but also the relative proportions of the different minerals present. The mineralogy of a series of sandstone samples from the Sydney and Bowen Basins of eastern Australia has been evaluated by X-ray diffraction (XRD) on a quantitative basis using the Australian-developed SIROQUANT data processing technique. Based on Rietveld principles, this technique generates a synthetic X-ray diffractogram by adjusting and combining full-profile patterns of minerals nominated as being present in the sample and interactively matches the synthetic diffractogram under operator instructions to the observed diffractogram of the sample being analysed. The individual mineral patterns may be refined in the process, to allow for variations in crystal structure of individual components or for factors such as preferred orientation in the sample mount. The resulting output provides mass percentages of the different minerals in the mixture, and an estimate of the error associated with each individual percentage determination. The chemical composition of the mineral mixtures indicated by SIROQUANT for each individual sandstone studied was estimated using a spreadsheet routine, and the indicated proportion of each oxide in each sample compared to the actual chemical analysis of the same sandstone as determined independently by X-ray fluorescence spectrometry. The results show a high level of agreement for all major chemical constituents, indicating consistency between the SIROQUANT XRD data and the whole-rock chemical composition. Supplementary testing with a synthetic corundum spike further

  4. Application of functional analysis techniques to supervisory systems

    International Nuclear Information System (INIS)

    Lambert, Manuel; Riera, Bernard; Martel, Gregory

    1999-01-01

    The aim of this paper is to apply firstly two interesting functional analysis techniques for the design of supervisory systems for complex processes, and secondly to discuss the strength and the weaknesses of each of them. Two functional analysis techniques have been applied, SADT (Structured Analysis and Design Technique) and FAST (Functional Analysis System Technique) on a process, an example of a Water Supply Process Control (WSPC) system. These techniques allow a functional description of industrial processes. The paper briefly discusses the functions of a supervisory system and some advantages of the application of functional analysis for the design of a 'human' centered supervisory system. Then the basic principles of the two techniques applied on the WSPC system are presented. Finally, the different results obtained from the two techniques are discussed

  5. Evaluation of nitrate quantification techniques for in-line analysis in drinking water

    International Nuclear Information System (INIS)

    Hernandez Alpizar, Laura; Coy Herrera, Ricardo

    2015-01-01

    The results of a study are presented to determine the potential use of four techniques for the quantification of nitrates in continuous sampling: ion chromatography, ultraviolet absorption spectrophotometry; one table equipment and two mini-spectrophotometers with continuous flow sample injection are used, one for measurements in the field of visible radiation and the other optimized for measurements of ultraviolet radiation absorption. Variables that are considered: reagent and accessory consumption, waste toxicity, analyte response, detection limit (LD), quantification limit (LC), linearity in the field of interest and sensitivity. Ultraviolet absorption detection spectro photometry with continuous flow sample injection is the best of the techniques for line analysis. The response has been between 0-10 mg / L linear, data recommended by WHO for the concentration of nitrates in drinking water. Low consumption of reagents and accessories is shown. This spectrophotometry without hazardous waste generated, has had LD 0.002 mg / L and LC 0.006 mg / L and an adequate sensitivity to respond rapidly to the concentration of the analyte without signal saturation. The desirable characteristics are fulfilled for an on-line analysis system. (author) [es

  6. Neutron activation analysis of geochemical samples

    International Nuclear Information System (INIS)

    Rosenberg, R.; Zilliacus, R.; Kaistila, M.

    1983-06-01

    The present paper will describe the work done at the Technical Research Centre of Finland in developing methods for the large-scale activation analysis of samples for the geochemical prospecting of metals. The geochemical prospecting for uranium started in Finland in 1974 and consequently a manually operated device for the delayed neutron activation analysis of uranium was taken into use. During 1974 9000 samples were analyzed. The small capacity of the analyzer made it necessary to develop a completely automated analyzer which was taken into use in August 1975. Since then 20000-30000 samples have been analyzed annually the annual capacity being about 60000 samples when running seven hours per day. Multielemental instrumental neutron activation analysis is used for the analysis of more than 40 elements. Using instrumental epithermal neutron activation analysis 25-27 elements can be analyzed using one irradiation and 20 min measurement. During 1982 12000 samples were analyzed for mining companies and Geological Survey of Finland. The capacity is 600 samples per week. Besides these two analytical methods the analysis of lanthanoids is an important part of the work. 11 lanthanoids have been analyzed using instrumental neutron activation analysis. Radiochemical separation methods have been developed for several elements to improve the sensitivity of the analysis

  7. Application of WSP method in analysis of environmental samples

    International Nuclear Information System (INIS)

    Stacho, M.; Slugen, V.; Hinca, R.; Sojak, S.; Krnac, S.

    2014-01-01

    Detection of activity in natural samples is specific especially because of its low level and high background interferences. Reduction of background interferences could be reached using low background chamber. Measurement geometry in shape of Marinelli beaker is commonly used according to low level of activity in natural samples. The Peak Net Area (PNA) method is the world-wide accepted technique for analysis of gamma-ray spectra. It is based on the net area calculation of the full energy peak, therefore, it takes into account only a fraction of measured gamma-ray spectrum. On the other hand, the Whole Spectrum Processing (WSP) approach to the gamma analysis makes possible to use entire information being in the spectrum. This significantly raises efficiency and improves energy resolution of the analysis. A principal step for the WSP application is building up the suitable response operator. Problems are put in an appearance when suitable standard calibration sources are unavailable. It may be occurred in the case of large volume samples and/or in the analysis of high energy range. Combined experimental and mathematical calibration may be a suitable solution. Many different detectors have been used to register the gamma ray and its energy. HPGe detectors produce the highest resolution commonly available today. Therefore they are they the most often used detectors in natural samples activity analysis. Scintillation detectors analysed using PNA method could be also used in simple cases, but for complicated spectra are practically inapplicable. WSP approach improves resolution of scintillation detectors and expands their applicability. WSP method allowed significant improvement of the energetic resolution and separation of "1"3"7Cs 661 keV peak from "2"1"4Bi 609 keV peak. At the other hand the statistical fluctuations in the lower part of the spectrum highlighted by background subtraction causes that this part is still not reliably analyzable. (authors)

  8. Neutron-activation analysis of routine mineral-processing samples

    International Nuclear Information System (INIS)

    Watterson, J.; Eddy, B.; Pearton, D.

    1974-01-01

    Instrumental neutron-activation analysis was applied to a suite of typical mineral-processing samples to establish which elements can be rapidly determined in them by this technique. A total of 35 elements can be determined with precisions (from the counting statistics) ranging from better than 1 per cent to approximately 20 per cent. The elements that can be determined have been tabulated together with the experimental conditions, the precision from the counting statistics, and the estimated number of analyses possible per day. With an automated system, this number can be as high as 150 in the most favourable cases [af

  9. Analysis of U and Pu resin bead samples with a single stage mass spectrometer

    International Nuclear Information System (INIS)

    Smith, D.H.; Walker, R.L.; Bertram, L.K.; Carter, J.A.

    1979-01-01

    Resin bead sampling enables the shipment of nanogram U and Pu quantities for analysis. Application of this sampling technique to safeguards was investigated with a single-stage mass spectrometer. Standards gave results in good agreement with NBS certified values. External precisions of +-0.5% were obtained on isotopic ratios of approx. 0.01; precisions on quantitative measurements are +-1.0%

  10. Measuring Sulfur Isotope Ratios from Solid Samples with the Sample Analysis at Mars Instrument and the Effects of Dead Time Corrections

    Science.gov (United States)

    Franz, H. B.; Mahaffy, P. R.; Kasprzak, W.; Lyness, E.; Raaen, E.

    2011-01-01

    The Sample Analysis at Mars (SAM) instrument suite comprises the largest science payload on the Mars Science Laboratory (MSL) "Curiosity" rover. SAM will perform chemical and isotopic analysis of volatile compounds from atmospheric and solid samples to address questions pertaining to habitability and geochemical processes on Mars. Sulfur is a key element of interest in this regard, as sulfur compounds have been detected on the Martian surface by both in situ and remote sensing techniques. Their chemical and isotopic composition can belp constrain environmental conditions and mechanisms at the time of formation. A previous study examined the capability of the SAM quadrupole mass spectrometer (QMS) to determine sulfur isotope ratios of SO2 gas from a statistical perspective. Here we discuss the development of a method for determining sulfur isotope ratios with the QMS by sampling SO2 generated from heating of solid sulfate samples in SAM's pyrolysis oven. This analysis, which was performed with the SAM breadboard system, also required development of a novel treatment of the QMS dead time to accommodate the characteristics of an aging detector.

  11. Development of core sampling technique for ITER Type B radwaste

    Energy Technology Data Exchange (ETDEWEB)

    Kim, S. G.; Hong, K. P.; Oh, W. H.; Park, M. C.; Jung, S. H.; Ahn, S. B. [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2016-10-15

    Type B radwaste (intermediate level and long lived radioactive waste) imported from ITER vacuum vessel are to be treated and stored in basement of hot cell building. The Type B radwaste treatment process is composed of buffer storage, cutting, sampling/tritium measurement, tritium removal, characterization, pre-packaging, inspection/decontamination, and storage etc. The cut slices of Type B radwaste components generated from cutting process undergo sampling process before and after tritium removal process. The purpose of sampling is to obtain small pieces of samples in order to investigate the tritium content and concentration of Type B radwaste. Core sampling, which is the candidates of sampling technique to be applied to ITER hot cell, is available for not thick (less than 50 mm) metal without use of coolant. Experimented materials were SS316L and CuCrZr in order to simulate ITER Type B radwaste. In core sampling, substantial secondary wastes from cutting chips will be produced unavoidably. Thus, core sampling machine will have to be equipped with disposal system such as suction equipment. Core sampling is considered an unfavorable method for tool wear compared to conventional drilling.

  12. Non-destructive high-resolution thermal imaging techniques to evaluate wildlife and delicate biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Lavers, C; Franklin, P; Franklin, P; Plowman, A; Sayers, G; Bol, J; Shepard, D; Fields, D, E-mail: brnc-radarcomms1@nrta.mod.u [Sensors Team, Plymouth University at Britannia Royal Naval College, Dartmouth, Devon (United Kingdom) and Paignton Zoological Park, Paignton, Devon (United Kingdom); Thermal Wave Imaging, Inc., 845 Livernoise St, Ferndale, MI (United States); Buckfast Butterfly and Otter Sanctuary, Buckfast, Devon (United Kingdom)

    2009-07-01

    Thermal imaging cameras now allows routine monitoring of dangerous yet endangered wildlife in captivity. This study looks at the potential applications of radiometrically calibrated thermal data to wildlife, as well as providing parameters for future materials applications. We present a non-destructive active testing technique suitable for enhancing imagery contrast of thin or delicate biological specimens yielding improved thermal contrast at room temperature, for analysis of sample thermal properties. A broad spectrum of animals is studied with different textured surfaces, reflective and emissive properties in the infra red part of the electromagnetic spectrum. Some surface features offer biomimetic materials design opportunities.

  13. Non-destructive high-resolution thermal imaging techniques to evaluate wildlife and delicate biological samples

    International Nuclear Information System (INIS)

    Lavers, C; Franklin, P; Franklin, P; Plowman, A; Sayers, G; Bol, J; Shepard, D; Fields, D

    2009-01-01

    Thermal imaging cameras now allows routine monitoring of dangerous yet endangered wildlife in captivity. This study looks at the potential applications of radiometrically calibrated thermal data to wildlife, as well as providing parameters for future materials applications. We present a non-destructive active testing technique suitable for enhancing imagery contrast of thin or delicate biological specimens yielding improved thermal contrast at room temperature, for analysis of sample thermal properties. A broad spectrum of animals is studied with different textured surfaces, reflective and emissive properties in the infra red part of the electromagnetic spectrum. Some surface features offer biomimetic materials design opportunities.

  14. 3D-Laser-Scanning Technique Applied to Bulk Density Measurements of Apollo Lunar Samples

    Science.gov (United States)

    Macke, R. J.; Kent, J. J.; Kiefer, W. S.; Britt, D. T.

    2015-01-01

    In order to better interpret gravimetric data from orbiters such as GRAIL and LRO to understand the subsurface composition and structure of the lunar crust, it is import to have a reliable database of the density and porosity of lunar materials. To this end, we have been surveying these physical properties in both lunar meteorites and Apollo lunar samples. To measure porosity, both grain density and bulk density are required. For bulk density, our group has historically utilized sub-mm bead immersion techniques extensively, though several factors have made this technique problematic for our work with Apollo samples. Samples allocated for measurement are often smaller than optimal for the technique, leading to large error bars. Also, for some samples we were required to use pure alumina beads instead of our usual glass beads. The alumina beads were subject to undesirable static effects, producing unreliable results. Other investigators have tested the use of 3d laser scanners on meteorites for measuring bulk volumes. Early work, though promising, was plagued with difficulties including poor response on dark or reflective surfaces, difficulty reproducing sharp edges, and large processing time for producing shape models. Due to progress in technology, however, laser scanners have improved considerably in recent years. We tested this technique on 27 lunar samples in the Apollo collection using a scanner at NASA Johnson Space Center. We found it to be reliable and more precise than beads, with the added benefit that it involves no direct contact with the sample, enabling the study of particularly friable samples for which bead immersion is not possible

  15. Lead isotope ratio analysis of bullet samples by using quadrupole ICP-MS

    International Nuclear Information System (INIS)

    Tamura, Shu-ichi; Hokura, Akiko; Nakai, Izumi; Oishi, Masahiro

    2006-01-01

    The measurement conditions for the precise analysis of the lead stable isotope ratio by using an ICP-MS equipped with a quadrupole mass spectrometer were studied in order to apply the technique to the forensic identification of bullet samples. The values of the relative standard deviation obtained for the ratio of 208 Pb/ 206 Pb, 207 Pb/ 206 Pb and 204 Pb/ 206 Pb were lower than 0.2% after optimization of the analytical conditions, including the optimum lead concentration of the sample solution to be about 70 ppb and an integration time for 1 m/s of 15 s. This method was applied to an analysis of lead in bullets for rifles and handguns; a stable isotope ratio of lead was found to be suitable for the identification of bullets. This study has demonstrated that the lead isotope ratio measured by using a quadrupole ICP-MS was useful for a practical analysis of bullet samples in forensic science. (author)

  16. Water stable isotope measurements of Antarctic samples by means of IRMS and WS-CRDS techniques

    Science.gov (United States)

    Michelini, Marzia; Bonazza, Mattia; Braida, Martina; Flora, Onelio; Dreossi, Giuliano; Stenni, Barbara

    2010-05-01

    of the sample in the box. In the WS-CRDS the path of laser is longer, producing higher-sensitivity measurements. The instrument is paired with an autosampler and can be used without it and the vaporizer to analyze directly the isotopic composition of the water vapour in the atmosphere. In addition, the instrument can be moved from the laboratory and also used for outdoor measurements. The more important improvements over traditional IRMS techniques are that WS-CRDS needs less sample in order to perform the analysis (water equilibration techniques) and the analyses are faster. Coversely, memory effects may affect the measurements so there is the need to increase the number of injection to have a high precision measurement. The laboratory of Isotope Geochemistry of the Department of Geosciences has recently acquired a WS-CRDS system from PICARRO. The isotopic data obtained with this new method have been compared with the ones obtained by means of IRMS methods. An HDO device coupled with a Thermo Finnigan Delta Plus Advantage mass spectrometer has been used, using the well know CO2 and H2/water equilibration technique. At the moment of the writing of the abstract the mean difference between the values obtained using PICARRO and using the traditional IRMS method is of the order of 0.1 per mil for the ratio 18O/16O and 1.00 per mil for the ratio D/H, but further measurements are currently underway. O'Keef A., Deacon D.A.G., 1988. Cavity ring-down optical spectrometer for absorption measurements using pulsed laser sources, Rev. Sci. Instrum., 59, 2544.

  17. A comparison of approximation techniques for variance-based sensitivity analysis of biochemical reaction systems

    Directory of Open Access Journals (Sweden)

    Goutsias John

    2010-05-01

    Full Text Available Abstract Background Sensitivity analysis is an indispensable tool for the analysis of complex systems. In a recent paper, we have introduced a thermodynamically consistent variance-based sensitivity analysis approach for studying the robustness and fragility properties of biochemical reaction systems under uncertainty in the standard chemical potentials of the activated complexes of the reactions and the standard chemical potentials of the molecular species. In that approach, key sensitivity indices were estimated by Monte Carlo sampling, which is computationally very demanding and impractical for large biochemical reaction systems. Computationally efficient algorithms are needed to make variance-based sensitivity analysis applicable to realistic cellular networks, modeled by biochemical reaction systems that consist of a large number of reactions and molecular species. Results We present four techniques, derivative approximation (DA, polynomial approximation (PA, Gauss-Hermite integration (GHI, and orthonormal Hermite approximation (OHA, for analytically approximating the variance-based sensitivity indices associated with a biochemical reaction system. By using a well-known model of the mitogen-activated protein kinase signaling cascade as a case study, we numerically compare the approximation quality of these techniques against traditional Monte Carlo sampling. Our results indicate that, although DA is computationally the most attractive technique, special care should be exercised when using it for sensitivity analysis, since it may only be accurate at low levels of uncertainty. On the other hand, PA, GHI, and OHA are computationally more demanding than DA but can work well at high levels of uncertainty. GHI results in a slightly better accuracy than PA, but it is more difficult to implement. OHA produces the most accurate approximation results and can be implemented in a straightforward manner. It turns out that the computational cost of the

  18. Techniques for sampling nuclear waste tank contents and in situ measurement of activity

    International Nuclear Information System (INIS)

    Lawrence, R.C.

    1978-04-01

    A study was conducted to develop suitable sampling equipment and techniques for characterizing the mechanical properties of nuclear wastes; identifying effective means of measuring radiation levels, temperatures, and neutron fluxes in situ in wastes; and developing a waste core sampler. A portable, stainless steel probe was developed which is placed in the tank through a riser. This probe is built for the insertion of instrumentation that can measure the contents of the tank at any level and take temperature, radiation, and neutron activation readings with reliable accuracy. A simple and reliable instrument for the in situ extraction of waste materials ranging from liquid to concrete-like substances was also developed. This portable, stainless steel waste core sampler can remove up to one liter of radioactive waste from tanks for transportation to hot cell laboratories for analysis of hardness, chemical form, and isotopic content. A cask for transporting the waste samples from the tanks to the laboratory under radiation-protected conditions was also fabricated. This cask was designed with a ''boot'' or inner-seal liner to contain any radioactive wastes that might remain on the outside of the waste core sampling device

  19. Burnout prediction using advance image analysis coal characterization techniques

    Energy Technology Data Exchange (ETDEWEB)

    Edward Lester; Dave Watts; Michael Cloke [University of Nottingham, Nottingham (United Kingdom). School of Chemical Environmental and Mining Engineering

    2003-07-01

    The link between petrographic composition and burnout has been investigated previously by the authors. However, these predictions were based on 'bulk' properties of the coal, including the proportion of each maceral or the reflectance of the macerals in the whole sample. Combustion studies relating burnout with microlithotype analysis, or similar, remain less common partly because the technique is more complex than maceral analysis. Despite this, it is likely that any burnout prediction based on petrographic characteristics will become more accurate if it includes information about the maceral associations and the size of each particle. Chars from 13 coals, 106-125 micron size fractions, were prepared using a Drop Tube Furnace (DTF) at 1300{degree}C and 200 millisecond and 1% Oxygen. These chars were then refired in the DTF at 1300{degree}C 5% oxygen and residence times of 200, 400 and 600 milliseconds. The progressive burnout of each char was compared with the characteristics of the initial coals. This paper presents an extension of previous studies in that it relates combustion behaviour to coals that have been characterized on a particle by particle basis using advanced image analysis techniques. 13 refs., 7 figs.

  20. Probabilistic techniques using Monte Carlo sampling for multi- component system diagnostics

    International Nuclear Information System (INIS)

    Aumeier, S.E.; Lee, J.C.; Akcasu, A.Z.

    1995-01-01

    We outline the structure of a new approach at multi-component system fault diagnostics which utilizes detailed system simulation models, uncertain system observation data, statistical knowledge of system parameters, expert opinion, and component reliability data in an effort to identify incipient component performance degradations of arbitrary number and magnitude. The technique involves the use of multiple adaptive Kalman filters for fault estimation, the results of which are screened using standard hypothesis testing procedures to define a set of component events that could have transpired. Latin Hypercube sample each of these feasible component events in terms of uncertain component reliability data and filter estimates. The capabilities of the procedure are demonstrated through the analysis of a simulated small magnitude binary component fault in a boiling water reactor balance of plant. The results show that the procedure has the potential to be a very effective tool for incipient component fault diagnosis

  1. The development and use of parametric sampling techniques for probabilistic risk assessment

    International Nuclear Information System (INIS)

    Dalrymple, G.J.; Broyd, T.W.

    1987-01-01

    In order to enable evaluation to be made of proposals for the underground disposal of low and intermediate level radioactive wastes in the United Kingdom, the Department of the Environment (DoE) research programme includes development of computer-based methods for use in a multistage assessment process. To test the adequacy of the various methods of data acquisitions and radiological assessment a mock assessment exercise is currently being conducted by the department. This paper outlines the proposed methodology which provides for the use of probabilistic modelling based upon the Atomic Energy of Canada Ltd SYVAC variability analysis approach using new models (SYVAC 'A') and data appropriate to UK conditions for a deep horizontal tunnel repository concept. This chapter describes the choice of a suitable technique for the sampling of data input to the SYVAC 'A' model and techniques for analysing the predictions of dose and risk made by the model. The sensitivity of the model predictions (risk and dose to man) to the input parameters was compared for four different methods. All four methods identified the same geological parameters as the most important. (author)

  2. Microbial and chemical analysis of illicit drugs samples confiscated from different areas of PakistanMicrobial and chemical analysis of illicit drugs samples confiscated from different areas of Pakistan.

    Science.gov (United States)

    Hussain, Shahzad; Khattak, Zainab; Mahmood, Sidra; Malik, Farnaz; Riaz, Humayun; Raza, Syed Atif; Khan, Samiullah

    2016-09-01

    The microbial and chemical analysis of illicit drug samples from different areas of Pakistan i.e. Quetta, Karachi, Lahore and Islamabad was conducted in a cross-sectional study at National Institute of Health, Islamabad. The drug samples were confiscated by Anti Narcotics Force (ANF), Pakistan. Microbial analysis was done by estimating bioburden which revealed the presence of gram negative and positive bacteria's, fungus, Streptococcus, Staphylococcus species. Trypton soya agar was used for total aerobic count, MacConkey agar for gram-negative bacteria, Sabouraud dextrose agar for fungus and Vogel-Johnson agar for Streptococcus and Staphylococcus species. Colour tests were applied to identify the drug samples. Qualitative and quantitative analysis of suspected samples of Heroin, morphine, cocaine and acetic anhydride was made by employing different chromatographic techniques i.e. Thin-layer chromatography (TLC) and High-performance liquid chromatography (HPLC). The samples were found to be adulterated with paracetamol, diazepam and Dextromethorphen. Acetic anhydride was adulterated with hydrochloric acid (HCl). There is lack of information providing structured advice on responses to the consequences of illicit drug adulteration. Robust and rehearsed interventions and communication strategies would provide a basis for response for a wide variety of organisations. Research into the usefulness of media warnings about adulteration of illicit drugs is required.

  3. Final Sampling and Analysis Plan for Background Sampling, Fort Sheridan, Illinois

    National Research Council Canada - National Science Library

    1995-01-01

    .... This Background Sampling and Analysis Plan (BSAP) is designed to address this issue through the collection of additional background samples at Fort Sheridan to support the statistical analysis and the Baseline Risk Assessment (BRA...

  4. Rapid analysis of steels using laser-based techniques

    International Nuclear Information System (INIS)

    Cremers, D.A.; Archuleta, F.L.; Dilworth, H.C.

    1985-01-01

    Based on the data obtained by this study, we conclude that laser-based techniques can be used to provide at least semi-quantitative information about the elemental composition of molten steel. Of the two techniques investigated here, the Sample-Only method appears preferable to the LIBS (laser-induced breakdown spectroscopy) method because of its superior analytical performance. In addition, the Sample-Only method would probably be easier to incorporate into a steel plant environment. However, before either technique can be applied to steel monitoring, additional research is needed

  5. Technique for radionuclide composition analysis of snow cover in the Chernobyl' NPP 30-km zone using fiber sorbents

    International Nuclear Information System (INIS)

    Kham'yanov, L.P.; Rau, D.F.; Amosov, M.M.; Strel'nikova, A.E.; Tereshchenko, V.I.; Veber, T.S.

    1989-01-01

    The high-sensitivity, simple and fast technique for analysis of large-dispersive and ionic components of snow cover radioactivity is suggested. It is based on separation of a sample by fractions, concentration of the dispersive fraction on mechanical filters and the dissolved one on ion-exchange sorbents and separated fraction spectrometry. The minimum measured contamination level is 3.7 Bq/dm 3 for each radionuclide analyzed. The conclusion is made that the technique suggested is the reliable method for radionuclide content analysis is snow cover samples of the Chernobyl' NPP zone. 1 tab

  6. Applications of neutron activation analysis technique in the IPR-R1 research reactor

    International Nuclear Information System (INIS)

    Sabino, C.V.S.; Mansur, N.

    1986-01-01

    A review is made of the neutron activation analysis technique used in the IPR-R1 reactor of the Centro de Desenvolvimento da Tecnologia Nuclear - NUCLEBRAS. Some characteristics of the method are described, types of samples and elements analyzed are also mentioned. (Author) [pt

  7. Analysis of natural milk and milk powder samples by NAA

    International Nuclear Information System (INIS)

    Al-Jobori, S.M.; Itawi, R.K.; Saad, A.; Shihab, K.M.; Jalil, M.; Farhan, S.S.

    1990-01-01

    As a part of the Iraqi Food Analysis Programme the concentration of Na, Mg, P, Cl, K, Ca, Zn, Se, Br, Rb and I in natural milk collected from different regions of Iraq, and in milk powder samples was determined by NAA technique. It was found that except for the elements I, Rb and Br the concentration of the elements was approximately identical in both natural milk and milk powders. (author) 4 refs.; 3 figs.; 5 tabs

  8. Analysis of natural milk and milk powder samples by NAA

    International Nuclear Information System (INIS)

    Al-Jobori, S. M.; Itawi, R. K.; Saad, A; Shihab, K. M.; Jalil, M.; Farhan, S. S.

    1993-01-01

    As a part of the Iraqi food analysis program (IFAP) the concentration of Na, Mg, P, Cl, K, Ca, Zn, Se, Br, Rb, and I in natural milk collected from different regions of Iraq, and in milk powder samples have been determined by using the NAA techniques. It was found that except for the elements I, Rb, and Br the concentrations of the elements was approximately identical in both the natural milk and milk powder. (author)

  9. Accelerated Solvent Extraction: An Innovative Sample Extraction Technique for Natural Products

    International Nuclear Information System (INIS)

    Hazlina Ahmad Hassali; Azfar Hanif Abd Aziz; Rosniza Razali

    2015-01-01

    Accelerated solvent extraction (ASE) is one of the novel techniques that have been developed for the extraction of phytochemicals from plants in order to shorten the extraction time, decrease the solvent consumption, increase the extraction yield and enhance the quality of extracts. This technique combines elevated temperatures and pressure with liquid solvents. This paper gives a brief overview of accelerated solvent extraction technique for sample preparation and its application to the extraction of natural products. Through practical examples, the effects of operational parameters such as temperature, volume of solvent used, extraction time and extraction yields on the performance of ASE are discussed. It is demonstrated that ASE technique allows reduced solvent consumption and shorter extraction time, while the extraction yields are even higher than those obtained with conventional methods. (author)

  10. Practical aspects of the resin bead technique for mass spectrometric sample loading

    International Nuclear Information System (INIS)

    Walker, R.L.; Pritchard, C.A.; Carter, J.A.; Smith, D.H.

    1976-07-01

    Using an anion resin bead as a loading vehicle for uranium and plutonium samples which are to be analyzed isotopically in a mass spectrometer has many advantages over conventional techniques. It is applicable to any laboratory routinely performing such analyses, but should be particularly relevant for Safeguards' purposes. Because the techniques required differ markedly from those of conventional methods, this report has been written to describe them in detail to enable those unfamiliar with the technique to master it with a minimum of trouble

  11. Statistical Symbolic Execution with Informed Sampling

    Science.gov (United States)

    Filieri, Antonio; Pasareanu, Corina S.; Visser, Willem; Geldenhuys, Jaco

    2014-01-01

    Symbolic execution techniques have been proposed recently for the probabilistic analysis of programs. These techniques seek to quantify the likelihood of reaching program events of interest, e.g., assert violations. They have many promising applications but have scalability issues due to high computational demand. To address this challenge, we propose a statistical symbolic execution technique that performs Monte Carlo sampling of the symbolic program paths and uses the obtained information for Bayesian estimation and hypothesis testing with respect to the probability of reaching the target events. To speed up the convergence of the statistical analysis, we propose Informed Sampling, an iterative symbolic execution that first explores the paths that have high statistical significance, prunes them from the state space and guides the execution towards less likely paths. The technique combines Bayesian estimation with a partial exact analysis for the pruned paths leading to provably improved convergence of the statistical analysis. We have implemented statistical symbolic execution with in- formed sampling in the Symbolic PathFinder tool. We show experimentally that the informed sampling obtains more precise results and converges faster than a purely statistical analysis and may also be more efficient than an exact symbolic analysis. When the latter does not terminate symbolic execution with informed sampling can give meaningful results under the same time and memory limits.

  12. A fully blanketed early B star LTE model atmosphere using an opacity sampling technique

    International Nuclear Information System (INIS)

    Phillips, A.P.; Wright, S.L.

    1980-01-01

    A fully blanketed LTE model of a stellar atmosphere with Tsub(e) = 21914 K (thetasub(e) = 0.23), log g = 4 is presented. The model includes an explicit representation of the opacity due to the strongest lines, and uses a statistical opacity sampling technique to represent the weaker line opacity. The sampling technique is subjected to several tests and the model is compared with an atmosphere calculated using the line-distribution function method. The limitations of the distribution function method and the particular opacity sampling method used here are discussed in the light of the results obtained. (author)

  13. Hospital survey on patient safety culture: psychometric analysis on a Scottish sample.

    Science.gov (United States)

    Sarac, Cakil; Flin, Rhona; Mearns, Kathryn; Jackson, Jeanette

    2011-10-01

    To investigate the psychometric properties of the Hospital Survey on Patient Safety Culture on a Scottish NHS data set. The data were collected from 1969 clinical staff (estimated 22% response rate) from one acute hospital from each of seven Scottish Health boards. Using a split-half validation technique, the data were randomly split; an exploratory factor analysis was conducted on the calibration data set, and confirmatory factor analyses were conducted on the validation data set to investigate and check the original US model fit in a Scottish sample. Following the split-half validation technique, exploratory factor analysis results showed a 10-factor optimal measurement model. The confirmatory factor analyses were then performed to compare the model fit of two competing models (10-factor alternative model vs 12-factor original model). An S-B scaled χ(2) square difference test demonstrated that the original 12-factor model performed significantly better in a Scottish sample. Furthermore, reliability analyses of each component yielded satisfactory results. The mean scores on the climate dimensions in the Scottish sample were comparable with those found in other European countries. This study provided evidence that the original 12-factor structure of the Hospital Survey on Patient Safety Culture scale has been replicated in this Scottish sample. Therefore, no modifications are required to the original 12-factor model, which is suggested for use, since it would allow researchers the possibility of cross-national comparisons.

  14. Sample preparation techniques based on combustion reactions in closed vessels - A brief overview and recent applications

    International Nuclear Information System (INIS)

    Flores, Erico M.M.; Barin, Juliano S.; Mesko, Marcia F.; Knapp, Guenter

    2007-01-01

    In this review, a general discussion of sample preparation techniques based on combustion reactions in closed vessels is presented. Applications for several kinds of samples are described, taking into account the literature data reported in the last 25 years. The operational conditions as well as the main characteristics and drawbacks are discussed for bomb combustion, oxygen flask and microwave-induced combustion (MIC) techniques. Recent applications of MIC techniques are discussed with special concern for samples not well digested by conventional microwave-assisted wet digestion as, for example, coal and also for subsequent determination of halogens

  15. Radiation damage of paper samples in in-air PIXE analysis

    International Nuclear Information System (INIS)

    Matsuyama, S.; Endo, H.; Ishii, K.; Yamazaki, H.; Tokai, Y.; Sugimoto, A.; Yamamoto, K.; Satoh, T.; Orihara, H.

    1999-01-01

    Degradation of paper caused by beam irradiation was investigated from a viewpoint of discoloration in PIXE analysis and its application to the paper samples of archaeology. Two types of paper (Japanese paper and fine quality paper) were tested in in-air PIXE analysis with 3 MeV protons. The degree of discoloration was quantitatively measured by the use of a colorimeter. The degree of discoloration was different for each tested paper and corresponded to the radiation dose of ions. It is resulted that even the in-air PIXE analysis should be carefully applied to archaeological treasures. Because discoloration of all tested paper decreased gradually at first but then increased after a few weeks. However, this phenomenon can be used to develop a technique of funny coloration. (author)

  16. Radiation damage of paper samples in in-air PIXE analysis

    Energy Technology Data Exchange (ETDEWEB)

    Matsuyama, S.; Endo, H.; Ishii, K.; Yamazaki, H.; Tokai, Y.; Sugimoto, A.; Yamamoto, K.; Satoh, T. [Department of Quantum Science and Energy Engineering, Tohoku University, Sendai, Miyagi (Japan); Orihara, H. [Tohoku Univ., Sendai (Japan). Cyclotron and Radioisotope Center

    1999-07-01

    Degradation of paper caused by beam irradiation was investigated from a viewpoint of discoloration in PIXE analysis and its application to the paper samples of archaeology. Two types of paper (Japanese paper and fine quality paper) were tested in in-air PIXE analysis with 3 MeV protons. The degree of discoloration was quantitatively measured by the use of a colorimeter. The degree of discoloration was different for each tested paper and corresponded to the radiation dose of ions. It is resulted that even the in-air PIXE analysis should be carefully applied to archaeological treasures. Because discoloration of all tested paper decreased gradually at first but then increased after a few weeks. However, this phenomenon can be used to develop a technique of funny coloration. (author)

  17. [Recent advances in analysis of petroleum geological samples by comprehensive two-dimensional gas chromatography].

    Science.gov (United States)

    Gao, Xuanbo; Chang, Zhenyang; Dai, Wei; Tong, Ting; Zhang, Wanfeng; He, Sheng; Zhu, Shukui

    2014-10-01

    Abundant geochemical information can be acquired by analyzing the chemical compositions of petroleum geological samples. The information obtained from the analysis provides scientifical evidences for petroleum exploration. However, these samples are complicated and can be easily influenced by physical (e. g. evaporation, emulsification, natural dispersion, dissolution and sorption), chemical (photodegradation) and biological (mainly microbial degradation) weathering processes. Therefore, it is very difficult to analyze the petroleum geological samples and they cannot be effectively separated by traditional gas chromatography/mass spectrometry. A newly developed separation technique, comprehensive two-dimensional gas chromatography (GC x GC), has unique advantages in complex sample analysis, and recently it has been applied to petroleum geological samples. This article mainly reviews the research progres- ses in the last five years, the main problems and the future research about GC x GC applied in the area of petroleum geology.

  18. Hepatic mitochondrial function analysis using needle liver biopsy samples.

    Directory of Open Access Journals (Sweden)

    Michael J J Chu

    Full Text Available BACKGROUNDS AND AIM: Current assessment of pre-operative liver function relies upon biochemical blood tests and histology but these only indirectly measure liver function. Mitochondrial function (MF analysis allows direct measurement of cellular metabolic function and may provide an additional index of hepatic health. Conventional MF analysis requires substantial tissue samples (>100 mg obtained at open surgery. Here we report a method to assess MF using <3 mg of tissue obtained by a Tru-cut® biopsy needle making it suitable for percutaneous application. METHODS: An 18G Bard® Max-core® biopsy instrument was used to collect samples. The optimal Tru-cut® sample weight, stability in ice-cold University of Wisconsin solution, reproducibility and protocol utility was initially evaluated in Wistar rat livers then confirmed in human samples. MF was measured in saponin-permeabilized samples using high-resolution respirometry. RESULTS: The average mass of a single rat and human liver Tru-cut® biopsy was 5.60±0.30 and 5.16±0.15 mg, respectively (mean; standard error of mean. Two milligram of sample was found the lowest feasible mass for the MF assay. Tissue MF declined after 1 hour of cold storage. Six replicate measurements within rats and humans (n = 6 each showed low coefficient of variation (<10% in measurements of State-III respiration, electron transport chain (ETC capacity and respiratory control ratio (RCR. Ischemic rat and human liver samples consistently showed lower State-III respiration, ETC capacity and RCR, compared to normal perfused liver samples. CONCLUSION: Consistent measurement of liver MF and detection of derangement in a disease state was successfully demonstrated using less than half the tissue from a single Tru-cut® biopsy. Using this technique outpatient assessment of liver MF is now feasible, providing a new assay for the evaluation of hepatic function.

  19. Analysis of sample composition using resonant ionization and time-of-flight techniques

    International Nuclear Information System (INIS)

    Cruz, A. de la; Ortiz, M.; Campos, J.

    1995-01-01

    This paper describes the setting up of a linear time-of-flight mass spectrometer that uses a tunable laser to produce resonant ionization of atoms and molecules in a pulsed supersonic beam. The ability of this kind of systems to produce time resolved signals for each species present in the sample allows quantitative analysis of its composition. By using a tunable laser beam of high spectral resolution to produce ionization, studies based on the structure of the photoionization spectra obtained are possible. In the present work several isotopic species of ordinary and deuterated benzene have been studied. Special care has been dedicated to the influence of the presence of a 13C in the ring. In this way values for spectroscopic constants and isotopic shifts have been obtained. Another system based in a homemade proportional counter has been designed and used is an auxiliary system. The results obtained with it are independent of these mentioned above and compatible with them. This system is of great utility for laser wavelength tuning to produce ionization in the mass spectrometer. (Author) 98 refs

  20. Analysis of sample composition using resonant ionization and time-of-flight techniques

    International Nuclear Information System (INIS)

    Luz, A. de la; Ortiz, M.; Campos, J.

    1995-01-01

    This paper describes the setting up of a linear time-of-flight mass spectrometer that uses a tunable laser to produce resonant ionization of atoms and molecules in a pulsed supersonic beam. The ability of this kind of systems to produce time resolved signals for each species present in the samples allows quantitative analysis of its composition. By using a tunable laser beam of high spectral resolution to produce ionization, studies based on the structure of the photoionization spectra obtained are possible. In the present work several isotopic species of ordinary and deuterated benzene have been studies. special care has been dedicated to the influence of the presence of a ''13 C in the ring. In this way values for spectroscopic constants and isotopic shifts have been obtained. Another system based in a homemade proportional counter has been designed and used as an auxiliary system. The results obtained with it are independent of these mentioned above and compatible with them. This system is of great utility for laser wavelength tuning to produce ionization in the mass spectrometer

  1. Application of tomographic techniques to two-dimensional surface analysis using the Harwell nuclear microprobe

    International Nuclear Information System (INIS)

    Huddleston, J.; Hutchinson, I.G.; Pierce, T.B.

    1983-01-01

    Nuclear methods of surface analysis are discussed briefly, and the circumstances are described in which a two-dimensional analysis of the sample surface is desirable to enable the surface composition to be mapped accurately. Tomographic techniques of data manipulation are outlined. Data acquisition in the present case is performed by moving the sample in a defined sequence of positions, at each of which analytical data are gathered by the proton microprobe. The method and equipment are outlined. Data processing leading to the reconstruction of the image is summarised. (U.K.)

  2. The application of statistical and/or non-statistical sampling techniques by internal audit functions in the South African banking industry

    Directory of Open Access Journals (Sweden)

    D.P. van der Nest

    2015-03-01

    Full Text Available This article explores the use by internal audit functions of audit sampling techniques in order to test the effectiveness of controls in the banking sector. The article focuses specifically on the use of statistical and/or non-statistical sampling techniques by internal auditors. The focus of the research for this article was internal audit functions in the banking sector of South Africa. The results discussed in the article indicate that audit sampling is still used frequently as an audit evidence-gathering technique. Non-statistical sampling techniques are used more frequently than statistical sampling techniques for the evaluation of the sample. In addition, both techniques are regarded as important for the determination of the sample size and the selection of the sample items

  3. Rapid Analysis of Carbohydrates in Bioprocess Samples: An Evaluation of the CarboPac SA10 for HPAE-PAD Analysis by Interlaboratory Comparison

    Energy Technology Data Exchange (ETDEWEB)

    Sevcik, R. S.; Hyman, D. A.; Basumallich, L.; Scarlata, C. J.; Rohrer, J.; Chambliss, C. K.

    2013-01-01

    A technique for carbohydrate analysis for bioprocess samples has been developed, providing reduced analysis time compared to current practice in the biofuels R&D community. The Thermofisher CarboPac SA10 anion-exchange column enables isocratic separation of monosaccharides, sucrose and cellobiose in approximately 7 minutes. Additionally, use of a low-volume (0.2 mL) injection valve in combination with a high-volume detection cell minimizes the extent of sample dilution required to bring sugar concentrations into the linear range of the pulsed amperometric detector (PAD). Three laboratories, representing academia, industry, and government, participated in an interlaboratory study which analyzed twenty-one opportunistic samples representing biomass pretreatment, enzymatic saccharification, and fermentation samples. The technique's robustness, linearity, and interlaboratory reproducibility were evaluated and showed excellent-to-acceptable characteristics. Additionally, quantitation by the CarboPac SA10/PAD was compared with the current practice method utilizing a HPX-87P/RID. While these two methods showed good agreement a statistical comparison found significant quantitation difference between them, highlighting the difference between selective and universal detection modes.

  4. Effect of sample preparation techniques on the concentrations and distributions of elements in biological tissues using µSRXRF: a comparative study

    International Nuclear Information System (INIS)

    Al-Ebraheem, A; Dao, E; Desouza, E; McNeill, F E; Farquharson, M J; Li, C; Wainman, B C

    2015-01-01

    Routine tissue sample preparation using chemical fixatives is known to preserve the morphology of the tissue being studied. A competitive method, cryofixation followed by freeze drying, involves no chemical agents and maintains the biological function of the tissue. The possible effects of both sample preparation techniques in terms of the distribution of bio-metals (calcium (Ca), copper (Cu) zinc (Zn), and iron (Fe) specifically) in human skin tissue samples was investigated. Micro synchrotron radiation x-ray fluorescence (μSRXRF) was used to map bio-metal distribution in epidermal and dermal layers of human skin samples from various locations of the body that have been prepared using both techniques. For Ca, Cu and Zn, there were statistically significant differences between the epidermis and dermis using the freeze drying technique (p = 0.02, p < 0.01, and p < 0.01, respectively). Also using the formalin fixed, paraffin embedded technique the levels of Ca, Cu and Zn, were significantly different between the epidermis and dermis layers (p = 0.03, p < 0.01, and p < 0.01, respectively). However, the difference in levels of Fe between the epidermis and dermis was unclear and further analysis was required. The epidermis was further divided into two sub-layers, one mainly composed of the stratum corneum and the other deeper layer, the stratum basale. It was found that the difference between the distribution of Fe in the two epidermal layers using the freeze drying technique resulted in a statistically significant difference (p = 0.012). This same region also showed a difference in Fe using the formalin fixed, paraffin embedded technique (p < 0.01). The formalin fixed, paraffin embedded technique also showed a difference between the deeper epidermal layer and the dermis (p < 0.01). It can be concluded that studies involving Ca, Cu and Zn might show similar results using both sample preparation techniques, however studies involving Fe would need more

  5. Current applications of miniaturized chromatographic and electrophoretic techniques in drug analysis.

    Science.gov (United States)

    Aturki, Zeineb; Rocco, Anna; Rocchi, Silvia; Fanali, Salvatore

    2014-12-01

    In the last decade, miniaturized separation techniques have become greatly popular in pharmaceutical analysis. Miniaturized separation methods are increasingly utilized in all processes of drug discovery as well as quality control of pharmaceutical preparation. The great advantages presented by the analytical miniaturized techniques, including high separation efficiency and resolution, rapid analysis and minimal consumption of reagents and samples, make them an attractive alternative to the conventional chromatographic methods for drug analysis. The purpose of this review is to give a general overview of the applicability of capillary electrophoresis (CE), capillary electrochromatography (CEC) and micro/capillary/nano-liquid chromatography (micro-LC/CLC/nano-LC) for the analysis of pharmaceutical formulations, active pharmaceutical ingredients (API), drug impurity testing, chiral drug separation, determination of drugs and metabolites in biological fluids. The results concerning the use of CEC, micro-LC, CLC, and nano-LC in the period 2009-2013, while for CE, those from 2012 up to the review draft are here summarized and some specific examples are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. Noble Gas Measurement and Analysis Technique for Monitoring Reprocessing Facilities

    International Nuclear Information System (INIS)

    William S. Charlton

    1999-01-01

    An environmental monitoring technique using analysis of stable noble gas isotopic ratios on-stack at a reprocessing facility was developed. This technique integrates existing technologies to strengthen safeguards at reprocessing facilities. The isotopic ratios are measured using a mass spectrometry system and are compared to a database of calculated isotopic ratios using a Bayesian data analysis method to determine specific fuel parameters (e.g., burnup, fuel type, fuel age, etc.). These inferred parameters can be used by investigators to verify operator declarations. A user-friendly software application (named NOVA) was developed for the application of this technique. NOVA included a Visual Basic user interface coupling a Bayesian data analysis procedure to a reactor physics database (calculated using the Monteburns 3.01 code system). The integrated system (mass spectrometry, reactor modeling, and data analysis) was validated using on-stack measurements during the reprocessing of target fuel from a U.S. production reactor and gas samples from the processing of EBR-II fast breeder reactor driver fuel. These measurements led to an inferred burnup that matched the declared burnup with sufficient accuracy and consistency for most safeguards applications. The NOVA code was also tested using numerous light water reactor measurements from the literature. NOVA was capable of accurately determining spent fuel type, burnup, and fuel age for these experimental results. Work should continue to demonstrate the robustness of this system for production, power, and research reactor fuels

  7. Laboratory manual on sample preparation procedures for x-ray micro-analysis

    International Nuclear Information System (INIS)

    1997-01-01

    X-ray micro fluorescence is a non-destructive and sensitive method for studying the microscopic distribution of different elements in almost all kinds of samples. Since the beginning of this century, x-rays and electrons have been used for the analysis of many different kinds of material. Techniques which rely on electrons are mainly developed for microscopic studies, and are used in conventional Electron Microscopy (EM) or Scanning Electron Microscopy (SEM), while x-rays are widely used for chemical analysis at the microscopic level. The first chemical analysis by fluorescence spectroscopy using small x-ray beams was conducted in 1928 by Glockner and Schreiber. Since then much work has been devoted to developing different types of optical systems for focusing an x-ray beam, but the efficiency of these systems is still inferior to the conventional electron optical systems. However, even with a poor optical efficiency, the x-ray microbeam has many advantages compared with electron or proton induced x-ray emission methods. These include: The analyses are non-destructive, losses of mass are negligible, and due to the low thermal loading of x-rays, materials which may be thermally degraded can be analysed; Samples can be analysed in air, and no vacuum is required, therefore specimens with volatile components such as water in biological samples, can be imaged at normal pressure and temperature; No charging occurs during analysis and therefore coating of the sample with a conductive layer is not necessary; With these advantages, simpler sample preparation procedures including mounting and preservation can be used

  8. Use of spectroscopic techniques for the chemical analysis of biomorphic silicon carbide ceramics

    International Nuclear Information System (INIS)

    Pavon, J.M. Cano; Alonso, E. Vereda; Cordero, M.T. Siles; Torres, A. Garcia de; Lopez-Cepero, J.M.

    2005-01-01

    Biomorphic silicon carbide ceramics are a new class of materials prepared by several complex processing steps including pre-processing (shaping, drying, high-temperature pyrolysis in an inert atmosphere) and reaction with liquid silicon to obtain silicon-carbide. The results of industrial process of synthesis (measured by the SiC content) must be evaluated by means of fast analytical methods. In the present work, diverse samples of biomorphic ceramics derived from wood are studied for to evaluate the capability of the different analytical techniques (XPS, LIBS, FT-IR and also atomic spectroscopy applied to previously dissolved samples) for the analysis of these materials. XPS and LIBS gives information about the major components, whereas XPS and FT-IR can be used to evaluate the content of SiC. On the other hand, .the use of atomic techniques (as ICP-MS and ETA-AAS) is more adequate for the analysis of metal ions, specially at trace level. The properties of ceramics depend decisively of the content of chemical elements. Major components found were C, Si, Al, S, B and Na in all cases. Previous dissolution of the samples was optimised by acid attack in an oven under microwave irradiation

  9. Analyses of archaeological pottery samples using X-ray fluorescence technique for provenance study

    International Nuclear Information System (INIS)

    Tamilarasu, S.; Swain, K.K.; Singhal, R.K; Reddy, A.V.R.; Acharya, R.; Velraj, G.

    2015-01-01

    Archaeological artifacts reveal information on past human activities, artifact preparation technology, art and possible trade. Ceramics are the most stable and abundant material in archaeological context. Pottery is the most abundant tracers in all archaeological excavations. Compared to major elements, elements present at trace concentrations levels are source specific and they maintain same concentration levels in source clay as well as finished products e.g., fired clay potteries. As it is difficult to find out exact source or origin, provenance study is carried out first to establish whether objects under study are from the same or different sources/origin. Various analytical techniques like instrumental neutron activation analysis (INAA), Ion beam analysis (IBA) and X-ray fluorescence (XRF) have been used for obtaining elemental concentrations in archaeological potteries. Portable X-ray fluorescence (pXRF) spectrometry provides a non-destructive means for elemental characterization of a wide range of archaeological materials. Ten archaeological pottery samples were collected from Kottapuram, Kerala under the supervision of archaeological survey of India. Portable X-ray fluorescence (pXRF) spectrometry using a handheld Olympus Innov-X Delta XRF device, ACD BARC, has been used for chemical characterization of the pottery samples. The instrument is equipped with the Delta Rhodium (Rh) anode X-Ray tube and uses a Silicon Drift Detector (resolution <200 eV at 5.95 keV Mn Kα X-ray). NIST 2781 SRM was analyzed for quality control purpose. Ten elements namely Fe, Ti, Mn, Co, Cu, Zn, Pb, Zr, Mo and Se were chosen for cluster analysis and their concentration values were utilized for multivariate statistical analysis using WinSTAT 9.0

  10. Analysis of IFR samples at ANL-E

    International Nuclear Information System (INIS)

    Bowers, D.L.; Sabau, C.S.

    1993-01-01

    The Analytical Chemistry Laboratory analyzes a variety of samples submitted by the different research groups within IFR. This talk describes the analytical work on samples generated by the Plutonium Electrorefiner, Large Scale Electrorefiner and Waste Treatment Studies. The majority of these samples contain Transuranics and necessitate facilities that safely contain these radioisotopes. Details such as: sample receiving, dissolution techniques, chemical separations, Instrumentation used, reporting of results are discussed. The Importance of Interactions between customer and analytical personnel Is also demonstrated

  11. Random sampling technique for ultra-fast computations of molecular opacities for exoplanet atmospheres

    Science.gov (United States)

    Min, M.

    2017-10-01

    Context. Opacities of molecules in exoplanet atmospheres rely on increasingly detailed line-lists for these molecules. The line lists available today contain for many species up to several billions of lines. Computation of the spectral line profile created by pressure and temperature broadening, the Voigt profile, of all of these lines is becoming a computational challenge. Aims: We aim to create a method to compute the Voigt profile in a way that automatically focusses the computation time into the strongest lines, while still maintaining the continuum contribution of the high number of weaker lines. Methods: Here, we outline a statistical line sampling technique that samples the Voigt profile quickly and with high accuracy. The number of samples is adjusted to the strength of the line and the local spectral line density. This automatically provides high accuracy line shapes for strong lines or lines that are spectrally isolated. The line sampling technique automatically preserves the integrated line opacity for all lines, thereby also providing the continuum opacity created by the large number of weak lines at very low computational cost. Results: The line sampling technique is tested for accuracy when computing line spectra and correlated-k tables. Extremely fast computations ( 3.5 × 105 lines per second per core on a standard current day desktop computer) with high accuracy (≤1% almost everywhere) are obtained. A detailed recipe on how to perform the computations is given.

  12. Reliability analysis techniques in power plant design

    International Nuclear Information System (INIS)

    Chang, N.E.

    1981-01-01

    An overview of reliability analysis techniques is presented as applied to power plant design. The key terms, power plant performance, reliability, availability and maintainability are defined. Reliability modeling, methods of analysis and component reliability data are briefly reviewed. Application of reliability analysis techniques from a design engineering approach to improving power plant productivity is discussed. (author)

  13. A comparison of quantitative reconstruction techniques for PIXE-tomography analysis applied to biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Beasley, D.G., E-mail: dgbeasley@ctn.ist.utl.pt [IST/C2TN, Universidade de Lisboa, Campus Tecnológico e Nuclear, E.N.10, 2686-953 Sacavém (Portugal); Alves, L.C. [IST/C2TN, Universidade de Lisboa, Campus Tecnológico e Nuclear, E.N.10, 2686-953 Sacavém (Portugal); Barberet, Ph.; Bourret, S.; Devès, G.; Gordillo, N.; Michelet, C. [Univ. Bordeaux, CENBG, UMR 5797, F-33170 Gradignan (France); CNRS, IN2P3, CENBG, UMR 5797, F-33170 Gradignan (France); Le Trequesser, Q. [Univ. Bordeaux, CENBG, UMR 5797, F-33170 Gradignan (France); CNRS, IN2P3, CENBG, UMR 5797, F-33170 Gradignan (France); Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB, UPR9048) CNRS, Université de Bordeaux, 87 avenue du Dr. A. Schweitzer, Pessac F-33608 (France); Marques, A.C. [IST/IPFN, Universidade de Lisboa, Campus Tecnológico e Nuclear, E.N.10, 2686-953 Sacavém (Portugal); Seznec, H. [Univ. Bordeaux, CENBG, UMR 5797, F-33170 Gradignan (France); CNRS, IN2P3, CENBG, UMR 5797, F-33170 Gradignan (France); Silva, R.C. da [IST/IPFN, Universidade de Lisboa, Campus Tecnológico e Nuclear, E.N.10, 2686-953 Sacavém (Portugal)

    2014-07-15

    The tomographic reconstruction of biological specimens requires robust algorithms, able to deal with low density contrast and low element concentrations. At the IST/ITN microprobe facility new GPU-accelerated reconstruction software, JPIXET, has been developed, which can significantly increase the speed of quantitative reconstruction of Proton Induced X-ray Emission Tomography (PIXE-T) data. It has a user-friendly graphical user interface for pre-processing, data analysis and reconstruction of PIXE-T and Scanning Transmission Ion Microscopy Tomography (STIM-T). The reconstruction of PIXE-T data is performed using either an algorithm based on a GPU-accelerated version of the Maximum Likelihood Expectation Maximisation (MLEM) method or a GPU-accelerated version of the Discrete Image Space Reconstruction Algorithm (DISRA) (Sakellariou (2001) [2]). The original DISRA, its accelerated version, and the MLEM algorithm, were compared for the reconstruction of a biological sample of Caenorhabditis elegans – a small worm. This sample was analysed at the microbeam line of the AIFIRA facility of CENBG, Bordeaux. A qualitative PIXE-T reconstruction was obtained using the CENBG software package TomoRebuild (Habchi et al. (2013) [6]). The effects of pre-processing and experimental conditions on the elemental concentrations are discussed.

  14. Quality control of the analysis of IAEA samples in the radium institute

    International Nuclear Information System (INIS)

    Belyaev, B.N.; Lovtsus, A.V.; Makarova, T.P.; Stepanov, A.V.

    1989-01-01

    Metrological chracteristics of mass and alpha spectrometric methods in the Radium Institute for analysis of spent fuel control samples are evaluated. The techniques of analysis and the procedure of quality control for isotopic ratio measurements based on the use of uranium and plutonium standard reference materials (NBS, NBL, SAL made in USSR) are described. The results of measurements performed during cooperation with IAEA are discussed, and the sources of systematic and random errors are analyzed. The results obtained agree well with the target values. (author)

  15. 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

  16. 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

  17. Self-Normalized Photoacoustic Technique for the Quantitative Analysis of Paper Pigments

    Science.gov (United States)

    Balderas-López, J. A.; Gómez y Gómez, Y. M.; Bautista-Ramírez, M. E.; Pescador-Rojas, J. A.; Martínez-Pérez, L.; Lomelí-Mejía, P. A.

    2018-03-01

    A self-normalized photoacoustic technique was applied for quantitative analysis of pigments embedded in solids. Paper samples (filter paper, Whatman No. 1), attached with the pigment: Direct Fast Turquoise Blue GL, were used for this study. This pigment is a blue dye commonly used in industry to dye paper and other fabrics. The optical absorption coefficient, at a wavelength of 660 nm, was measured for this pigment at various concentrations in the paper substrate. It was shown that Beer-Lambert model for light absorption applies well for pigments in solid substrates and optical absorption coefficients as large as 220 cm^{-1} can be measured with this photoacoustic technique.

  18. Using Quantitative Data Analysis Techniques for Bankruptcy Risk Estimation for Corporations

    Directory of Open Access Journals (Sweden)

    Ştefan Daniel ARMEANU

    2012-01-01

    Full Text Available Diversification of methods and techniques for quantification and management of risk has led to the development of many mathematical models, a large part of which focused on measuring bankruptcy risk for businesses. In financial analysis there are many indicators which can be used to assess the risk of bankruptcy of enterprises but to make an assessment it is needed to reduce the number of indicators and this can be achieved through principal component, cluster and discriminant analyses techniques. In this context, the article aims to build a scoring function used to identify bankrupt companies, using a sample of companies listed on Bucharest Stock Exchange.

  19. The use of laser-induced fluorescence or ultraviolet detectors for sensitive and selective analysis of tobramycin or erythropoietin in complex samples

    Science.gov (United States)

    Ahmed, Hytham M.; Ebeid, Wael B.

    2015-05-01

    Complex samples analysis is a challenge in pharmaceutical and biopharmaceutical analysis. In this work, tobramycin (TOB) analysis in human urine samples and recombinant human erythropoietin (rhEPO) analysis in the presence of similar protein were selected as representative examples of such samples analysis. Assays of TOB in urine samples are difficult because of poor detectability. Therefore laser induced fluorescence detector (LIF) was combined with a separation technique, micellar electrokinetic chromatography (MEKC), to determine TOB through derivatization with fluorescein isothiocyanate (FITC). Borate was used as background electrolyte (BGE) with negative-charged mixed micelles as additive. The method was successively applied to urine samples. The LOD and LOQ for Tobramycin in urine were 90 and 200 ng/ml respectively and recovery was >98% (n = 5). All urine samples were analyzed by direct injection without sample pre-treatment. Another use of hyphenated analytical technique, capillary zone electrophoresis (CZE) connected to ultraviolet (UV) detector was also used for sensitive analysis of rhEPO at low levels (2000 IU) in the presence of large amount of human serum albumin (HSA). Analysis of rhEPO was achieved by the use of the electrokinetic injection (EI) with discontinuous buffers. Phosphate buffer was used as BGE with metal ions as additive. The proposed method can be used for the estimation of large number of quality control rhEPO samples in a short period.

  20. Rapid analysis of mixed waste samples via the optical emission from laser initiated microplasmas

    International Nuclear Information System (INIS)

    Barefield, J.E. II; Ferran, M.D.; Cremers, D.A.

    1993-01-01

    Wavelength resolved optical emission from laser initiated microplasmas in samples containing Pu, Am, Pb, Cr, and Be was used to determine elemental compositions. Traditionally, samples of this type are analyzed by neutron activation, X-ray fluorescence, atomic absorption (AA), inductively coupled plasma - atomic emission spectroscopy (ICP-AES), and inductively coupled plasma mass spectroscopy (ICP-MS). Analysis via the traditional analytical spectroscopic techniques involves extensive sample separation and preparation which results in the generation of significant quantities of additional waste. In the laser based method, little to no sample preparation is required. The method is essentially waste free since only a few micrograms of material is removed from the sample in the generation of the microplasma. Detection limits of the laser based method typically range between subppm to tens of ppM. In this report, the optical emission from samples containing Pu, Am, Pb, Cr, and Be will be discussed. we will also discuss the essential elements of the analysis method

  1. Experimental technique to measure thoron generation rate of building material samples using RAD7 detector

    International Nuclear Information System (INIS)

    Csige, I.; Szabó, Zs.; Szabó, Cs.

    2013-01-01

    Thoron ( 220 Rn) is the second most abundant radon isotope in our living environment. In some dwellings it is present in significant amount which calls for its identification and remediation. Indoor thoron originates mainly from building materials. In this work we have developed and tested an experimental technique to measure thoron generation rate in building material samples using RAD7 radon-thoron detector. The mathematical model of the measurement technique provides the thoron concentration response of RAD7 as a function of the sample thickness. For experimental validation of the technique an adobe building material sample was selected for measuring the thoron concentration at nineteen different sample thicknesses. Fitting the parameters of the model to the measurement results, both the generation rate and the diffusion length of thoron was estimated. We have also determined the optimal sample thickness for estimating the thoron generation rate from a single measurement. -- Highlights: • RAD7 is used for the determination of thoron generation rate (emanation). • The described model takes into account the thoron decay and attenuation. • The model describes well the experimental results. • A single point measurement method is offered at a determined sample thickness

  2. Nuclear analysis techniques and environmental sciences

    International Nuclear Information System (INIS)

    1997-10-01

    31 theses are collected in this book. It introduced molecular activation analysis micro-PIXE and micro-probe analysis, x-ray fluorescence analysis and accelerator mass spectrometry. The applications about these nuclear analysis techniques are presented and reviewed for environmental sciences

  3. Subsurface stormflow modeling with sensitivity analysis using a Latin-hypercube sampling technique

    International Nuclear Information System (INIS)

    Gwo, J.P.; Toran, L.E.; Morris, M.D.; Wilson, G.V.

    1994-09-01

    Subsurface stormflow, because of its dynamic and nonlinear features, has been a very challenging process in both field experiments and modeling studies. The disposal of wastes in subsurface stormflow and vadose zones at Oak Ridge National Laboratory, however, demands more effort to characterize these flow zones and to study their dynamic flow processes. Field data and modeling studies for these flow zones are relatively scarce, and the effect of engineering designs on the flow processes is poorly understood. On the basis of a risk assessment framework and a conceptual model for the Oak Ridge Reservation area, numerical models of a proposed waste disposal site were built, and a Latin-hypercube simulation technique was used to study the uncertainty of model parameters. Four scenarios, with three engineering designs, were simulated, and the effectiveness of the engineering designs was evaluated. Sensitivity analysis of model parameters suggested that hydraulic conductivity was the most influential parameter. However, local heterogeneities may alter flow patterns and result in complex recharge and discharge patterns. Hydraulic conductivity, therefore, may not be used as the only reference for subsurface flow monitoring and engineering operations. Neither of the two engineering designs, capping and French drains, was found to be effective in hydrologically isolating downslope waste trenches. However, pressure head contours indicated that combinations of both designs may prove more effective than either one alone

  4. Advanced analytical techniques

    International Nuclear Information System (INIS)

    Mrochek, J.E.; Shumate, S.E.; Genung, R.K.; Bahner, C.T.; Lee, N.E.; Dinsmore, S.R.

    1976-01-01

    The development of several new analytical techniques for use in clinical diagnosis and biomedical research is reported. These include: high-resolution liquid chromatographic systems for the early detection of pathological molecular constituents in physiologic body fluids; gradient elution chromatography for the analysis of protein-bound carbohydrates in blood serum samples, with emphasis on changes in sera from breast cancer patients; electrophoretic separation techniques coupled with staining of specific proteins in cellular isoenzymes for the monitoring of genetic mutations and abnormal molecular constituents in blood samples; and the development of a centrifugal elution chromatographic technique for the assay of specific proteins and immunoglobulins in human blood serum samples

  5. Techniques involving extreme environment, nondestructive techniques, computer methods in metals research, and data analysis

    International Nuclear Information System (INIS)

    Bunshah, R.F.

    1976-01-01

    A number of different techniques which range over several different aspects of materials research are covered in this volume. They are concerned with property evaluation of 4 0 K and below, surface characterization, coating techniques, techniques for the fabrication of composite materials, computer methods, data evaluation and analysis, statistical design of experiments and non-destructive test techniques. Topics covered in this part include internal friction measurements; nondestructive testing techniques; statistical design of experiments and regression analysis in metallurgical research; and measurement of surfaces of engineering materials

  6. Trends in grazing emission x-ray analysis techniques

    International Nuclear Information System (INIS)

    Grieken, R. van; Tsuji, K.; Injuk, J.

    2000-01-01

    then, the detection limits imposed by the semiconductor industry roadmap can probably not be obtained by tube-excited GEXRF. Th perspectives for tube-excited GE-XRF are thus rather poor. Future developments imply the combination of GEXRF with synchrotron radiation excitation. Grazing-emission particle-induced X-ray emission (GE-PIXE) suffers of similar quantification Problems for material deposited on a carrier, but it makes PIXE a surface-sensitive technique, while normally the protons penetrate some tens of μm in the sample. Similarly, grazing-emission electron probe micro-analysis (GE-EPNIA) allows to selectively analyze particles on a flat carrier, allows surface sensitivities in the nm rather than μ range, and yields, in principle, a spatial resolution for chemical analysis similar to the size of the impinging electron beam, rather than of the electron-excited volume. Both GE-PIXE and GE-EPMA need to be explored more fully in the near future. (author)

  7. Large sample neutron activation analysis: establishment at CDTN/CNEN, Brazil

    Energy Technology Data Exchange (ETDEWEB)

    Menezes, Maria Angela de B.C., E-mail: menezes@cdtn.b [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil); Jacimovic, Radojko, E-mail: radojko.jacimovic@ijs.s [Jozef Stefan Institute, Ljubljana (Slovenia). Dept. of Environmental Sciences. Group for Radiochemistry and Radioecology

    2011-07-01

    In order to improve the application of the neutron activation technique at CDTN/CNEN, the large sample instrumental neutron activation analysis is being established, IAEA BRA 14798 and FAPEMIG APQ-01259-09 projects. This procedure, LS-INAA, usually requires special facilities for the activation as well as for the detection. However, the TRIGA Mark I IPR R1, CDTN/CNEN has not been adapted for the irradiation and the usual gamma spectrometry has being carried out. To start the establishment of the LS-INAA, a 5g sample - IAEA/Soil 7 reference material was analyzed by k{sub 0}-standardized method. This paper is about the detector efficiency over the volume source using KayWin v2.23 and ANGLE V3.0 software. (author)

  8. PIXE–PIGE analysis of size-segregated aerosol samples from remote areas

    Energy Technology Data Exchange (ETDEWEB)

    Calzolai, G., E-mail: calzolai@fi.infn.it [Department of Physics and Astronomy, University of Florence and National Institute of Nuclear Physics (INFN), Via G. Sansone 1, 50019 Sesto Fiorentino (Italy); Chiari, M.; Lucarelli, F.; Nava, S.; Taccetti, F. [Department of Physics and Astronomy, University of Florence and National Institute of Nuclear Physics (INFN), Via G. Sansone 1, 50019 Sesto Fiorentino (Italy); Becagli, S.; Frosini, D.; Traversi, R.; Udisti, R. [Department of Chemistry, University of Florence, Via della Lastruccia 3, 50019 Sesto Fiorentino (Italy)

    2014-01-01

    The chemical characterization of size-segregated samples is helpful to study the aerosol effects on both human health and environment. The sampling with multi-stage cascade impactors (e.g., Small Deposit area Impactor, SDI) produces inhomogeneous samples, with a multi-spot geometry and a non-negligible particle stratification. At LABEC (Laboratory of nuclear techniques for the Environment and the Cultural Heritage), an external beam line is fully dedicated to PIXE–PIGE analysis of aerosol samples. PIGE is routinely used as a sidekick of PIXE to correct the underestimation of PIXE in quantifying the concentration of the lightest detectable elements, like Na or Al, due to X-ray absorption inside the individual aerosol particles. In this work PIGE has been used to study proper attenuation correction factors for SDI samples: relevant attenuation effects have been observed also for stages collecting smaller particles, and consequent implications on the retrieved aerosol modal structure have been evidenced.

  9. Comparison of results analysis of chemical composition of alloys inside the U-Zr-Nb by XRF and AAS techniques

    International Nuclear Information System (INIS)

    Masrukan; Tri Yulianto; Anwar Muchsin

    2011-01-01

    U-Zr-Nb alloy chemical composition analysis using X Ray Fluorescence (XRF) and Atomic Absorption Spectroscopy (AAS) techniques have been conducted, where U-Zr- Nb alloy was chosen as candidates for new high-density fuel for future research reactors . Composition analysis is necessary because the composition of elements in the fuel will determine the characteristics of fuel during the fabrication process and in the reactor. The use of two kinds of analysis techniques were designed to obtain accurate analysis results. The experiment was conducted to determine the major element composition and impurities in the alloy U-Zr-Nb. First U-Zr-Nb varying alloy composition Nb were respectively 1%, 4%, 7% (U10% Zr1% Nb, U10% Zr4% Nb and U10% 7% Nb) as results of the melting process of measuring the diameter of 120 mm crushed on the surface bottom. Once on the bottom surface is smooth, then analyzed using XRF techniques. To analyze the elements using AAS techniques, alloy U-Zr-Nb cut into 10 mm x 5 mm then dissolved using HF and nitric acid. Solution that occurred were analyzed using AAS technique. From the analysis using the XRF technique is obtained the alloy U-10% Zr-1% Nb, U-10% Zr-4% Nb and Zr-10% U-7% Nb) had a content of each element as follows: U (87.8858%), Zr (2.6097%) and Nb (0.2206%), U (87.8556%), Zr (2.6302%), and Nb (0.6573%); U (84.6334%), Zr (2.5773%), and Nb (1.0940) weight. Results of analysis using AAS techniques on samples obtained third consecutive Zr content of 9.25%, 8.90% and 9.80% while the content of Nb was not detected. Meanwhile, the results of elemental analysis of impurities in all three samples showed that almost all the elements are still qualify as fuel except Zn element. Element Zn at the three samples of each alloys U-10% Zr-1% Nb, U-10% Zr-4% Nb and U-10% Zr-7%Nb is 1.3266%, 3.2756% and 1.0927% weight. It could be concluded that the results of analysis of elemental content and impurities in the alloy U-Nb-Zr using both XRF and AAS visible

  10. Evaluation of nuclear reactor based activation analysis techniques

    International Nuclear Information System (INIS)

    Obrusnik, I.; Kucera, J.

    1977-09-01

    A survey is presented of the basic types of activation analysis applied in environmental control. Reactor neutron activation analysis is described (including the reactor as a neutron source, sample activation in the reactor, methodology of neutron activation analysis, sample transport into the reactor and sample packaging after irradiation, instrumental activation analysis with radiochemical separation, data measurement and evaluation, sampling and sample preparation). Sources of environmental contamination with trace elements, sampling and sample analysis by neutron activation are described. The analysis is described of soils, waters and biological materials. Methods are shown of evaluating neutron activation analysis results and of their interpretation for purposes of environmental control. (J.B.)

  11. Sampling phased array - a new technique for ultrasonic signal processing and imaging

    OpenAIRE

    Verkooijen, J.; Boulavinov, A.

    2008-01-01

    Over the past 10 years, the improvement in the field of microelectronics and computer engineering has led to significant advances in ultrasonic signal processing and image construction techniques that are currently being applied to non-destructive material evaluation. A new phased array technique, called 'Sampling Phased Array', has been developed in the Fraunhofer Institute for Non-Destructive Testing([1]). It realises a unique approach of measurement and processing of ultrasonic signals. Th...

  12. Sensitivity/uncertainty analysis of a borehole scenario comparing Latin Hypercube Sampling and deterministic sensitivity approaches

    International Nuclear Information System (INIS)

    Harper, W.V.; Gupta, S.K.

    1983-10-01

    A computer code was used to study steady-state flow for a hypothetical borehole scenario. The model consists of three coupled equations with only eight parameters and three dependent variables. This study focused on steady-state flow as the performance measure of interest. Two different approaches to sensitivity/uncertainty analysis were used on this code. One approach, based on Latin Hypercube Sampling (LHS), is a statistical sampling method, whereas, the second approach is based on the deterministic evaluation of sensitivities. The LHS technique is easy to apply and should work well for codes with a moderate number of parameters. Of deterministic techniques, the direct method is preferred when there are many performance measures of interest and a moderate number of parameters. The adjoint method is recommended when there are a limited number of performance measures and an unlimited number of parameters. This unlimited number of parameters capability can be extremely useful for finite element or finite difference codes with a large number of grid blocks. The Office of Nuclear Waste Isolation will use the technique most appropriate for an individual situation. For example, the adjoint method may be used to reduce the scope to a size that can be readily handled by a technique such as LHS. Other techniques for sensitivity/uncertainty analysis, e.g., kriging followed by conditional simulation, will be used also. 15 references, 4 figures, 9 tables

  13. Applications of Electromigration Techniques: Applications of Electromigration Techniques in Food Analysis

    Science.gov (United States)

    Wieczorek, Piotr; Ligor, Magdalena; Buszewski, Bogusław

    Electromigration techniques, including capillary electrophoresis (CE), are widely used for separation and identification of compounds present in food products. These techniques may also be considered as alternate and complementary with respect to commonly used analytical techniques, such as high-performance liquid chromatography (HPLC), or gas chromatography (GC). Applications of CE concern the determination of high-molecular compounds, like polyphenols, including flavonoids, pigments, vitamins, food additives (preservatives, antioxidants, sweeteners, artificial pigments) are presented. Also, the method developed for the determination of proteins and peptides composed of amino acids, which are basic components of food products, are studied. Other substances such as carbohydrates, nucleic acids, biogenic amines, natural toxins, and other contaminations including pesticides and antibiotics are discussed. The possibility of CE application in food control laboratories, where analysis of the composition of food and food products are conducted, is of great importance. CE technique may be used during the control of technological processes in the food industry and for the identification of numerous compounds present in food. Due to the numerous advantages of the CE technique it is successfully used in routine food analysis.

  14. Two-compartment, two-sample technique for accurate estimation of effective renal plasma flow: Theoretical development and comparison with other methods

    International Nuclear Information System (INIS)

    Lear, J.L.; Feyerabend, A.; Gregory, C.

    1989-01-01

    Discordance between effective renal plasma flow (ERPF) measurements from radionuclide techniques that use single versus multiple plasma samples was investigated. In particular, the authors determined whether effects of variations in distribution volume (Vd) of iodine-131 iodohippurate on measurement of ERPF could be ignored, an assumption implicit in the single-sample technique. The influence of Vd on ERPF was found to be significant, a factor indicating an important and previously unappreciated source of error in the single-sample technique. Therefore, a new two-compartment, two-plasma-sample technique was developed on the basis of the observations that while variations in Vd occur from patient to patient, the relationship between intravascular and extravascular components of Vd and the rate of iodohippurate exchange between the components are stable throughout a wide range of physiologic and pathologic conditions. The new technique was applied in a series of 30 studies in 19 patients. Results were compared with those achieved with the reference, single-sample, and slope-intercept techniques. The new two-compartment, two-sample technique yielded estimates of ERPF that more closely agreed with the reference multiple-sample method than either the single-sample or slope-intercept techniques

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

    International Nuclear Information System (INIS)

    2016-03-01

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

  16. Simultaneous multi-element determination in different seed samples of Dodonaea viscosa hopseed using instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    El-Sweify, Fatma H.; El-Amir, Mahmoud A.; Mostafa, Mohamed; Ramadan, Hala E.; Rashad, Ghada M.

    2016-01-01

    Instrumental neutron activation analysis technique (INAA) was applied for nondestructive multi-element analysis of seed samples of the plant Dodonaea viscosa hopseed. This plant is distributed all over Egypt, because of its suitable properties. The samples were collected from some bushes grown at different sites in some governorates, in July of each year during the period from 2004 to 2011. The determined elements are: Co, Cs, Eu, Fe, Hg, Ni, Rb, Sc, Se, Sr and Zn, under the chosen irradiation and cooling times. The content of some elements has been compared with data obtained from previous work on analysis of various kinds of seeds. The influence of some parameters on the determined elemental content is discussed. Standard reference materials IAEA-155 and IAEA-V-10 were used to assure quality control, accuracy and precision of the technique.

  17. Simultaneous multi-element determination in different seed samples of Dodonaea viscosa hopseed using instrumental neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    El-Sweify, Fatma H.; El-Amir, Mahmoud A.; Mostafa, Mohamed; Ramadan, Hala E.; Rashad, Ghada M. [Atomic Energy Authority, Cairo (Egypt). Hot Lab. Center

    2016-07-01

    Instrumental neutron activation analysis technique (INAA) was applied for nondestructive multi-element analysis of seed samples of the plant Dodonaea viscosa hopseed. This plant is distributed all over Egypt, because of its suitable properties. The samples were collected from some bushes grown at different sites in some governorates, in July of each year during the period from 2004 to 2011. The determined elements are: Co, Cs, Eu, Fe, Hg, Ni, Rb, Sc, Se, Sr and Zn, under the chosen irradiation and cooling times. The content of some elements has been compared with data obtained from previous work on analysis of various kinds of seeds. The influence of some parameters on the determined elemental content is discussed. Standard reference materials IAEA-155 and IAEA-V-10 were used to assure quality control, accuracy and precision of the technique.

  18. The Comparison Study of Neutron Activation Analysis and Fission Track Technique for Uranium Determination

    International Nuclear Information System (INIS)

    Sirinuntavid, Alice; Rodthongkom, Chouvana

    2007-08-01

    Full text: Comparison between Neutron Activation Analysis (NAA) and fission track technique for uranium determination in solid samples was studied by use of standard reference materials, i.e., ore, coal fly ash, soil. For NAA, the epithermal neutron was applied for activated irradiation. Then, the 74.5 keV gamma from U-239 or 277.7 keV gamma from Np-239 was measured. For high Uranium content samples, NAA method with 74.5 keV gamma measurement, gave higher precision result than the 277.7 keV gamma measurement method. NAA method with 277.7 keV gamma measurement, gave higher sensitivity and precision result for low Uranium content samples and the uranium contained less than 10 ppm samples. Nevertheless, the latter procedure needed longer time for neutron irradiation and analysis procedure. In comparison the results of Uranium analysis between NAA and fission track, it was found that no significant difference within 95 % of confidence level

  19. Trace Analysis of Irradiated Granite Samples from Hiroshima by Laser Ablation Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Amr, M.A.; Helal, N.F.; Zahran, N.F.; Becker, J.S.; Pickhardt, C.; Dietze, H.J.

    1999-01-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is widely accepted as a rapid and sensitive technique for trace elemental analysis of solid materials and for local analysis of inhomogeneous materials (such as geological samples). Due to its direct solid sample analysis capability, LA-ICP-MS (using a quadrupole based ICP-MS and at the Research Center Juelich developed laser ablation system: Nd-YAG-laser, 226 nm, 10 Hz and 5 ns) is applied for the analysis of geological (granite) samples from Hiroshima. In order to prepare homogeneous targets, these samples were melted together with a lithium-borate mixture in a muffle furnace at 1050 degree c. Furthermore, for investigating of matrix effects the powder of these samples is mixed with graphite and pressed as targets for laser ablation. The quantification of the analysis results was carried out using granite (GM) as standard reference material. The relative sensitivity coefficients (RSCs) for most elements, which were determined for correction of the measured values, varied between 0.3 and 3

  20. Application of slip-band visualization technique to tensile analysis of laser-welded aluminum alloy

    Science.gov (United States)

    Muchiar, -; Yoshida, Sanichiro J.; Widiastuti, Rini; Kusnowo, A.; Takahashi, Kunimitsu; Sato, Shunichi

    1997-03-01

    Recently we have developed a new optical interferometric technique capable of visualizing slip band occurring in a deforming solid-state object. In this work we applied this technique to a tensile analysis of laser-welded aluminum plate samples, and successfully revealed stress concentration that shows strong relationships with the tensile strength and the fracture mechanism. We believe that this method is a new, convenient way to analyze the deformation characteristics of welded objects and evaluate the quality of welding. The analysis has been made for several types of aluminum alloys under various welding conditions, and has shown the following general results. When the penetration is deep, a slip band starts appearing at the fusion zone in an early stage of the elastic region of the strain-stress curve and stays there till the sample fractures at that point. When the penetration is shallow, a slip band appears only after the yield point and moves vigorously over the whole surface of the sample till a late stage of plastic deformation when the slip band stays at the fusion zone where the sample eventually fractures. When the penetration depth is medium, some intermediate situation of the above two extreme cases is observed.

  1. Elemental analysis of bead samples using a laser-induced plasma at low pressure

    International Nuclear Information System (INIS)

    Lie, Tjung Jie; Kurniawan, Koo Hendrik; Kurniawan, Davy P.; Pardede, Marincan; Suliyanti, Maria Margaretha; Khumaeni, Ali; Natiq, Shouny A.; Abdulmadjid, Syahrun Nur; Lee, Yong Inn; Kagawa, Kiichiro; Idris, Nasrullah; Tjia, May On

    2006-01-01

    An Nd:YAG laser (1064 nm, 8 ns, 30 mJ) was focused on various types of fresh, fossilized white coral and giant shell samples, including samples of imitation shell and marble. Such samples are extremely important as material for preparing prayer beads that are extensively used in the Buddhist faith. The aim of this research was to develop a non-destructive method to distinguish original beads from their imitations by means of spectral measurements of the carbon, hydrogen, sodium and magnesium emission intensities and by measuring the hardness of the sample using the ratio between Ca (II) 396.8 nm and Ca (I) 422.6 nm. Based on these measurements, original fresh coral beads can be distinguished from any imitation made from hard wood. The same technique was also effective in distinguishing beads made of shell from its imitation. A spectral analysis of bead was also performed on a fossilized white coral sample and the result can be used to distinguish to some extent the fossilized white coral beads from any imitation made from marble. It was also found that the plasma plume should be generated at low ambient pressure to significantly improve the hydrogen and carbon emission intensity and also to avoid energy loss inside the crater during laser irradiation at atmospheric pressure. The results of this study confirm that operating the laser-induced plasma spectroscopy at reduced ambient pressure offers distinct advantage for bead analysis over the conventional laser-induced breakdown spectroscopy (LIBS) technique operated at atmospheric pressure

  2. Elemental analysis of bead samples using a laser-induced plasma at low pressure

    Energy Technology Data Exchange (ETDEWEB)

    Lie, Tjung Jie [Research Center of Maju Makmur Mandiri Foundation, 40 Srengseng Raya, Kembangan, Jakarta Barat 11630 (Indonesia); Kurniawan, Koo Hendrik [Research Center of Maju Makmur Mandiri Foundation, 40 Srengseng Raya, Kembangan, Jakarta Barat 11630 (Indonesia)]. E-mail: kurnia18@cbn.net.id; Kurniawan, Davy P. [Research Center of Maju Makmur Mandiri Foundation, 40 Srengseng Raya, Kembangan, Jakarta Barat 11630 (Indonesia); Pardede, Marincan [Research Center of Maju Makmur Mandiri Foundation, 40 Srengseng Raya, Kembangan, Jakarta Barat 11630 (Indonesia); Suliyanti, Maria Margaretha [Graduate Program in Opto Electrotechniques and Laser Applications, Faculty of Engineering, The University of Indonesia, 4 Salemba Raya, Jakarta 10430 (Indonesia); Khumaeni, Ali [Department of Physics, Faculty of Mathematics and Natural Sciences, Diponegoro University, Tembalang Campus, Semarang 50275 (Indonesia); Natiq, Shouny A. [Department of Physics, Faculty of Mathematics and Natural Sciences, Diponegoro University, Tembalang Campus, Semarang 50275 (Indonesia); Abdulmadjid, Syahrun Nur [Department of Physics, Faculty of Mathematics and Natural Sciences, Syiah Kuala University, Darussalam, Banda Aceh 23116 (Indonesia); Lee, Yong Inn [Physics Department, Chonbuk National University, Chonju 561-756, South Korea (Korea); Kagawa, Kiichiro [Department of Physics, Faculty of Education and Regional Studies, Fukui University, 9-1 bunkyo 3-chome, Fukui 910-8507 (Japan); Idris, Nasrullah [Department of Physics, Faculty of Education and Regional Studies, Fukui University, 9-1 bunkyo 3-chome, Fukui 910-8507 (Japan); Tjia, May On [Department of Physics, Faculty of Mathematics and Natural Sciences, Bandung Institute of Technology, 10 Ganesha, Bandung 40132 (Indonesia)

    2006-01-15

    An Nd:YAG laser (1064 nm, 8 ns, 30 mJ) was focused on various types of fresh, fossilized white coral and giant shell samples, including samples of imitation shell and marble. Such samples are extremely important as material for preparing prayer beads that are extensively used in the Buddhist faith. The aim of this research was to develop a non-destructive method to distinguish original beads from their imitations by means of spectral measurements of the carbon, hydrogen, sodium and magnesium emission intensities and by measuring the hardness of the sample using the ratio between Ca (II) 396.8 nm and Ca (I) 422.6 nm. Based on these measurements, original fresh coral beads can be distinguished from any imitation made from hard wood. The same technique was also effective in distinguishing beads made of shell from its imitation. A spectral analysis of bead was also performed on a fossilized white coral sample and the result can be used to distinguish to some extent the fossilized white coral beads from any imitation made from marble. It was also found that the plasma plume should be generated at low ambient pressure to significantly improve the hydrogen and carbon emission intensity and also to avoid energy loss inside the crater during laser irradiation at atmospheric pressure. The results of this study confirm that operating the laser-induced plasma spectroscopy at reduced ambient pressure offers distinct advantage for bead analysis over the conventional laser-induced breakdown spectroscopy (LIBS) technique operated at atmospheric pressure.

  3. The use of the foil technique for the elimination of charging, and for beam monitoring in microbeam analysis of thick insulating samples

    International Nuclear Information System (INIS)

    Chaudhri, M.A.; Melbourne Univ., Austin

    1982-01-01

    It has been demonstrated that the 'thin-foil-technique' for the elimination of charging and accurate beam current/charge measurement, first developed by us, can also be conveniently applied to microbeam analysis of thick insulating samples. We have calculated the spatial broadening of proton microbeams of 1-20 MeV energies at the target, due to thin carbon foils of different thicknesses ranging from 10-40 μg/cm 2 placed either 2 or 5 mm in front of the target by using Moliere's theory of multiple scattering. The results show that at higher proton energies there is very little broadening of the incident beam even from thicker foils. But for lower energy protons (1 and 2 MeV) this broadening or worsening of the spatial resolution is relatively larger, especially from thicker foils. However, we have further shown that, even at these energies, the beam broadening can be minimized to acceptable limits by selecting a suitable thickness of carbon foil and placing it as close to the insulating target as possible. A comprehensive table is provided, which would help in selecting the most suitable carbon-foil thickness and the distance in front of the target where this foil should be placed, for microprobe application requiring different beam spots and proton energies. The advantages of this foil technique are described. (orig.)

  4. TV content analysis techniques and applications

    CERN Document Server

    Kompatsiaris, Yiannis

    2012-01-01

    The rapid advancement of digital multimedia technologies has not only revolutionized the production and distribution of audiovisual content, but also created the need to efficiently analyze TV programs to enable applications for content managers and consumers. Leaving no stone unturned, TV Content Analysis: Techniques and Applications provides a detailed exploration of TV program analysis techniques. Leading researchers and academics from around the world supply scientifically sound treatment of recent developments across the related subject areas--including systems, architectures, algorithms,

  5. Multielement analysis of aerosol samples by X-ray fluorescence analysis with totally reflecting sample holders

    International Nuclear Information System (INIS)

    Ketelsen, P.; Knoechel, A.

    1984-01-01

    Aerosole samples on filter support were analyzed using the X-ray flourescence analytical method (Mo excitation) with totally reflecting sample carrier (TXFA). Wet decomposition of the sample material with HNO 3 in an enclosed system and subsequent sample preparation by evaporating an aliquot of the solution on the sample carrier yields detection limits up to 0.3 ng/cm 2 . The reproducibilities of the measurements of the elements K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, As, Se, Rb, Sr, Ba and Pb lie between 5 and 25%. Similar detection limits and reproducibilities are obtained, when low-temperature oxygen plasma is employed for the direct ashing of the homogenously covered filter on the sample carrier. For the systematic loss of elements both methods were investigated with radiotracers as well as with inactive techniques. A comparison of the results with those obtained by NAA, AAS and PIXE shows good agreement in most cases. For the bromine determination and the fast coverage of the main elements a possibility for measuring the filter membrane has been indicated, which neglects the ashing step. The corresponding detection limits are up to 3 ng/cm 2 . (orig.) [de

  6. Multiplex Ligation-Dependent Probe Amplification Technique for Copy Number Analysis on Small Amounts of DNA Material

    DEFF Research Database (Denmark)

    Sørensen, Karina; Andersen, Paal; Larsen, Lars

    2008-01-01

    The multiplex ligation-dependent probe amplification (MLPA) technique is a sensitive technique for relative quantification of up to 50 different nucleic acid sequences in a single reaction, and the technique is routinely used for copy number analysis in various syndromes and diseases. The aim...... of the study was to exploit the potential of MLPA when the DNA material is limited. The DNA concentration required in standard MLPA analysis is not attainable from dried blood spot samples (DBSS) often used in neonatal screening programs. A novel design of MLPA probes has been developed to permit for MLPA...... analysis on small amounts of DNA. Six patients with congenital adrenal hyperplasia (CAH) were used in this study. DNA was extracted from both whole blood and DBSS and subjected to MLPA analysis using normal and modified probes. Results were analyzed using GeneMarker and manual Excel analysis. A total...

  7. Sample preparation and fractionation for proteome analysis and cancer biomarker discovery by mass spectrometry.

    Science.gov (United States)

    Ahmed, Farid E

    2009-03-01

    Sample preparation and fractionation technologies are one of the most crucial processes in proteomic analysis and biomarker discovery in solubilized samples. Chromatographic or electrophoretic proteomic technologies are also available for separation of cellular protein components. There are, however, considerable limitations in currently available proteomic technologies as none of them allows for the analysis of the entire proteome in a simple step because of the large number of peptides, and because of the wide concentration dynamic range of the proteome in clinical blood samples. The results of any undertaken experiment depend on the condition of the starting material. Therefore, proper experimental design and pertinent sample preparation is essential to obtain meaningful results, particularly in comparative clinical proteomics in which one is looking for minor differences between experimental (diseased) and control (nondiseased) samples. This review discusses problems associated with general and specialized strategies of sample preparation and fractionation, dealing with samples that are solution or suspension, in a frozen tissue state, or formalin-preserved tissue archival samples, and illustrates how sample processing might influence detection with mass spectrometric techniques. Strategies that dramatically improve the potential for cancer biomarker discovery in minimally invasive, blood-collected human samples are also presented.

  8. NID Copper Sample Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kouzes, Richard T.; Zhu, Zihua

    2011-09-12

    The current focal point of the nuclear physics program at PNNL is the MAJORANA DEMONSTRATOR, and the follow-on Tonne-Scale experiment, a large array of ultra-low background high-purity germanium detectors, enriched in 76Ge, designed to search for zero-neutrino double-beta decay (0νββ). This experiment requires the use of germanium isotopically enriched in 76Ge. The MAJORANA DEMONSTRATOR is a DOE and NSF funded project with a major science impact. The DEMONSTRATOR will utilize 76Ge from Russia, but for the Tonne-Scale experiment it is hoped that an alternate technology, possibly one under development at Nonlinear Ion Dynamics (NID), will be a viable, US-based, lower-cost source of separated material. Samples of separated material from NID require analysis to determine the isotopic distribution and impurities. DOE is funding NID through an SBIR grant for development of their separation technology for application to the Tonne-Scale experiment. The Environmental Molecular Sciences facility (EMSL), a DOE user facility at PNNL, has the required mass spectroscopy instruments for making isotopic measurements that are essential to the quality assurance for the MAJORANA DEMONSTRATOR and for the development of the future separation technology required for the Tonne-Scale experiment. A sample of isotopically separated copper was provided by NID to PNNL in January 2011 for isotopic analysis as a test of the NID technology. The results of that analysis are reported here. A second sample of isotopically separated copper was provided by NID to PNNL in August 2011 for isotopic analysis as a test of the NID technology. The results of that analysis are also reported here.

  9. Application of digital sampling techniques to particle identification in scintillation detectors

    International Nuclear Information System (INIS)

    Bardelli, L.; Bini, M.; Poggi, G.; Taccetti, N.

    2002-01-01

    In this paper, the use of a fast digitizing system for identification of fast charged particles with scintillation detectors is discussed. The three-layer phoswich detectors developed in the framework of the FIASCO experiment for the detection of light charged particles (LCP) and intermediate mass fragments (IMF) emitted in heavy-ion collisions at Fermi energies are briefly discussed. The standard analog electronics treatment of the signals for particle identification is illustrated. After a description of the digitizer designed to perform a fast digital sampling of the phoswich signals, the feasibility of particle identification on the sampled data is demonstrated. The results obtained with two different pulse shape discrimination analyses based on the digitally sampled data are compared with the standard analog signal treatment. The obtained results suggest, for the present application, the replacement of the analog methods with the digital sampling technique

  10. Attempts to develop a new nuclear measurement technique of β-glucuronidase levels in biological samples

    International Nuclear Information System (INIS)

    Unak, T.; Avcibasi, U.; Yildirim, Y.; Cetinkaya, B.

    2003-01-01

    β-Glucuronidase is one of the most important hydrolytic enzymes in living systems and plays an essential role in the detoxification pathway of toxic materials incorporated into the metabolism. Some organs, especially liver and some tumour tissues, have high level of β-glucuronidase activity. As a result the enzymatic activity of some kind of tumour cells, the radiolabelled glucuronide conjugates of cytotoxic, as well as radiotoxic compounds have potentially very valuable diagnostic and therapeutic applications in cancer research. For this reason, a sensitive measurement of β-glucuronidase levels in normal and tumour tissues is a very important step for these kinds of applications. According to the classical measurement method of β-glucuronidase activity, in general, the quantity of phenolphthalein liberated from its glucuronide conjugate, i.e. phenolphthalein-glucuronide, by β-glucuronidase has been measured by use of the spectrophotometric technique. The lower detection limit of phenolphthalein by the spectrophotometric technique is about 1-3 mg. This means that the β-glucuronidase levels could not be detected in biological samples having lower levels of β-glucuronidase activity and therefore the applications of the spectrophotometric technique in cancer research are very seriously limited. Starting from this consideration, we recently attempted to develop a new nuclear technique to measure much lower concentrations of β-glucuronidase in biological samples. To improve the detection limit, phenolphthalein-glucuronide and also phenyl-N-glucuronide were radioiodinated with 131 I and their radioactivity was measured by use of the counting technique. Therefore, the quantity of phenolphthalein or aniline radioiodinated with 131 I and liberated by the deglucuronidation reactivity of β-glucuronidase was used in an attempt to measure levels lower than the spectrophotometric measurement technique. The results obtained clearly verified that 0.01 pg level of

  11. 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

  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. PHOTOGRAMMETRIC TECHNIQUES FOR ROAD SURFACE ANALYSIS

    Directory of Open Access Journals (Sweden)

    V. A. Knyaz

    2016-06-01

    Full Text Available The quality and condition of a road surface is of great importance for convenience and safety of driving. So the investigations of the behaviour of road materials in laboratory conditions and monitoring of existing roads are widely fulfilled for controlling a geometric parameters and detecting defects in the road surface. Photogrammetry as accurate non-contact measuring method provides powerful means for solving different tasks in road surface reconstruction and analysis. The range of dimensions concerned in road surface analysis can have great variation from tenths of millimetre to hundreds meters and more. So a set of techniques is needed to meet all requirements of road parameters estimation. Two photogrammetric techniques for road surface analysis are presented: for accurate measuring of road pavement and for road surface reconstruction based on imagery obtained from unmanned aerial vehicle. The first technique uses photogrammetric system based on structured light for fast and accurate surface 3D reconstruction and it allows analysing the characteristics of road texture and monitoring the pavement behaviour. The second technique provides dense 3D model road suitable for road macro parameters estimation.

  14. Generation and Analysis of Constrained Random Sampling Patterns

    DEFF Research Database (Denmark)

    Pierzchlewski, Jacek; Arildsen, Thomas

    2016-01-01

    Random sampling is a technique for signal acquisition which is gaining popularity in practical signal processing systems. Nowadays, event-driven analog-to-digital converters make random sampling feasible in practical applications. A process of random sampling is defined by a sampling pattern, which...... indicates signal sampling points in time. Practical random sampling patterns are constrained by ADC characteristics and application requirements. In this paper, we introduce statistical methods which evaluate random sampling pattern generators with emphasis on practical applications. Furthermore, we propose...... algorithm generates random sampling patterns dedicated for event-driven-ADCs better than existed sampling pattern generators. Finally, implementation issues of random sampling patterns are discussed....

  15. Nuclear techniques for bulk ore analysis and their application to quality control

    International Nuclear Information System (INIS)

    Holmes, R.J.

    1981-01-01

    Bulk analysis techniques developed for the mining industry in which analyses are obtained directly from 3-30kg ore samples or from ore on conveyor belts are outlined. They include the determination of iron in iron ores from backscattered gamma radiation, shale in sedimentary iron ores from natural gamma activity, iron from a thermal-neutron capture reaction, and aluminium from the thermal neutron activation reaction

  16. Sample volume and alignment analysis for an optical particle counter sizer, and other applications

    International Nuclear Information System (INIS)

    Holve, D.J.; Davis, G.W.

    1985-01-01

    Optical methods for particle size distribution measurements in practical high temperature environments are approaching feasibility and offer significant advantages over conventional sampling methods. A key requirement of single particle counting techniques is the need to know features of the sample volume intensity distribution which in general are a function of the particle scattering properties and optical system geometry. In addition, the sample volume intensity distribution is sensitive to system alignment and thus calculations of alignment sensitivity are required for assessment of practical alignment tolerances. To this end, an analysis of sample volume characteristics for single particle counters in general has been developed. Results from the theory are compared with experimental measurements and shown to be in good agreement. A parametric sensitivity analysis is performed and a criterion for allowable optical misalignment is derived for conditions where beam steering caused by fluctuating refractive-index gradients is significant

  17. Comparative analysis of metal samples

    International Nuclear Information System (INIS)

    Lopez M, J.; Ramirez T, J.J.; Sandoval J, A.R.; Villasenor S, P.; Aspiazu F, J.A.

    2001-01-01

    Metal wastes were analysed to establish its origin with respect to a set of pieces. The elemental analysis was realized using the PIXE technique (Proton induced X-ray emission). Results are presented. (Author)

  18. Improved sampling and analysis of images in corneal confocal microscopy.

    Science.gov (United States)

    Schaldemose, E L; Fontain, F I; Karlsson, P; Nyengaard, J R

    2017-10-01

    Corneal confocal microscopy (CCM) is a noninvasive clinical method to analyse and quantify corneal nerve fibres in vivo. Although the CCM technique is in constant progress, there are methodological limitations in terms of sampling of images and objectivity of the nerve quantification. The aim of this study was to present a randomized sampling method of the CCM images and to develop an adjusted area-dependent image analysis. Furthermore, a manual nerve fibre analysis method was compared to a fully automated method. 23 idiopathic small-fibre neuropathy patients were investigated using CCM. Corneal nerve fibre length density (CNFL) and corneal nerve fibre branch density (CNBD) were determined in both a manual and automatic manner. Differences in CNFL and CNBD between (1) the randomized and the most common sampling method, (2) the adjusted and the unadjusted area and (3) the manual and automated quantification method were investigated. The CNFL values were significantly lower when using the randomized sampling method compared to the most common method (p = 0.01). There was not a statistical significant difference in the CNBD values between the randomized and the most common sampling method (p = 0.85). CNFL and CNBD values were increased when using the adjusted area compared to the standard area. Additionally, the study found a significant increase in the CNFL and CNBD values when using the manual method compared to the automatic method (p ≤ 0.001). The study demonstrated a significant difference in the CNFL values between the randomized and common sampling method indicating the importance of clear guidelines for the image sampling. The increase in CNFL and CNBD values when using the adjusted cornea area is not surprising. The observed increases in both CNFL and CNBD values when using the manual method of nerve quantification compared to the automatic method are consistent with earlier findings. This study underlines the importance of improving the analysis of the

  19. Constrained principal component analysis and related techniques

    CERN Document Server

    Takane, Yoshio

    2013-01-01

    In multivariate data analysis, regression techniques predict one set of variables from another while principal component analysis (PCA) finds a subspace of minimal dimensionality that captures the largest variability in the data. How can regression analysis and PCA be combined in a beneficial way? Why and when is it a good idea to combine them? What kind of benefits are we getting from them? Addressing these questions, Constrained Principal Component Analysis and Related Techniques shows how constrained PCA (CPCA) offers a unified framework for these approaches.The book begins with four concre

  20. Time-series-analysis techniques applied to nuclear-material accounting

    International Nuclear Information System (INIS)

    Pike, D.H.; Morrison, G.W.; Downing, D.J.

    1982-05-01

    This document is designed to introduce the reader to the applications of Time Series Analysis techniques to Nuclear Material Accountability data. Time series analysis techniques are designed to extract information from a collection of random variables ordered by time by seeking to identify any trends, patterns, or other structure in the series. Since nuclear material accountability data is a time series, one can extract more information using time series analysis techniques than by using other statistical techniques. Specifically, the objective of this document is to examine the applicability of time series analysis techniques to enhance loss detection of special nuclear materials. An introductory section examines the current industry approach which utilizes inventory differences. The error structure of inventory differences is presented. Time series analysis techniques discussed include the Shewhart Control Chart, the Cumulative Summation of Inventory Differences Statistics (CUSUM) and the Kalman Filter and Linear Smoother

  1. Quality assurance procedures for the analysis of TRU waste samples

    International Nuclear Information System (INIS)

    Glasgow, D.C. Giaquinto, J.M.; Robinson, L.

    1995-01-01

    The Waste Isolation Pilot Plant (WIPP) project was undertaken in response to the growing need for a national repository for transuranic (TRU) waste. Guidelines for WIPP specify that any waste item to be interred must be fully characterized and analyzed to determine the presence of chemical compounds designated hazardous and certain toxic elements. The Transuranic Waste Characterization Program (TWCP) was launched to develop analysis and quality guidelines, certify laboratories, and to oversee the actual waste characterizations at the laboratories. ORNL is participating in the waste characterization phase and brings to bear a variety of analytical techniques including ICP-AES, cold vapor atomic absorption, and instrumental neutron activation analysis (INAA) to collective determine arsenic, cadmium, barium, chromium, mercury, selenium, silver, and other elements. All of the analytical techniques involved participate in a cooperative effort to meet the project objectives. One important component of any good quality assurance program is determining when an alternate method is more suitable for a given analytical problem. By bringing to bear a whole arsenal of analytical techniques working toward common objectives, few analytical problems prove to be insurmountable. INAA and ICP-AES form a powerful pair when functioning in this cooperative manner. This paper will provide details of the quality assurance protocols, typical results from quality control samples for both INAA and ICP-AES, and detail method cooperation schemes used

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

    International Nuclear Information System (INIS)

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

    2002-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2002-07-01

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

  4. A comparison of transmission, reflection and photoacoustic FTIR techniques in the analysis of recycled and irradiated polyamide-6

    International Nuclear Information System (INIS)

    Evora, Maria C.; Goncalez, Odair L.

    2002-01-01

    A comparative study involving transmission, reflection and photoacoustic FTIR techniques is presented with analysis of polyamide-6. The potential and limitations of these methods are investigated by analyzing structural variations that take place at the surface in the bulk in recycled and irradiated polyamide-6 with a 1.5 MeV electron beam with a 500kGY dose, in the presence of O 2 . FTIR techniques appear to be sensitive in detecting small structural changes that occur in recycled and irradiated polyamide-6. The analysis of samples indicated the formation of OH, HOC=O-, - C=O groups. Also, small structural changes were detected which are characterisitic of NH and CN-C=O groups. Transmission techniques show better the structural changes in the bulk, and microscopy-FTIR appears to be more sensitive in detecting what occurs at the sample surface. (author)

  5. Rare earth analysis in human biological samples by atomic absorption using electrothermal atomization

    International Nuclear Information System (INIS)

    Citron, I.M.; Holtzman, R.B.; Leiman, J.

    1982-01-01

    The determination of Sc and seven rare earth elements, Nd, Sm, Dy, Ho, Eu, Tm, and Yb, in biological samplesby atomic absorption spectrophotometric analysis (AAS) using electrothermal atomization in a pyrolytic graphite tube is shown to be rapid, precise and accurate. The technique utilizes the method of standard additions and linear regression analysis to determine results from peak area data. Inter-elemental interferences are negligible. The elements found sensitive enough for this type of analysis are, in order of decreasing sensitivity, Yb, Eu, Tm, Dy, Sc, Ho, Sm and Nd. The determination in these types of materials of Gd and elements less sensitive to AAS detection than Gd does not appear to be feasible. Results are presented on the concentrations of these elements in 41 samples from human subjects, cows and vegetables with normal environmental exposure to the rare earth elements. The composite percent mean deviation in peak-area readings for all samples and all elements examined was 4%. The mean standard error in the results among samples was about 6.5%

  6. Applying a low energy HPGe detector gamma ray spectrometric technique for the evaluation of Pu/Am ratio in biological samples.

    Science.gov (United States)

    Singh, I S; Mishra, Lokpati; Yadav, J R; Nadar, M Y; Rao, D D; Pradeepkumar, K S

    2015-10-01

    The estimation of Pu/(241)Am ratio in the biological samples is an important input for the assessment of internal dose received by the workers. The radiochemical separation of Pu isotopes and (241)Am in a sample followed by alpha spectrometry is a widely used technique for the determination of Pu/(241)Am ratio. However, this method is time consuming and many times quick estimation is required. In this work, Pu/(241)Am ratio in the biological sample was estimated with HPGe detector based measurements using gamma/X-rays emitted by these radionuclides. These results were compared with those obtained from alpha spectroscopy of sample after radiochemical analysis and found to be in good agreement. Copyright © 2015 Elsevier Ltd. All rights reserved.

  7. Modern sample preparation techniques for gas chromatography-mass spectrometry analysis of environmental markers of chemical warfare agents use

    NARCIS (Netherlands)

    Terzic, O.; de Voogt, P.; Banoub, J.

    2014-01-01

    The chapter introduces problematics of on-site chemical analysis in the investigations of past chemical warfare agents (CWA) events. An overview of primary environmental degradation pathways of CWA leading to formation of chemical markers of their use is given. Conventional and modern sample

  8. Direct sampling technique of bees on Vriesea philippocoburgii (Bromeliaceae, Tillandsioideae flowers

    Directory of Open Access Journals (Sweden)

    Afonso Inácio Orth

    2004-11-01

    Full Text Available In our study on Vriesea philippocoburgii Wawra pollination, due to the small proportion of flowers in anthesis on a single day and the damage caused to inflorescences when netting directly on flowers, we used the direct sampling technique (DST of bees on flowers. This technique was applied to 40 flowering plants and resulted in the capture of 160 specimens, belonging to nine genera of Apoidea and separated into 19 morph species. As DST maintains the integrity of flowers for later Bees’ visits, it can enhance the survey’s performance, constituting an alternative methodology for the collection of bees visiting flowering plants.

  9. Analysis and analytical techniques

    Energy Technology Data Exchange (ETDEWEB)

    Batuecas Rodriguez, T [Department of Chemistry and Isotopes, Junta de Energia Nuclear, Madrid (Spain)

    1967-01-01

    ). For any analytical technique to be efficient two pre-requisites must be met: The sample must be truly representative; and the results must be available at the time when required. The papers mentioned here are PL-194/3, PL-194/4, PL-194/6, PL-194/7, PL-194/8 and PL-194/11, of which abstracts are given in Section III.

  10. Influence of sampling depth and post-sampling analysis time on the ...

    African Journals Online (AJOL)

    Bacteriological analysis was carried out for samples taken at water depth and at 1, 6, 12 and 24 hours post-sampling. It was observed that the total and faecal coliform bacteria were significantly higher in the 3 m water depth samples than in the surface water samples (ANOVA, F = 59.41, 26.751, 9.82 (T.C); 46.41, 26.81, ...

  11. An appraisal of neutron activation analysis and other analytical techniques for the determination of arsenic, selenium and tin in environmental samples

    International Nuclear Information System (INIS)

    Peterson, P.J.; Girling, C.A.; Klumpp, D.W.; Minski, M.J.

    1979-01-01

    The paper presents an experimental comparison between neutron activation analysis, atomic absorption spectrophotometry and fluorescence spectrophotometry used for the determination of trace amounts of As, Se and Sn and the other two analytical techniques mentioned. Gamma-ray spectrometry has been used to determine 76 As (tsub(1/2)=26.3 h) after 1 day's irradiation at a thermal neutron flux of 1.6x10 12 n.cm -2 .s -1 . High sensitivity was also obtained using an atomic absorption spectrophotometer coupled with covalent hydride generation. Advantages of the latter technique include simplicity of operation, high speed of analysis and negligible background correction. When used in conjuction with selective reduction and a cold-trap this method quantitatively distinguishes between the valence states and some methylated derivatives. Selenium has been analysed by gamma-ray spectrometry using 77 Sesup(m) (tsub(1/2)=17.5 s) after cyclic activation at a thermal neutron flux of 2x10 12 n.cm -2 .s -1 . Atomic absorption spectrophotometry following hydride generation, or fluorescence spectrophotometry of the 2,3 diaminonaphthalene complex constitute additional sensitive analytical methods for the determination of Se. These have the added advantage that valence states can be selectively measured. Low concentrations of Sn have been determined by neutron activation analysis and by spectrophotometric techniques using phenylfluorone as the complexing reagent, but these methods depend on selective extraction of Sn(IV) iodide. Whilst maintaining high sensitivity, these problems were avoided by using the hydride generation technique with an atomic absorption spectrophotometer. Comparative analytical values for Bowen's kale and NBS orchard leaves are presented

  12. [Applications of spectral analysis technique to monitoring grasshoppers].

    Science.gov (United States)

    Lu, Hui; Han, Jian-guo; Zhang, Lu-da

    2008-12-01

    Grasshopper monitoring is of great significance in protecting environment and reducing economic loss. However, how to predict grasshoppers accurately and effectively is a difficult problem for a long time. In the present paper, the importance of forecasting grasshoppers and its habitat is expounded, and the development in monitoring grasshopper populations and the common arithmetic of spectral analysis technique are illustrated. Meanwhile, the traditional methods are compared with the spectral technology. Remote sensing has been applied in monitoring the living, growing and breeding habitats of grasshopper population, and can be used to develop a forecast model combined with GIS. The NDVI values can be analyzed throughout the remote sensing data and be used in grasshopper forecasting. Hyper-spectra remote sensing technique which can be used to monitor grasshoppers more exactly has advantages in measuring the damage degree and classifying damage areas of grasshoppers, so it can be adopted to monitor the spatial distribution dynamic of rangeland grasshopper population. Differentialsmoothing can be used to reflect the relations between the characteristic parameters of hyper-spectra and leaf area index (LAI), and indicate the intensity of grasshopper damage. The technology of near infrared reflectance spectroscopy has been employed in judging grasshopper species, examining species occurrences and monitoring hatching places by measuring humidity and nutrient of soil, and can be used to investigate and observe grasshoppers in sample research. According to this paper, it is concluded that the spectral analysis technique could be used as a quick and exact tool in monitoring and forecasting the infestation of grasshoppers, and will become an important means in such kind of research for their advantages in determining spatial orientation, information extracting and processing. With the rapid development of spectral analysis methodology, the goal of sustainable monitoring

  13. Development of SYVAC sampling techniques

    International Nuclear Information System (INIS)

    Prust, J.O.; Dalrymple, G.J.

    1985-04-01

    This report describes the requirements of a sampling scheme for use with the SYVAC radiological assessment model. The constraints on the number of samples that may be taken is considered. The conclusions from earlier studies using the deterministic generator sampling scheme are summarised. The method of Importance Sampling and a High Dose algorithm, which are designed to preferentially sample in the high dose region of the parameter space, are reviewed in the light of experience gained from earlier studies and the requirements of a site assessment and sensitivity analyses. In addition the use of an alternative numerical integration method for estimating risk is discussed. It is recommended that the method of Importance Sampling is developed and tested for use with SYVAC. An alternative numerical integration method is not recommended for investigation at this stage but should be the subject of future work. (author)

  14. IDMS analysis of blank swipe samples for uranium quantity and isotopic composition

    International Nuclear Information System (INIS)

    Ryjinski, M.; Donohue, D.

    2001-01-01

    Since 1996 the IAEA has started routine implementation of environmental sampling. During the last 5 years more than 1700 swipe samples were collected and analyzed in the Network of Analytical Laboratories (NWAL). One sensitive point of analyzing environmental samples is evidence of the presence of enriched U. The U content on swipes is extremely low and therefore there is a relatively high probability of a false positive, e.g. small contamination or a measurement bias. In order to avoid and/or control this the IAEA systematically sends to the laboratories blind blank QC samples. In particular more than 50 blank samples were analyzed during the last two years. A preliminary analysis of blank swipes showed the swipe material itself contains up to 10 ng of NU per swipe. However, about 50% of blind blank swipes analyzed show the presence of enriched uranium. A source of this bias has to be clarified and excluded. This paper presents the results of modeling of IDMS analysis for quantity and isotopic composition of uranium in order to identify the possible contribution of different factors to the final measurement uncertainty. This modeling was carried out based on the IAEA Clean Laboratory measurement data and simulation technique

  15. Comparison of PIXE and XRF analysis of airborne particulate matter samples collected on Teflon and quartz fibre filters

    Science.gov (United States)

    Chiari, M.; Yubero, E.; Calzolai, G.; Lucarelli, F.; Crespo, J.; Galindo, N.; Nicolás, J. F.; Giannoni, M.; Nava, S.

    2018-02-01

    Within the framework of research projects focusing on the sampling and analysis of airborne particulate matter, Particle Induced X-ray Emission (PIXE) and Energy Dispersive X-ray Fluorescence (ED-XRF) techniques are routinely used in many laboratories throughout the world to determine the elemental concentration of the particulate matter samples. In this work an inter-laboratory comparison of the results obtained from analysing several samples (collected on both Teflon and quartz fibre filters) using both techniques is presented. The samples were analysed by PIXE (in Florence, at the 3 MV Tandetron accelerator of INFN-LABEC laboratory) and by XRF (in Elche, using the ARL Quant'X EDXRF spectrometer with specific conditions optimized for specific groups of elements). The results from the two sets of measurements are in good agreement for all the analysed samples, thus validating the use of the ARL Quant'X EDXRF spectrometer and the selected measurement protocol for the analysis of aerosol samples. Moreover, thanks to the comparison of PIXE and XRF results on Teflon and quartz fibre filters, possible self-absorption effects due to the penetration of the aerosol particles inside the quartz fibre-filters were quantified.

  16. 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

  17. Analysis of wastewater samples by direct combination of thin-film microextraction and desorption electrospray ionization mass spectrometry.

    Science.gov (United States)

    Strittmatter, Nicole; Düring, Rolf-Alexander; Takáts, Zoltán

    2012-09-07

    An analysis method for aqueous samples by the direct combination of C18/SCX mixed mode thin-film microextraction (TFME) and desorption electrospray ionization mass spectrometry (DESI-MS) was developed. Both techniques make analytical workflow simpler and faster, hence the combination of the two techniques enables considerably shorter analysis time compared to the traditional liquid chromatography mass spectrometry (LC-MS) approach. The method was characterized using carbamazepine and triclosan as typical examples for pharmaceuticals and personal care product (PPCP) components which draw increasing attention as wastewater-derived environmental contaminants. Both model compounds were successfully detected in real wastewater samples and their concentrations determined using external calibration with isotope labeled standards. Effects of temperature, agitation, sample volume, and exposure time were investigated in the case of spiked aqueous samples. Results were compared to those of parallel HPLC-MS determinations and good agreement was found through a three orders of magnitude wide concentration range. Serious matrix effects were observed in treated wastewater, but lower limits of detection were still found to be in the low ng L(-1) range. Using an Orbitrap mass spectrometer, the technique was found to be ideal for screening purposes and led to the detection of various different PPCP components in wastewater treatment plant effluents, including beta-blockers, nonsteroidal anti-inflammatory drugs, and UV filters.

  18. Multielemental speciation analysis by advanced hyphenated technique - HPLC/ICP-MS: A review.

    Science.gov (United States)

    Marcinkowska, Monika; Barałkiewicz, Danuta

    2016-12-01

    Speciation analysis has become an invaluable tool in human health risk assessment, environmental monitoring or food quality control. Another step is to develop reliable multielemental speciation methodologies, to reduce costs, waste and time needed for the analysis. Separation and detection of species of several elements in a single analytical run can be accomplished by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Our review assembles articles concerning multielemental speciation determination of: As, Se, Cr, Sb, I, Br, Pb, Hg, V, Mo, Te, Tl, Cd and W in environmental, biological, food and clinical samples analyzed with HPLC/ICP-MS. It addresses the procedures in terms of following issues: sample collection and pretreatment, selection of optimal conditions for elements species separation by HPLC and determination using ICP-MS as well as metrological approach. The presented work is the first review article concerning multielemental speciation analysis by advanced hyphenated technique HPLC/ICP-MS. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Validation of methods for WDXRF and OES-spark techniques in steel analysis. Determination of the uncertainty of measurements for API steel plant sample

    International Nuclear Information System (INIS)

    Silva, Carlos Eduardo da

    2009-01-01

    The increase of gas and petroleum demanding in the national and international markets, the specification and certification of the chemical analysis results of gas and oil pipe-line have became more and more challenging. A continuous development has been outlined to improve API grade alloy steels (American Petroleum Institute). The steel properties depend on the chemical composition control and process parameters during its manufacturing. In this work, a comparison of the measurement uncertainty between X-ray fluorescence (WD system) and Optical Emission (OES-spark) spectrometry, for API grade steel plant samples analysis, was outlined. Usually, this kind of analyze requires less than 40 seconds for full chemical characterization for adjustment in the process parameters production. The main influence source in the chemical analysis was evaluated for design of experiments. The constituents and trace elements such as Al, Si, P, S, Ti, V, Cr, Mn, Co, Ni, Cu, As, Nb, Mo and Sn were determined using the ASTM E-322, E-415, E-1009 and E-1085 standard methodologies. The 185A and 187A certified reference materials from CMI (Czech Metrology Institute) were used for evaluation of the methods. The uncertainty of the measurement, precision, accuracy, repeatability and reproducibility of the measurements were obtained applying statistic tests, recommended by ISO/IEC 17025. The uncertainty of measurement for each element is discussed for both techniques. (author)

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

    International Nuclear Information System (INIS)

    Marske, S.G.

    1996-07-01

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

  1. Radiochemical analysis of phosphorus in milk samples

    International Nuclear Information System (INIS)

    Oliveira, R.M. de; Cunha, I.I.L.

    1991-01-01

    The determination of phosphorus in milk samples by thermal neutron activation analysis employing radiochemical separation is described. The radiochemical separation consists of the simultaneous irradiation of samples and standards, dissolution of the milk samples in a perchloric acid and nitric acid mixture, addition of zinc hold-back carrier, precipitation of phosphorus as ammonium phospho molybdate (A.M.P.) and sample counting in a Geiger-Mueller detector. The analysis sources of error were studied and the established method was applied to phosphorus analyses in commercial milk samples. (author)

  2. [Establishment and assessment of QA/QC method for sampling and analysis of atmosphere background CO2].

    Science.gov (United States)

    Liu, Li-xin; Zhou, Ling-xi; Xia, Ling-jun; Wang, Hong-yang; Fang, Shuang-xi

    2014-12-01

    To strengthen scientific management and sharing of greenhouse gas data obtained from atmospheric background stations in China, it is important to ensure the standardization of quality assurance and quality control method for background CO2 sampling and analysis. Based on the greenhouse gas sampling and observation experience of CMA, using portable sampling observation and WS-CRDS analysis technique as an example, the quality assurance measures for atmospheric CO,sampling and observation in the Waliguan station (Qinghai), the glass bottle quality assurance measures and the systematic quality control method during sample analysis, the correction method during data processing, as well as the data grading quality markers and data fitting interpolation method were systematically introduced. Finally, using this research method, the CO2 sampling and observation data at the atmospheric background stations in 3 typical regions were processed and the concentration variation characteristics were analyzed, indicating that this research method could well catch the influences of the regional and local environmental factors on the observation results, and reflect the characteristics of natural and human activities in an objective and accurate way.

  3. Multielemental analysis of milk samples

    International Nuclear Information System (INIS)

    Omar Al-Dayel; Jameel Al-Hefne; Didarul A Chowdhury; Turki Al-Ajyan

    2002-01-01

    Milk is a basic food since it provides essential nutrients (proteins, lipids, carbohydrates) and micronutrients (minerals, Vitamins, enzymes). In fact, in formula milk essential elements have been usually added in order to satisfy nutritional requirements. However, too high additions of these elements can produce detrimental effects on human health. More important, milk can also constitute a source of exposure to toxic elements, especially dangerous for infants. Method is presented for the multielemental analysis of a wide range of elements in milk samples. The aim of this work is the development of a multielemental method for the analysis of major, minor and trace essential and toxic elements in milk. Several milk samples with different origins were collected from the Saudi Arabia markets and analyzed by Inductively Coupled Plasma Mass Spectrometer (ICP-MS). For preparation of the samples for analysis, they were digested by closed vessel microwave digestion system with H 2 O 2 /HNO 3 . About 40 elements were determined. A reference material was analysed for the validation of the proposed method. (Author)

  4. Analysis of formalin-fixed, paraffin-embedded (FFPE) tissue via proteomic techniques and misconceptions of antigen retrieval.

    Science.gov (United States)

    O'Rourke, Matthew B; Padula, Matthew P

    2016-01-01

    Since emerging in the late 19(th) century, formaldehyde fixation has become a standard method for preservation of tissues from clinical samples. The advantage of formaldehyde fixation is that fixed tissues can be stored at room temperature for decades without concern for degradation. This has led to the generation of huge tissue banks containing thousands of clinically significant samples. Here we review techniques for proteomic analysis of formalin-fixed, paraffin-embedded (FFPE) tissue samples with a specific focus on the methods used to extract and break formaldehyde crosslinks. We also discuss an error-of-interpretation associated with the technique known as "antigen retrieval." We have discovered that this term has been mistakenly applied to two disparate molecular techniques; therefore, we argue that a terminology change is needed to ensure accurate reporting of experimental results. Finally, we suggest that more investigation is required to fully understand the process of formaldehyde fixation and its subsequent reversal.

  5. Trace elements detection in whole food samples by Neutron Activation Analysis, k0-method

    International Nuclear Information System (INIS)

    Sathler, Márcia Maia; Menezes, Maria Ângela de Barros Correia; Salles, Paula Maria Borges de

    2017-01-01

    Inorganic elements, from natural and anthropogenic sources are present in foods in different concentrations. With the increase in anthropogenic activities, there was also a considerable increase in the emission of these elements in the environment, leading to the need of monitoring the elemental composition of foods available for consumption. Numerous techniques have been used to detect inorganic elements in biological and environmental matrices, always aiming at reaching lower detection limits in order to evaluate the trace element content in the sample. Neutron activation analysis (INAA), applying the k 0 -method, produces accurate and precise results without the need of chemical preparation of the samples – that could cause their contamination. This study evaluated the presence of inorganic elements in whole foods samples, mainly elements on trace levels. For this purpose, seven samples of different types of whole foods were irradiated in the TRIGA MARK I IPR-R1 research reactor - located at CDTN/CNEN, in Belo Horizonte, MG. It was possible to detect twenty two elements above the limit of detection in, at least, one of the samples analyzed. This study reaffirms the INAA, k 0 - method, as a safe and efficient technique for detecting trace elements in food samples. (author)

  6. Comparison of Techniques for Sampling Adult Necrophilous Insects From Pig Carcasses.

    Science.gov (United States)

    Cruise, Angela; Hatano, Eduardo; Watson, David W; Schal, Coby

    2018-02-06

    Studies of the pre-colonization interval and mechanisms driving necrophilous insect ecological succession depend on effective sampling of adult insects and knowledge of their diel and successional activity patterns. The number of insects trapped, their diversity, and diel periodicity were compared with four sampling methods on neonate pigs. Sampling method, time of day and decomposition age of the pigs significantly affected the number of insects sampled from pigs. We also found significant interactions of sampling method and decomposition day, time of sampling and decomposition day. No single method was superior to the other methods during all three decomposition days. Sampling times after noon yielded the largest samples during the first 2 d of decomposition. On day 3 of decomposition however, all sampling times were equally effective. Therefore, to maximize insect collections from neonate pigs, the method used to sample must vary by decomposition day. The suction trap collected the most species-rich samples, but sticky trap samples were the most diverse, when both species richness and evenness were factored into a Shannon diversity index. Repeated sampling during the noon to 18:00 hours period was most effective to obtain the maximum diversity of trapped insects. The integration of multiple sampling techniques would most effectively sample the necrophilous insect community. However, because all four tested methods were deficient at sampling beetle species, future work should focus on optimizing the most promising methods, alone or in combinations, and incorporate hand-collections of beetles. © The Author(s) 2018. Published by Oxford University Press on behalf of Entomological Society of America. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  7. Emanation thermal analysis. Principle of the method, preparation of samples and apparatus

    International Nuclear Information System (INIS)

    Balek, V.; Pentinghaus, H.J.

    1993-12-01

    Principles of the title method are outlined and the sample preparation procedures and instrumental designs are described. The publication is divided into chapters as follows: (I) Introduction; (II) Sample labelling: (II.1) Introducing parent nuclides as a source of inert gas in solid; Distribution of inert gas in the sample; (II.2) Introducing inert gases without parent nuclides (using the recoil effect of nuclear reactions and using ion bombardment); (II.3) Choice of the suitable labelling technique; (III) Equipment for emanation thermal analysis: (III.1) Inert gas detection and measurement of inert gas release rate; (III.2) System of carrier gas flow and stabilization; (IV) Determination of the optimal conditions for radon release rate measurement; (V) Example of ETA measurement. (P.A.). 1 tab., 10 figs. 5 refs

  8. Design and building of a homemade sample changer for automation of the irradiation in neutron activation analysis technique; Diseno y construccion de un prototipo de intercambiador para la automatizacion de la tecnica de analisis por activacion neutronica

    Energy Technology Data Exchange (ETDEWEB)

    Gago, Javier; Hernandez, Yuri; Baltuano, Oscar; Bedregal, Patricia [Direccion de Investigacion y Desarrollo, Instituto Peruano de Energia Nuclear, Lima (Peru); Lopez, Yon [Universidad Nacional de Ingenieria, Lima (Peru); Urquizo, Rafael [Universidad Tecnologica del Peru, Lima (Peru)

    2014-07-01

    Because the RP-10 research reactor operates during weekends, it was necessary to design and build a sample changer for irradiation as part of the automation process of neutron activation analysis technique. The device is formed by an aluminum turntable disk which can accommodate 19 polyethylene capsules, containing samples to be sent using the pneumatic transfer system from the laboratory to the irradiation position. The system is operate by a control switchboard to send and return capsules in a variable preset time and by two different ways, allowing the determination of short, medium and long lived radionuclides. Also another mechanism is designed called 'exchange valve' for changing travel paths (pipelines) allowing the irradiated samples to be stored for a longer time in the reactor hall. The system design has allowed complete automation of this technique, enabling the irradiation of samples without the presence of an analyst. The design, construction and operation of the device is described and presented in this article. (authors).

  9. Analysis of chlorpheniramine in human urine samples using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Mehdi Maham

    2014-09-01

    Full Text Available A simple and environmentally friendly microextraction technique was used for determination of chlorpheniramine (CPM, an antihistamine drug, in human urine samples using dispersive liquid-liquid microextraction (DLLME followed by high performance liquid chromatography with diode array detection (HPLC-DAD. In this extraction technique, an appropriate mixture of acetonitrile (disperser solvent and carbon tetrachloride (extraction solvent was rapidly injected into the urine sample containing the target analyte. Tiny droplets of extractant were formed and dispersed into the sample solution and then sedimented at the bottom of the conical test tube by centrifugation. Under optimal conditions, the calibration curve was linear in the range of 0.055-5.5 µg mL-1, with a detection limit of 16.5 ng mL-1. This proposed method was successfully applied to the analysis of real urine samples. Low consumption of toxic organic solvents, simplicity of operation, low cost and acceptable figures of merit are the main advantages of the proposed technique.

  10. Sample Data Synchronization and Harmonic Analysis Algorithm Based on Radial Basis Function Interpolation

    Directory of Open Access Journals (Sweden)

    Huaiqing Zhang

    2014-01-01

    Full Text Available The spectral leakage has a harmful effect on the accuracy of harmonic analysis for asynchronous sampling. This paper proposed a time quasi-synchronous sampling algorithm which is based on radial basis function (RBF interpolation. Firstly, a fundamental period is evaluated by a zero-crossing technique with fourth-order Newton’s interpolation, and then, the sampling sequence is reproduced by the RBF interpolation. Finally, the harmonic parameters can be calculated by FFT on the synchronization of sampling data. Simulation results showed that the proposed algorithm has high accuracy in measuring distorted and noisy signals. Compared to the local approximation schemes as linear, quadric, and fourth-order Newton interpolations, the RBF is a global approximation method which can acquire more accurate results while the time-consuming is about the same as Newton’s.

  11. Comparative study between the PIXE technique and neutron activation analysis for Zinc determination

    International Nuclear Information System (INIS)

    Cruvinel, Paulo Estevao; Crestana, Silvio; Artaxo Netto, Paulo Eduardo

    1997-01-01

    This work presents a comparative study between the PIXE, proton beams and neutron activation analysis (NAA) techniques, for determination of total zinc concentration. Particularly, soil samples from the Pindorama, Instituto Agronomico de Campinas, Sao Paulo State, Brazil, experimental station have been analysed and measuring the zinc contents in μg/g. The results presented good correlation between the mentioned techniques. The PIXE and NAA analyses have been carried out by using the series S, 2.4 MeV proton beams Pelletron accelerator and the IPEN/CNEN-IEA-R1 reactor, both installed at the Sao Paulo - Brazil university

  12. Human mixed lymphocyte cultures. Evaluation of microculture technique utilizing the multiple automated sample harvester (MASH)

    Science.gov (United States)

    Thurman, G. B.; Strong, D. M.; Ahmed, A.; Green, S. S.; Sell, K. W.; Hartzman, R. J.; Bach, F. H.

    1973-01-01

    Use of lymphocyte cultures for in vitro studies such as pretransplant histocompatibility testing has established the need for standardization of this technique. A microculture technique has been developed that has facilitated the culturing of lymphocytes and increased the quantity of cultures feasible, while lowering the variation between replicate samples. Cultures were prepared for determination of tritiated thymidine incorporation using a Multiple Automated Sample Harvester (MASH). Using this system, the parameters that influence the in vitro responsiveness of human lymphocytes to allogeneic lymphocytes have been investigated. PMID:4271568

  13. Issues in the analyze of low content gold mining samples by fire assay technique

    Science.gov (United States)

    Cetean, Valentina

    2016-04-01

    The classic technique analyze of samples with low gold content - below 0.1 g/t (=100 ppb = parts per billion), either ore or gold sediments, involves the preparation of sample by fire assay extraction, followed by the chemical attack with aqua regia (hydrochloric and nitric acid) and measuring the gold content by atomic absorption spectrometry or inductively coupled mass spectrometry. The issues raised by this analysis are well known for the world laboratories, commercial or research ones. The author's knowledge regarding this method of determining the gold content, accumulated in such laboratory from Romania (with more than 40 years of experience, even if not longer available from 2014) confirms the obtaining of reliable results required a lot of attention, amount of work and the involving of an experienced fire assayer specialist. The analytical conclusion for a research laboratory is that most reliable and statistically valid results are till reached for samples with more than 100 ppb gold content; the degree of confidence below this value is lower than 90%. Usually, for samples below 50 ppb, it does not exceed 50-70 %, unless without very strictly control of each stage, that involve additional percentage of hours allocated for successive extracting tests and knowing more precisely the other compounds that appear in the sample (Cu, Sb, As, sulfur / sulphides, Te, organic matter, etc.) or impurities. The most important operation is the preparation, namely: - grinding and splitting of sample (which can cause uneven distribution of gold flakes in the double samples for analyzed); - pyro-metallurgical recovery of gold = fire assay stage, involving the more precise temperature control in furnace during all stages (fusion and cupellation) and adjusting of the fire assay flux components to produce a successful fusion depending of the sample matrix and content; - reducing the sample weight to decrease the amount of impurities that can be concentrated in the lead button

  14. [Influence of Natural Dissolved Organic Matter on the Passive Sampling Technique and its Application].

    Science.gov (United States)

    Yu, Shang-yun; Zhou, Yan-mei

    2015-08-01

    This paper studied the effects of different concentrations of natural dissolved organic matter (DOM) on the passive sampling technique. The results showed that the presence of DOM affected the organic pollutant adsorption ability of the membrane. For lgK(OW), 3-5, DOM had less impact on the adsorption of organic matter by the membrane; for lgK(OW), > 5.5, DOM significantly increased the adsorption capacity of the membrane. Meanwhile, LDPE passive sampling technique was applied to monitor PAHs and PAEs in pore water of three surface sediments in Taizi River. All of the target pollutants were detected in varying degrees at each sampling point. Finally, the quotient method was used to assess the ecological risks of PAHs and PAEs. The results showed that fluoranthene exceeded the reference value of the aquatic ecosystem, meaning there was a big ecological risk.

  15. Investigations on the comparator technique used in epithermal neutron activation analysis

    International Nuclear Information System (INIS)

    Bereznai, T.; Bodizs, D.; Keoemley, G.

    1977-01-01

    The possible extension of the comparator technique of reactor neutron activation analysis into the field of epithermal neutron activation has been investigated. Ruthenium was used for multi-isotopic comparator. Experiments show that conversion of the so-called reference k-factors - determined by irradiation with reactor neutrons - into ksup(epi)-factors usable at activation under cadmium filter, can be evaluated with fair accuracy. Sources and extent of errors and their contribution to the final error of analysis are discussed. For equal irradiation and counting times advantage of ENAA for several elements is obvious: the much lower background activity permitted the sample to be measured closer to the detector, under better geometry conditions, consequently, permitting several elements to be determined quantitatively. The number of elements determined and the sensitivity of the method are much dependent on the experimental conditions, especially on the composition of the sample, on the PHIsub(e) value, the irradiation time and the efficiency of the Ge(Li) detector. (T.G.)

  16. Nested sampling as a tool for LISA data analysis

    International Nuclear Information System (INIS)

    Gair, Jonathan R; Feroz, Farhan; Graff, Philip; Hobson, Michael P; Babak, Stanislav; Petiteau, Antoine; Porter, Edward K

    2010-01-01

    Nested sampling is a technique for efficiently computing the probability of a data set under a particular hypothesis, also called the Bayesian Evidence or Marginal Likelihood, and for evaluating the posterior. MULTINEST is a multi-modal nested sampling algorithm which has been designed to efficiently explore and characterize posterior probability surfaces containing multiple secondary solutions. We have applied the MULTINEST algorithm to a number of problems in gravitational wave data analysis. In this article, we describe the algorithm and present results for several applications of the algorithm to analysis of mock LISA data. We summarise recently published results for a test case in which we searched for two non-spinning black hole binary merger signals in simulated LISA data. We also describe results obtained with MULTINEST in the most recent round of the Mock LISA Data Challenge (MLDC), in which the algorithm was used to search for and characterise both spinning supermassive black hole binary inspirals and bursts from cosmic string cusps. In all these applications, the algorithm found the correct number of signals and efficiently recovered the posterior probability distribution. Moreover, in most cases the waveform corresponding to the best a-posteriori parameters had an overlap in excess of 99% with the true signal.

  17. Nested sampling as a tool for LISA data analysis

    Energy Technology Data Exchange (ETDEWEB)

    Gair, Jonathan R [Institute of Astronomy, Madingley Road, CB3 0HA, Cambridge (United Kingdom); Feroz, Farhan; Graff, Philip; Hobson, Michael P [Astrophysics Group, Cavendish Laboratory, JJ Thomson Avenue, Cambridge CB3 0HE (United Kingdom); Babak, Stanislav; Petiteau, Antoine [Max-Planck-Institut fuer Gravitationsphysik, Am Muehlenberg 1, 14476, Potsdam (Germany); Porter, Edward K, E-mail: jgair@ast.cam.ac.u [APC, UMR 7164, Universite Paris 7 Denis Diderot, 10, rue Alice Domon et Leonie Duquet, 75205 Paris Cedex 13 (France)

    2010-05-01

    Nested sampling is a technique for efficiently computing the probability of a data set under a particular hypothesis, also called the Bayesian Evidence or Marginal Likelihood, and for evaluating the posterior. MULTINEST is a multi-modal nested sampling algorithm which has been designed to efficiently explore and characterize posterior probability surfaces containing multiple secondary solutions. We have applied the MULTINEST algorithm to a number of problems in gravitational wave data analysis. In this article, we describe the algorithm and present results for several applications of the algorithm to analysis of mock LISA data. We summarise recently published results for a test case in which we searched for two non-spinning black hole binary merger signals in simulated LISA data. We also describe results obtained with MULTINEST in the most recent round of the Mock LISA Data Challenge (MLDC), in which the algorithm was used to search for and characterise both spinning supermassive black hole binary inspirals and bursts from cosmic string cusps. In all these applications, the algorithm found the correct number of signals and efficiently recovered the posterior probability distribution. Moreover, in most cases the waveform corresponding to the best a-posteriori parameters had an overlap in excess of 99% with the true signal.

  18. The Use of Multi-Criteria Decision Analysis Weight Elicitation Techniques in Patients with Mild Cognitive Impairment

    NARCIS (Netherlands)

    van Til, Janine Astrid; Dolan, James G.; Stiggelbout, Anne M.; Groothuis-Oudshoorn, Catharina Gerarda Maria; IJzerman, Maarten Joost

    2008-01-01

    Objective: To test the applicability of multi-criteria decision analysis preference elicitation techniques in cognitively impaired individuals. - Method: A convenience sample of 16 cognitively impaired subjects and 12 healthy controls was asked to participate in a small pilot study. The subjects

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

    Directory of Open Access Journals (Sweden)

    Helena Prosen

    2014-05-01

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

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

    Science.gov (United States)

    Prosen, Helena

    2014-05-23

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

  1. Major and minor elements analysis in soil samples by neutron activation analysis and X-ray fluorescence

    International Nuclear Information System (INIS)

    Morcelli, Claudia Petronilho Ribeiro; Ana Maria Graciano; Enzweiler, Jacinta

    2002-01-01

    In the present work, Instrumental Neutron Activation Analysis (INAA) and X-Ray Fluorescence were employed to analyze major and minor elements in soil samples collected near Bandeirantes road. Elements of environmental interest, such as Al, Sb, As, Ba, Cd, Pb, Co, Cu, Cr, Fe, Mn, Mo, Ni, Se, V and Zn, which have reference background levels, were determined. The samples were dried in an oven at 40 deg C, were sieved (<2 mm), grinded and were analyzed by INAA and FRX. The aims of this work were: to evaluate the possible variations in the concentration levels in soil due to emission of particulate from vehicles and other anthropogenic sources; to compare the results obtained by using both techniques. This preliminary study showed that the concentration levels of the elements of environmental interest agree with reference values for tropical soils in the sampling sites, except for Ba, which presented higher values. (author)

  2. Effect of rootstock on the scion of Hevea brasiliensis through metabolic analysis of latex samples by 1H NMR

    Directory of Open Access Journals (Sweden)

    Eduardo Sanches Pereira do Nascimento

    2011-01-01

    Full Text Available In this study, the effect of rootstock on grafting through metabolomic analysis of latex (Hevea brasiliensis samples was verified by 1H nuclear magnetic resonance (NMR and multivariate data analysis. Sixteen metabolites present in the latex cytosol were characterized by NMR. PCA analysis showed that the latex samples of the RR and GR groups can be differentiated. The GR group samples present a metabolic profile similar to the RR group samples, while the RG group is in an intermediate position between RR and GG groups. Sucrose and formate contributed greatly to the separation obtained by PCA, presenting a good correlation between the results. 1H NMR was an efficient technique to differentiate latex samples from different types of rootstocks and grafting and in the future could be used to predict rubber production by latex analysis.

  3. Anodic electrode position of cyanometallates as sample preparation for the determination of transition metals from water samples using X-ray fluorescence analysis

    International Nuclear Information System (INIS)

    Wundt, K.; Duschner, H.; Starke, K.

    1978-01-01

    The anodic separation of cyanometallates of propanol -2/Water mixtures at high electrical field strengths was developed as new technique for sample preparation. The optimization of the parameters of the system (high voltage applied, current density, separation time and composition of the solution) resulted in quantitative precipitation of the metallates of Fe, Co, Ni, Cu, Zn, Cd and Ag in homogeneous, thin and strong-adhering layer with mass densities of between 1 nmol cm -2 and 1 μmol cm -2 on high-purity aluminium foils. Metals not forming anionic complexes remain in solution with simualtaneous quantitative multielement separation. The described technique is part of a method to determine heavy metal traces in water samples. It comprises the nonspecific sorption on cation exchangers, the elution of the transition metals as cyanometallates, their electrode position on aluminium foil and the determination by X-ray fluorescence analysis. Model experiments illustrate the possible applications of the method. (orig.) [de

  4. Diurnal activity of four species of thrips (Thysanoptera: Thripidae) and efficiencies of three nondestructive sampling techniques for thrips in mango inflorescences.

    Science.gov (United States)

    Aliakbarpour, H; Rawi, Che Salmah Md

    2010-06-01

    Thrips cause considerable economic loss to mango, Mangifera indica L., in Penang, Malaysia. Three nondestructive sampling techniques--shaking mango panicles over a moist plastic tray, washing the panicles with ethanol, and immobilization of thrips by using CO2--were evaluated for their precision to determine the most effective technique to capture mango flower thrips (Thysanoptera: Thripidae) in an orchard located at Balik Pulau, Penang, Malaysia, during two flowering seasons from December 2008 to February 2009 and from August to September 2009. The efficiency of each of the three sampling techniques was compared with absolute population counts on whole panicles as a reference. Diurnal flight activity of thrips species was assessed using yellow sticky traps. All three sampling methods and sticky traps were used at two hourly intervals from 0800 to 1800 hours to get insight into diurnal periodicity of thrips abundance in the orchard. Based on pooled data for the two seasons, the CO2 method was the most efficient procedure extracting 80.7% adults and 74.5% larvae. The CO2 method had the lowest relative variation and was the most accurate procedure compared with the absolute method as shown by regression analysis. All collection techniques showed that the numbers of all thrips species in mango panicles increased after 0800 hours, reaching a peak between 1200 and 1400 hours. Adults thrips captured on the sticky traps were the most abundant between 0800-1000 and 1400-1600 hours. According to results of this study, the CO2 method is recommended for sampling of thrips in the field. It is a nondestructive sampling procedure that neither damages flowers nor diminishes fruit production. Management of thrips populations in mango orchards with insecticides would be more effectively carried out during their peak population abundance on the flower panicles at midday to 1400 hours.

  5. Ergonomic analysis of radiopharmaceuticals samples preparation process

    International Nuclear Information System (INIS)

    Gomes, Luciene Betzler C.; Santos, Isaac Luquetti dos; Fonseca, Antonio Carlos C. da; Pellini, Marcos Pinto; Rebelo, Ana Maria

    2005-01-01

    The doses of radioisotopes to be administrated in patients for diagnostic effect or therapy are prepared in the radiopharmacological sector. The preparation process adopts techniques that are aimed to reduce the exposition time of the professionals and the absorption of excessive doses for patients. The ergonomic analysis of this process contributes in the prevention of occupational illnesses and to prevent risks of accidents during the routines, providing welfare and security to the involved users and conferring to the process an adequate working standard. In this context it is perceived relevance of studies that deal with the analysis of factors that point with respect to the solution of problems and for establishing proposals that minimize risks in the exercise of the activities. Through a methodology that considers the application of the concepts of Ergonomics, it is searched the improvement of the effectiveness or the quality and reduction of the difficulties lived for the workers. The work prescribed, established through norms and procedures codified will be faced with the work effectively carried through, the real work, shaped to break the correct appreciation, with focus in the activities. This work has as objective to argue an ergonomic analysis of samples preparation process of radioisotopes in the Setor de Radiofarmacia do Hospital Universitario Clementino Fraga Filho da Universidade Federal do Rio de Janeiro (UFRJ). (author)

  6. Comparison between XRF and IBA techniques in analysis of fine aerosols collected in Rijeka, Croatia

    Energy Technology Data Exchange (ETDEWEB)

    Ivošević, Tatjana [Faculty of Engineering, University of Rijeka, Vukovarska 58, HR-51000 Rijeka (Croatia); Mandić, Luka, E-mail: lukam@phy.uniri.hr [Department of Physics, University of Rijeka, Radmile Matejčić 2, HR-51000 Rijeka (Croatia); Orlić, Ivica [Department of Physics, University of Rijeka, Radmile Matejčić 2, HR-51000 Rijeka (Croatia); Stelcer, Eduard; Cohen, David D. [Institute for Environmental Research, Australian Nuclear Science and Technology Organisation, Kirrawee DC, NSW 2232 (Australia)

    2014-10-15

    The new system for energy dispersive X-ray fluorescence (EDXRF) analysis has been installed at the Laboratory for Elemental Micro-Analysis (LEMA) at the University of Rijeka. Currently the key application of this new XRF system is in the field of environmental science, i.e. in the analysis of fine airborne particles. In this work, results of initial multi-elemental analysis of PM{sub 2.5} fraction is reported for the first time in the region of Rijeka, Croatia. Sampling was performed at the Rijeka City center, during a continuous 9-day period in February/March 2012. All samples were collected on stretched Teflon filters in 12 h periods. To check the reliability of the new XRF system, results of XRF analysis are compared with the results obtained by the well-established Ion Beam Analysis (IBA) laboratory at Australian Nuclear Science and Technology Organisation (ANSTO). The concentrations of H, Na, Al, Si, P, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Br and Pb were determined. In addition, black carbon was determined by Laser Integrating Plate Method (LIPM). Very good agreement between XRF and IBA techniques is obtained for all elements detected by both techniques. Elemental concentrations were correlated with the traffic volume and wind speed and direction. The summary of our findings is presented and discussed in this paper.

  7. Multimodal optical analysis discriminates freshly extracted human sample of gliomas, metastases and meningiomas from their appropriate controls

    Science.gov (United States)

    Zanello, Marc; Poulon, Fanny; Pallud, Johan; Varlet, Pascale; Hamzeh, H.; Abi Lahoud, Georges; Andreiuolo, Felipe; Ibrahim, Ali; Pages, Mélanie; Chretien, Fabrice; di Rocco, Federico; Dezamis, Edouard; Nataf, François; Turak, Baris; Devaux, Bertrand; Abi Haidar, Darine

    2017-02-01

    Delineating tumor margins as accurately as possible is of primordial importance in surgical oncology: extent of resection is associated with survival but respect of healthy surrounding tissue is necessary for preserved quality of life. The real-time analysis of the endogeneous fluorescence signal of brain tissues is a promising tool for defining margins of brain tumors. The present study aims to demonstrate the feasibility of multimodal optical analysis to discriminate fresh samples of gliomas, metastases and meningiomas from their appropriate controls. Tumor samples were studied on an optical fibered endoscope using spectral and fluorescence lifetime analysis and then on a multimodal set-up for acquiring spectral, one and two-photon fluorescence images, second harmonic generation signals and two-photon fluorescence lifetime datasets. The obtained data allowed us to differentiate healthy samples from tumor samples. These results confirmed the possible clinical relevance of this real-time multimodal optical analysis. This technique can be easily applied to neurosurgical procedures for a better delineation of surgical margins.

  8. Neutron activation analysis for antimetabolites. [in food samples

    Science.gov (United States)

    1973-01-01

    Determination of metal ion contaminants in food samples is studied. A weighed quantity of each sample was digested in a concentrated mixture of nitric, hydrochloric and perchloric acids to affect complete solution of the food products. The samples were diluted with water and the pH adjusted according to the specific analysis performed. The samples were analyzed by neutron activation analysis, polarography, and atomic absorption spectrophotometry. The solid food samples were also analyzed by neutron activation analysis for increased sensitivity and lower levels of detectability. The results are presented in tabular form.

  9. High Throughput Sample Preparation and Analysis for DNA Sequencing, PCR and Combinatorial Screening of Catalysis Based on Capillary Array Technique

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yonghua [Iowa State Univ., Ames, IA (United States)

    2000-01-01

    Sample preparation has been one of the major bottlenecks for many high throughput analyses. The purpose of this research was to develop new sample preparation and integration approach for DNA sequencing, PCR based DNA analysis and combinatorial screening of homogeneous catalysis based on multiplexed capillary electrophoresis with laser induced fluorescence or imaging UV absorption detection. The author first introduced a method to integrate the front-end tasks to DNA capillary-array sequencers. protocols for directly sequencing the plasmids from a single bacterial colony in fused-silica capillaries were developed. After the colony was picked, lysis was accomplished in situ in the plastic sample tube using either a thermocycler or heating block. Upon heating, the plasmids were released while chromsomal DNA and membrane proteins were denatured and precipitated to the bottom of the tube. After adding enzyme and Sanger reagents, the resulting solution was aspirated into the reaction capillaries by a syringe pump, and cycle sequencing was initiated. No deleterious effect upon the reaction efficiency, the on-line purification system, or the capillary electrophoresis separation was observed, even though the crude lysate was used as the template. Multiplexed on-line DNA sequencing data from 8 parallel channels allowed base calling up to 620 bp with an accuracy of 98%. The entire system can be automatically regenerated for repeated operation. For PCR based DNA analysis, they demonstrated that capillary electrophoresis with UV detection can be used for DNA analysis starting from clinical sample without purification. After PCR reaction using cheek cell, blood or HIV-1 gag DNA, the reaction mixtures was injected into the capillary either on-line or off-line by base stacking. The protocol was also applied to capillary array electrophoresis. The use of cheaper detection, and the elimination of purification of DNA sample before or after PCR reaction, will make this approach an

  10. Urine storage under refrigeration preserves the sample in chemical, cellularity and bacteriuria analysis of ACS

    OpenAIRE

    Karen Cristina Barcellos Ribeiro; Bruno Rotondo Levenhagem Serabion; Eduardo Lima Nolasco; Chislene Pereira Vanelli; Harleson Lopes de Mesquita; José Otávio do Amaral Corrêa

    2013-01-01

    INTRODUCTION: The analysis of urine abnormal constituents and sediment (ACS) comprises tests of great diagnostic and prognostic value in clinical practice. When the analysis of ACS cannot be performed within two hours after collection, the sample must be preserved in order to avoid pre-analytical interferences. Refrigeration is the most applied technique due to its cost effectiveness. Moreover, it presents fewer inconveniences when compared to chemical preservation. However, changes in ACS ma...

  11. Texture investigation in aluminium and iron - silicon samples by neutron diffraction technique

    International Nuclear Information System (INIS)

    Pugliese, R.; Yamasaki, J.M.

    1988-09-01

    By means of the neutron diffraction technique the texture of 5% and 98% rolled-aluminium and of iron-silicon steel used in the core of electric transformers, have been determined. The measurements were performed by using a neutron diffractometer installed at the IEA-R1 Nuclear Research Reactor, in the Beam-Hole n 0 . 6. To avoid corrections such as neutron absorption and sample luminosity the geometric form of the samples were approximated to spheric or octagonal prism, and its dimensions do not exceed that of the neutron beam. The texture of the samples were analysed with the help of a computer programme that analyses the intensity of the diffracted neutron beam and plot the pole figures. (author) [pt

  12. High-throughput, 384-well, LC-MS/MS CYP inhibition assay using automation, cassette-analysis technique, and streamlined data analysis.

    Science.gov (United States)

    Halladay, Jason S; Delarosa, Erlie Marie; Tran, Daniel; Wang, Leslie; Wong, Susan; Khojasteh, S Cyrus

    2011-08-01

    Here we describe a high capacity and high-throughput, automated, 384-well CYP inhibition assay using well-known HLM-based MS probes. We provide consistently robust IC(50) values at the lead optimization stage of the drug discovery process. Our method uses the Agilent Technologies/Velocity11 BioCel 1200 system, timesaving techniques for sample analysis, and streamlined data processing steps. For each experiment, we generate IC(50) values for up to 344 compounds and positive controls for five major CYP isoforms (probe substrate): CYP1A2 (phenacetin), CYP2C9 ((S)-warfarin), CYP2C19 ((S)-mephenytoin), CYP2D6 (dextromethorphan), and CYP3A4/5 (testosterone and midazolam). Each compound is incubated separately at four concentrations with each CYP probe substrate under the optimized incubation condition. Each incubation is quenched with acetonitrile containing the deuterated internal standard of the respective metabolite for each probe substrate. To minimize the number of samples to be analyzed by LC-MS/MS and reduce the amount of valuable MS runtime, we utilize timesaving techniques of cassette analysis (pooling the incubation samples at the end of each CYP probe incubation into one) and column switching (reducing the amount of MS runtime). Here we also report on the comparison of IC(50) results for five major CYP isoforms using our method compared to values reported in the literature.

  13. More Poop, More Precision: Improving Epidemiologic Surveillance of Soil-Transmitted Helminths with Multiple Fecal Sampling using the Kato-Katz Technique.

    Science.gov (United States)

    Liu, Chengfang; Lu, Louise; Zhang, Linxiu; Bai, Yu; Medina, Alexis; Rozelle, Scott; Smith, Darvin Scott; Zhou, Changhai; Zang, Wei

    2017-09-01

    Soil-transmitted helminths, or parasitic intestinal worms, are among the most prevalent and geographically widespread parasitic infections in the world. Accurate diagnosis and quantification of helminth infection are critical for informing and assessing deworming interventions. The Kato-Katz thick smear technique, the most widely used laboratory method to quantitatively assess infection prevalence and infection intensity of helminths, has often been compared with other methods. Only a few small-scale studies, however, have considered ways to improve its diagnostic sensitivity. This study, conducted among 4,985 school-age children in an area of rural China with moderate prevalence of helminth infection, examines the effect on diagnostic sensitivity of the Kato-Katz technique when two fecal samples collected over consecutive days are examined and compared with a single sample. A secondary aim was to consider cost-effectiveness by calculating an estimate of the marginal costs of obtaining an additional fecal sample. Our findings show that analysis of an additional fecal sample led to increases of 23%, 26%, and 100% for Ascaris lumbricoides, Trichuris trichiura , and hookworm prevalence, respectively. The cost of collecting a second fecal sample for our study population was approximately USD4.60 per fecal sample. Overall, the findings suggest that investing 31% more capital in fecal sample collection prevents an underestimation of prevalence by about 21%, and hence improves the diagnostic sensitivity of the Kato-Katz method. Especially in areas with light-intensity infections of soil-transmitted helminths and limited public health resources, more accurate epidemiological surveillance using multiple fecal samples will critically inform decisions regarding infection control and prevention.

  14. Failure analysis of burst tested fuel tube samples

    International Nuclear Information System (INIS)

    Padmaprabu, C.; Ramana Rao, S.V.; Srivatsava, R.K.

    2005-01-01

    The Total Circumferential Elongation (TCE) is an important parameter for evaluation of ductility of the Zircaloy-4 fuel tubes for the PHWR reactors. The TCE values of the fuel tubes were obtained using the burst testing technique. In some lots there is a variation in the values of the TCE. To investigate the reasons for such a large variation in the TCE, samples were selected at appropriate intervals and sectioned at the fractured portion. The surface morphology of the fractured surfaces was examined under Scanning Electron Microscope (SEM) equipped with Energy Dispersive Spectrometer (EDS). The morphologies show segregation of elements at specific locations. Energy dispersive spectra was obtained from those segregated particles. According to the magnitude of TCE value the samples were classified into low, intermediate and high ductility. Low ductility samples were found to contain large amount of segregations along the thickness direction of the tube. This forms a brittle region and a path for the easy crack growth along thickness direction. In the case of intermediate samples the segregation occurred in fewer locations compared to low ductile samples and also confined to the circumferential direction of the outside surface of the tube. Due to this, probability of crack formation at the surface of the tube could be high. But crack growth would be slower in the ductile matrix along the thickness direction resulting in the enhancement of TCE value compared to the low ductile sample. In the high ductile samples, the segregations were very scarce and found to be isolated and embedded in the ductile matrix. The mode of failure in these types of samples was found to be purely ductile. Cracks were found to originate solely from the micro voids in the material. As the probability of crack formation and its propagation is low, very high TCE values were observed in these samples. Microstructural observations of fractured surfaces and EDAX analysis was able to identify the

  15. Determination of organic fluorine in aqueous samples with neutron activation analysis in comparison with the DIN method

    Energy Technology Data Exchange (ETDEWEB)

    Rollinger, D. [Institut fuer Kernchemie, Universitaet Mainz, Fritz-Strassmann-Weg 2, D-55099 Mainz (Germany); Kratz, K.L. [Institut fuer Kernchemie, Universitaet Mainz, Fritz-Strassmann-Weg 2, D-55099 Mainz (Germany)

    1996-04-01

    Neutron activation analysis (NAA) has been used as detection technique for adsorbable organic fluorine in aqueous samples. The results have been compared with the standardized DIN method which uses a fluoride-ion-selective electrode (ISE). (orig.). With 3 tabs.

  16. Report of the advisory group meeting on elemental analysis of extremely small samples

    International Nuclear Information System (INIS)

    2002-01-01

    This publication contains summary of discussions held at the meeting with brief description and comparative characteristics of most common nuclear analytical techniques used for analysis of very small samples as well as the conclusions of the meeting. Some aspect of reference materials and quality control are also discussed. The publication also contains individual contributions made by the participants, each of these papers haven provided with an abstract and indexed separately

  17. Five decades of promotion techniques in cigarette advertising: a longitudinal content analysis.

    Science.gov (United States)

    Paek, Hye-Jin; Reid, Leonard N; Jeong, Hyun Ju; Choi, Hojoon; Krugman, Dean

    2012-01-01

    This study examines frequencies and types of promotion techniques featured in five decades of cigarette advertising relative to five major smoking eras. Analysis of 1,133 cigarette advertisements collected through multistage sampling of 1954 through 2003 issues of three youth-oriented magazines found that 7.6% of the analyzed ads featured at least one promotion technique. Across smoking eras the proportion of promotion in the ads steadily increased from 1.6% in the "pre-broadcast ban era" to 10.9% in the "the pre-Master Settlement Agreement (MSA) era" and 9% in "post-MSA era." The increased use of sponsorships/events in cigarette ads for youth-oriented brands warrants more attention from tobacco control experts and government regulators.

  18. High priority tank sampling and analysis report

    International Nuclear Information System (INIS)

    Brown, T.M.

    1998-01-01

    In July 1993, the Defense Nuclear Facilities Board issued Recommendation 93-5 (Conway 1993) which noted that there was insufficient tank waste technical information and the pace to obtain it was too slow to ensure that Hanford Site wastes could be safely stored, that associated operations could be conducted safely, and that future disposal data requirements could be met. In response, the US Department of Energy, in May 1996, issued Revision 1 of the Recommendation 93-5 Implementation Plan (DOE-RL 1996). The Implementation Plan presented a modified approach to achieve the original plan's objectives, concentrating on actions necessary to ensure that wastes can be safely stored, that operations can be safely conducted, and that timely characterization information for the tank waste Disposal Program could be obtained. The Implementation Plan proposed 28 High Priority tanks for near term core sampling and analysis, which along with sampling and analysis of other non-High Priority tanks, could provide the scientific and technical data to confirm assumptions, calibrate models, and.measure safety related phenomenology of the waste. When the analysis results of the High Priority and other-tank sampling were reviewed, it was expected that a series of 12 questions, 9 related to safety issues and 3 related to planning for the disposal process, should be answered allowing key decisions to be made. This report discusses the execution of the Implementation Plan and the results achieved in addressing the questions. Through sampling and analysis, all nine safety related questions have been answered and extensive data for the three disposal planning related questions have been collected, allowing for key decision making. Many more tanks than the original 28 High Priority tanks identified in the Implementation Plan were sampled and analyzed. Twenty-one High Priority tanks and 85 other tanks were core sampled and used to address the questions. Thirty-eight additional tanks were auger

  19. Refinement of NMR structures using implicit solvent and advanced sampling techniques.

    Science.gov (United States)

    Chen, Jianhan; Im, Wonpil; Brooks, Charles L

    2004-12-15

    NMR biomolecular structure calculations exploit simulated annealing methods for conformational sampling and require a relatively high level of redundancy in the experimental restraints to determine quality three-dimensional structures. Recent advances in generalized Born (GB) implicit solvent models should make it possible to combine information from both experimental measurements and accurate empirical force fields to improve the quality of NMR-derived structures. In this paper, we study the influence of implicit solvent on the refinement of protein NMR structures and identify an optimal protocol of utilizing these improved force fields. To do so, we carry out structure refinement experiments for model proteins with published NMR structures using full NMR restraints and subsets of them. We also investigate the application of advanced sampling techniques to NMR structure refinement. Similar to the observations of Xia et al. (J.Biomol. NMR 2002, 22, 317-331), we find that the impact of implicit solvent is rather small when there is a sufficient number of experimental restraints (such as in the final stage of NMR structure determination), whether implicit solvent is used throughout the calculation or only in the final refinement step. The application of advanced sampling techniques also seems to have minimal impact in this case. However, when the experimental data are limited, we demonstrate that refinement with implicit solvent can substantially improve the quality of the structures. In particular, when combined with an advanced sampling technique, the replica exchange (REX) method, near-native structures can be rapidly moved toward the native basin. The REX method provides both enhanced sampling and automatic selection of the most native-like (lowest energy) structures. An optimal protocol based on our studies first generates an ensemble of initial structures that maximally satisfy the available experimental data with conventional NMR software using a simplified

  20. Detection of Certain Spices Subjected to Gamma Irradiation By Using Thermal Analysis Technique

    International Nuclear Information System (INIS)

    Sayed, M.S.; Ali, H.G.M.; Abdeldaiem, M.H.

    2013-01-01

    The present investigation was carried out to apply a detection method of some irradiated spices using thermal analysis technique. Black pepper, cumin and ginger were irradiated using gamma irradiation at dose levels 5, 10 and 15 kGy and stored for 12 months at room temperature. Thermal analysis techniques TGA and DTA were studied for characterizing irradiated spices. Thermo gravimetric analysis (TGA) is a method where the measurement of mass as a function of heating is recorded. TGA was used to determine the moisture and ash contents and thermal stabilities. Non-significant changes of the weight loss percent due to the irradiation were occurred on the studied spices up to 10 kGy. The weight loss was decreased at the first step up to 100 degree C due to the release of water of hydration. Another sharp decreasing in weight loss percent at the second step 220-300 degree C may be due to volatilization of the sample. The final weight loss weight loss stage up to 500 degree C may be due to burn out the fixed carbon remaining in the sample. As the irradiation dose increased from control up to 15 kGy, the weight loss percent at the dehydration step was decreased. The kinetics of the spices decomposition were studied in order to ascertain the type of weight loss mechanism and calculate the activation energy (E a ). The differential thermal analysis (DTA) of the studied samples showed two main characteristic peaks; endothermic one due to the dehydration process and the second peak may be due to the partial volatilization of the aromatic compounds of the main constituent of the studied spices. It could be concluded that using gamma irradiation (up to 15.0 kGy) for black pepper, cumin and ginger are thermally stable to human consumption.