k-Means: Random Sampling Procedure

Indian Academy of Sciences (India)

First page Back Continue Last page Overview Graphics. k-Means: Random Sampling Procedure. Optimal 1-Mean is. Approximation of Centroid (Inaba et al). S = random sample of size O(1/ ); Centroid of S is a (1+ )-approx centroid of P with constant probability.

Minimization of the blank values in the neutron activation analysis of biological samples considering the whole procedure

International Nuclear Information System (INIS)

Lux, F.; Bereznai, T.; Haeberlin, T.H.

1986-01-01

In our determination of trace element contents of animal tissue by neutron activation analysis in the course of structure-activity relationship studies on platinum containing cancer drugs and wound healing we have tried to minimize the blank values that are caused by different sources of contamination during surgery, sampling and the activation analysis procedure. The following topics have been investigated: the abrasions from scalpels made of stainless steel, titanium or quartz; the type of surgery; the homogenisation of the samples before irradiation by use of a ball milll; the surface contaminations of the quartz ampoules that pass into the digestion solution of the irradiated samples. The appropriate measures taken in order to reduce the blank values are described. The results of analyses performed under these conditions indicate the effectiveness of the given measures, especially shown by the low values obtained for the chromium contents of the analysed muscle samples. (author)

A novel sample preparation procedure for effect-directed analysis of micro-contaminants of emerging concern in surface waters.

Science.gov (United States)

Osorio, Victoria; Schriks, Merijn; Vughs, Dennis; de Voogt, Pim; Kolkman, Annemieke

2018-08-15

A novel sample preparation procedure relying on Solid Phase Extraction (SPE) combining different sorbent materials on a sequential-based cartridge was optimized and validated for the enrichment of 117 widely diverse contaminants of emerging concern (CECs) from surface waters (SW) and further combined chemical and biological analysis on subsequent extracts. A liquid chromatography coupled to high resolution tandem mass spectrometry LC-(HR)MS/MS protocol was optimized and validated for the quantitative analysis of organic CECs in SW extracts. A battery of in vitro CALUX bioassays for the assessment of endocrine, metabolic and genotoxic interference and oxidative stress were performed on the same SW extracts. Satisfactory recoveries ([70-130]%) and precision ( 0.99) over three orders of magnitude. Instrumental limits of detection and method limits of quantification were of [1-96] pg injected and [0.1-58] ng/L, respectively; while corresponding intra-day and inter-day precision did not exceed 11% and 20%. The developed procedure was successfully applied for the combined chemical and toxicological assessment of SW intended for drinking water supply. Levels of compounds varied from < 10 ng/L to < 500 ng/L. Endocrine (i.e. estrogenic and anti-androgenic) and metabolic interference responses were observed. Given the demonstrated reliability of the validated sample preparation method, the authors propose its integration in an effect-directed analysis procedure for a proper evaluation of SW quality and hazard assessment of CECs. Copyright © 2018 Elsevier B.V. All rights reserved.

Delineating sampling procedures: Pedagogical significance of analysing sampling descriptions and their justifications in TESL experimental research reports

Directory of Open Access Journals (Sweden)

Jason Miin-Hwa Lim

2011-04-01

Full Text Available Teaching second language learners how to write research reports constitutes a crucial component in programmes on English for Specific Purposes (ESP in institutions of higher learning. One of the rhetorical segments in research reports that merit attention has to do with the descriptions and justifications of sampling procedures. This genre-based study looks into sampling delineations in the Method-related sections of research articles on the teaching of English as a second language (TESL written by expert writers and published in eight reputed international refereed journals. Using Swales’s (1990 & 2004 framework, I conducted a quantitative analysis of the rhetorical steps and a qualitative investigation into the language resources employed in delineating sampling procedures. This investigation has considerable relevance to ESP students and instructors as it has yielded pertinent findings on how samples can be appropriately described to meet the expectations of dissertation examiners, reviewers, and supervisors. The findings of this study have furnished insights into how supervisors and instructors can possibly teach novice writers ways of using specific linguistic mechanisms to lucidly describe and convincingly justify the sampling procedures in the Method sections of experimental research reports.

Summative Mass Analysis of Algal Biomass - Integration of Analytical Procedures: Laboratory Analytical Procedure (LAP)

Energy Technology Data Exchange (ETDEWEB)

Laurens, Lieve M. L.

2016-01-13

This procedure guides the integration of laboratory analytical procedures to measure algal biomass constituents in an unambiguous manner and ultimately achieve mass balance closure for algal biomass samples. Many of these methods build on years of research in algal biomass analysis.

Comparison of transition-matrix sampling procedures

DEFF Research Database (Denmark)

Yevick, D.; Reimer, M.; Tromborg, Bjarne

2009-01-01

We compare the accuracy of the multicanonical procedure with that of transition-matrix models of static and dynamic communication system properties incorporating different acceptance rules. We find that for appropriate ranges of the underlying numerical parameters, algorithmically simple yet high...... accurate procedures can be employed in place of the standard multicanonical sampling algorithm....

The MacDonald and savage titrimetric procedure for plutonium scaled-down to the milligram level: Automated procedure for routine analysis of safeguards samples containing 2 to 5 mg plutonium

International Nuclear Information System (INIS)

Ronesch, K.; Jammet, G.; Berger, J.; Doubek, N.; Bagliano, G.; Deron, S.

1992-08-01

A selective titrimetric procedure directly applicable to both input and product solutions from fast reactor fuel reprocessing was set up by MacDonald and Savage and scaled down to 3 mg of plutonium in sample aliquots at the request of the Safeguards Analytical Laboratory (SAL) of the International Atomic Energy Agency (IAEA), which needed to replace its silver (II) oxide titration procedure by a more selective electrochemical method. Although the procedure is very selective the following species still interfere: Vanadates (almost quantitatively), Neptunium (one electron exchange per mole); Nitrites, Fluorosilicates and Iodates present in mg amount yield slight biases. This paper describes the fully automatized procedure presently applied in SAL for the routine determination of 2 to 5 mg plutonium dissolved in nitric acid solution. The method allows the unattended analysis of 20 aliquots within a five hour period. The equipment including the reagent distribution system, the sample changer and the control units are introduced and the principle design of the software is shortly described. Safety requirements have been addressed and are also reviewed in the report. Results obtained on standard reference materials, international intercomparison samples and actual safeguards samples routinely analyzed with the proposed procedure are presented and compared with results achieved with the semiautomatic mode to demonstrate the performance. International requirements to reduce the amount of radioactive materials in waste will certainly lead to a further reduction of the amount of plutonium in one aliquot. Some future perspective to titrate 1 mg samples are presented in the discussion. 12 refs, 10 figs, 8 tabs

Minimization of the blank values in the neutron activation analysis of biological samples considering the whole procedure

International Nuclear Information System (INIS)

Lux, F.; Bereznai, T.; Trebert Haeberlin, S.

1987-01-01

During the determination of trace element contents of animal tissue by neutron activation analysis in the course of structure-activity relationship studies on platinum containing cancer drugs and wound healing the authors tried to minimize the blank values that are caused by different sources of contamination during surgery, sampling and the activation analysis procedure. The following topics were investigated: abrasions from scalpels made of stainless steel, titanium or quartz, the type of surgery, the surface contaminations of the quartz ampoules, etc. The measures to be taken to reduce tha blank values are described. (author) 19 refs.; 4 tables

IXM gas sampling procedure

International Nuclear Information System (INIS)

Pingel, L.A.

1995-01-01

Ion Exchange Modules (IXMs) are used at the 105-KE and -KW Fuel Storage Basins to control radionuclide concentrations in the water. A potential safety concern relates to production of hydrogen gas by radiolysis of the water trapped in the ion exchange media of spent IXMs. This document provides a procedure for sampling the gases in the head space of the IXM

NHEXAS PHASE I MARYLAND STUDY--STANDARD OPERATING PROCEDURE FOR COLLECTION, STORAGE, AND SHIPMENT OF URINE SAMPLES FOR METAL, PESTICIDE, AND CREATININE ANALYSIS (F10)

Science.gov (United States)

The purpose of this SOP is to describe the procedures for collection, storage, and shipment of urine samples for metal, pesticides, and creatinine analysis. Samples were collected on Days 2 and 8 of each Cycle. The Day 2 sample was analyzed for metals and creatinine. The Day 8...

Transuranium analysis methodologies for biological and environmental samples

International Nuclear Information System (INIS)

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

1978-01-01

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

Influence of Freezing and Storage Procedure on Human Urine Samples in NMR-Based Metabolomics

Directory of Open Access Journals (Sweden)

Burkhard Luy

2013-04-01

Full Text Available It is consensus in the metabolomics community that standardized protocols should be followed for sample handling, storage and analysis, as it is of utmost importance to maintain constant measurement conditions to identify subtle biological differences. The aim of this work, therefore, was to systematically investigate the influence of freezing procedures and storage temperatures and their effect on NMR spectra as a potentially disturbing aspect for NMR-based metabolomics studies. Urine samples were collected from two healthy volunteers, centrifuged and divided into aliquots. Urine aliquots were frozen either at −20 °C, on dry ice, at −80 °C or in liquid nitrogen and then stored at −20 °C, −80 °C or in liquid nitrogen vapor phase for 1–5 weeks before NMR analysis. Results show spectral changes depending on the freezing procedure, with samples frozen on dry ice showing the largest deviations. The effect was found to be based on pH differences, which were caused by variations in CO2 concentrations introduced by the freezing procedure. Thus, we recommend that urine samples should be frozen at −20 °C and transferred to lower storage temperatures within one week and that freezing procedures should be part of the publication protocol.

Influence of Freezing and Storage Procedure on Human Urine Samples in NMR-Based Metabolomics.

Science.gov (United States)

Rist, Manuela J; Muhle-Goll, Claudia; Görling, Benjamin; Bub, Achim; Heissler, Stefan; Watzl, Bernhard; Luy, Burkhard

2013-04-09

It is consensus in the metabolomics community that standardized protocols should be followed for sample handling, storage and analysis, as it is of utmost importance to maintain constant measurement conditions to identify subtle biological differences. The aim of this work, therefore, was to systematically investigate the influence of freezing procedures and storage temperatures and their effect on NMR spectra as a potentially disturbing aspect for NMR-based metabolomics studies. Urine samples were collected from two healthy volunteers, centrifuged and divided into aliquots. Urine aliquots were frozen either at -20 °C, on dry ice, at -80 °C or in liquid nitrogen and then stored at -20 °C, -80 °C or in liquid nitrogen vapor phase for 1-5 weeks before NMR analysis. Results show spectral changes depending on the freezing procedure, with samples frozen on dry ice showing the largest deviations. The effect was found to be based on pH differences, which were caused by variations in CO2 concentrations introduced by the freezing procedure. Thus, we recommend that urine samples should be frozen at -20 °C and transferred to lower storage temperatures within one week and that freezing procedures should be part of the publication protocol.

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

International Nuclear Information System (INIS)

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

2009-01-01

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

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

Analytical procedures for determining Pb and Sr isotopic compositions in water samples by ID-TIMS

Directory of Open Access Journals (Sweden)

Veridiana Martins

2008-01-01

Full Text Available Few articles deal with lead and strontium isotopic analysis of water samples. The aim of this study was to define the chemical procedures for Pb and Sr isotopic analyses of groundwater samples from an urban sedimentary aquifer. Thirty lead and fourteen strontium isotopic analyses were performed to test different analytical procedures. Pb and Sr isotopic ratios as well as Sr concentration did not vary using different chemical procedures. However, the Pb concentrations were very dependent on the different procedures. Therefore, the choice of the best analytical procedure was based on the Pb results, which indicated a higher reproducibility from samples that had been filtered and acidified before the evaporation, had their residues totally dissolved, and were purified by ion chromatography using the Biorad® column. Our results showed no changes in Pb ratios with the storage time.

Rapid Microwave Digestion Procedures for the Elemental Analysis of Alloy and Slag Samples of Smelted Ocean Bed Polymetallic Nodules

Directory of Open Access Journals (Sweden)

Kumari Smita

2013-01-01

Full Text Available The use of microwave digester for digestion of alloy and slag samples of smelted ocean bed polymetallic nodules has permitted the complete digestion of samples, thereby replacing the tedious classical methods of digestion of samples. The digestion procedure includes two acid-closed digestions of samples in a microwave oven. Owing to the hazardous nature of perchloric acid, it was not used in developed digestion procedure. Digested sample solutions were analyzed for concentrations of various radicals and the effectiveness of the developed digestion methodology was tested using certified reference materials. It was found that the developed method is giving results comparable with that obtained from conventionally digested samples. In this digestion procedure, time required for digestion of samples was reduced to about 1 hour only from 8-9 hours of conventional digestion.

New procedure of selected biogenic amines determination in wine samples by HPLC

Energy Technology Data Exchange (ETDEWEB)

Piasta, Anna M.; Jastrzębska, Aneta, E-mail: aj@chem.uni.torun.pl; Krzemiński, Marek P.; Muzioł, Tadeusz M.; Szłyk, Edward

2014-06-27

Highlights: • We proposed new procedure for derivatization of biogenic amines. • The NMR and XRD analysis confirmed the purity and uniqueness of derivatives. • Concentration of biogenic amines in wine samples were analyzed by RP-HPLC. • Sample contamination and derivatization reactions interferences were minimized. - Abstract: A new procedure for determination of biogenic amines (BA): histamine, phenethylamine, tyramine and tryptamine, based on the derivatization reaction with 2-chloro-1,3-dinitro-5-(trifluoromethyl)-benzene (CNBF), is proposed. The amines derivatives with CNBF were isolated and characterized by X-ray crystallography and {sup 1}H, {sup 13}C, {sup 19}F NMR spectroscopy in solution. The novelty of the procedure is based on the pure and well-characterized products of the amines derivatization reaction. The method was applied for the simultaneous analysis of the above mentioned biogenic amines in wine samples by the reversed phase-high performance liquid chromatography. The procedure revealed correlation coefficients (R{sup 2}) between 0.9997 and 0.9999, and linear range: 0.10–9.00 mg L{sup −1} (histamine); 0.10–9.36 mg L{sup -1} (tyramine); 0.09–8.64 mg L{sup −1} (tryptamine) and 0.10–8.64 mg L{sup −1} (phenethylamine), whereas accuracy was 97%–102% (recovery test). Detection limit of biogenic amines in wine samples was 0.02–0.03 mg L{sup −1}, whereas quantification limit ranged 0.05–0.10 mg L{sup −1}. The variation coefficients for the analyzed amines ranged between 0.49% and 3.92%. Obtained BA derivatives enhanced separation the analytes on chromatograms due to the inhibition of hydrolysis reaction and the reduction of by-products formation.

Procedure for the analysis of americium in complex matrices

International Nuclear Information System (INIS)

Knab, D.

1978-02-01

A radioanalytical procedure for the analysis of americium in complex matrices has been developed. Clean separations of americium can be obtained from up to 100 g of sample ash, regardless of the starting material. The ability to analyze large masses of material provides the increased sensitivity necessary to detect americium in many environmental samples. The procedure adequately decontaminates from rare earth elements and natural radioactive nuclides that interfere with the alpha spectrometric measurements

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

Direct analysis of 210Pb in sediment samples: Self-absorption corrections

International Nuclear Information System (INIS)

Cutshall, N.H.; Larsen, I.L.; Olsen, C.R.

1983-01-01

A procedure for the direct #betta#-ray instrumental analysis of 210 Pb in sediment samples is presented. The problem of dependence of self-absorption on sample composition is solved by making a direct transmission measurement on each sample. The procedure has been verified by intercalibrations and other tests. (orig.)

Sample processing procedures and radiocarbon dating

International Nuclear Information System (INIS)

Svetlik, Ivo; Tomaskova, Lenka; Dreslerova, Dagmar

2010-01-01

The article outlines radiocarbon dating routines and highlights the potential and limitations of this method. The author's institutions have been jointly running a conventional radiocarbon dating laboratory using the international CRL code. A procedure based on the synthesis of benzene is used. Small samples are sent abroad for dating because no AMS instrumentation is available in the Czech Republic so far. Our laboratory plans to introduce routines for the processing of milligram samples and preparation of graphitized targets for AMS

The utilisation of thermal analysis to optimise radiocarbon dating procedures

International Nuclear Information System (INIS)

Brandova, D.; Keller, W.A.; Maciejewski, M.

1999-01-01

Thermal analysis combined with mass spectrometry was applied to radiocarbon dating procedures (age determination of carbon-containing samples). Experiments carried out under an oxygen atmosphere were used to determine carbon content and combustion range of soil and wood samples. Composition of the shell sample and its decomposition were investigated. The quantification of CO 2 formed by the oxidation of carbon was done by the application of pulse thermal analysis. Experiments carried out under an inert atmosphere determined the combustion range of coal with CuO as an oxygen source. To eliminate a possible source of contamination in the radiocarbon dating procedures the adsorption of CO 2 by CuO was investigated. (author)

GET electronics samples data analysis

International Nuclear Information System (INIS)

Giovinazzo, J.; Goigoux, T.; Anvar, S.; Baron, P.; Blank, B.; Delagnes, E.; Grinyer, G.F.; Pancin, J.; Pedroza, J.L.; Pibernat, J.; Pollacco, E.; Rebii, A.

2016-01-01

The General Electronics for TPCs (GET) has been developed to equip a generation of time projection chamber detectors for nuclear physics, and may also be used for a wider range of detector types. The goal of this paper is to propose first analysis procedures to be applied on raw data samples from the GET system, in order to correct for systematic effects observed on test measurements. We also present a method to estimate the response function of the GET system channels. The response function is required in analysis where the input signal needs to be reconstructed, in terms of time distribution, from the registered output samples.

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

Procedures for cryogenic X-ray ptychographic imaging of biological samples.

Science.gov (United States)

Yusuf, M; Zhang, F; Chen, B; Bhartiya, A; Cunnea, K; Wagner, U; Cacho-Nerin, F; Schwenke, J; Robinson, I K

2017-03-01

Biological sample-preparation procedures have been developed for imaging human chromosomes under cryogenic conditions. A new experimental setup, developed for imaging frozen samples using beamline I13 at Diamond Light Source, is described. This manuscript describes the equipment and experimental procedures as well as the authors' first ptychographic reconstructions using X-rays.

Synthetic Multiple-Imputation Procedure for Multistage Complex Samples

Directory of Open Access Journals (Sweden)

Zhou Hanzhi

2016-03-01

Full Text Available Multiple imputation (MI is commonly used when item-level missing data are present. However, MI requires that survey design information be built into the imputation models. For multistage stratified clustered designs, this requires dummy variables to represent strata as well as primary sampling units (PSUs nested within each stratum in the imputation model. Such a modeling strategy is not only operationally burdensome but also inferentially inefficient when there are many strata in the sample design. Complexity only increases when sampling weights need to be modeled. This article develops a generalpurpose analytic strategy for population inference from complex sample designs with item-level missingness. In a simulation study, the proposed procedures demonstrate efficient estimation and good coverage properties. We also consider an application to accommodate missing body mass index (BMI data in the analysis of BMI percentiles using National Health and Nutrition Examination Survey (NHANES III data. We argue that the proposed methods offer an easy-to-implement solution to problems that are not well-handled by current MI techniques. Note that, while the proposed method borrows from the MI framework to develop its inferential methods, it is not designed as an alternative strategy to release multiply imputed datasets for complex sample design data, but rather as an analytic strategy in and of itself.

Procedures for cryogenic X-ray ptychographic imaging of biological samples

Directory of Open Access Journals (Sweden)

M. Yusuf

2017-03-01

Full Text Available Biological sample-preparation procedures have been developed for imaging human chromosomes under cryogenic conditions. A new experimental setup, developed for imaging frozen samples using beamline I13 at Diamond Light Source, is described. This manuscript describes the equipment and experimental procedures as well as the authors' first ptychographic reconstructions using X-rays.

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

Role of microextraction sampling procedures in forensic toxicology.

Science.gov (United States)

Barroso, Mário; Moreno, Ivo; da Fonseca, Beatriz; Queiroz, João António; Gallardo, Eugenia

2012-07-01

The last two decades have provided analysts with more sensitive technology, enabling scientists from all analytical fields to see what they were not able to see just a few years ago. This increased sensitivity has allowed drug detection at very low concentrations and testing in unconventional samples (e.g., hair, oral fluid and sweat), where despite having low analyte concentrations has also led to a reduction in sample size. Along with this reduction, and as a result of the use of excessive amounts of potentially toxic organic solvents (with the subsequent environmental pollution and costs associated with their proper disposal), there has been a growing tendency to use miniaturized sampling techniques. Those sampling procedures allow reducing organic solvent consumption to a minimum and at the same time provide a rapid, simple and cost-effective approach. In addition, it is possible to get at least some degree of automation when using these techniques, which will enhance sample throughput. Those miniaturized sample preparation techniques may be roughly categorized in solid-phase and liquid-phase microextraction, depending on the nature of the analyte. This paper reviews recently published literature on the use of microextraction sampling procedures, with a special focus on the field of forensic toxicology.

Acceptance test procedure for core sample trucks

International Nuclear Information System (INIS)

Smalley, J.L.

1995-01-01

The purpose of this Acceptance Test Procedure is to provide instruction and documentation for acceptance testing of the rotary mode core sample trucks, HO-68K-4600 and HO-68K-4647. The rotary mode core sample trucks were based upon the design of the second core sample truck (HO-68K-4345) which was constructed to implement rotary mode sampling of the waste tanks at Hanford. Acceptance testing of the rotary mode core sample trucks will verify that the design requirements have been met. All testing will be non-radioactive and stand-in materials shall be used to simulate waste tank conditions. Compressed air will be substituted for nitrogen during the majority of testing, with nitrogen being used only for flow characterization

Effects of blood sample handling procedures on measurable inflammatory markers in plasma, serum and dried blood spot samples

DEFF Research Database (Denmark)

Skogstrand, K.; Thorsen, P.; Vogel, I.

2008-01-01

of whole blood samples at low temperatures and rapid isolation of plasma and serum. Effects of different handling procedures for all markers studied are given. DBSS proved to be a robust and convenient way to handle samples for immunoassay analysis of inflammatory markers in whole blood Udgivelsesdato......The interests in monitoring inflammation by immunoassay determination of blood inflammatory markers call for information on the stability of these markers in relation to the handling of blood samples. The increasing use of stored biobank samples for such ventures that may have been collected...... and stored for other purposes, justifies the study hereof. Blood samples were stored for 0, 4, 24, and 48 h at 4 degrees C, room temperature (RT), and at 35 degrees C, respectively, before they were separated into serum or plasma and frozen. Dried blood spot samples (DBSS) were stored for 0, 1, 2, 3, 7...

Secondary School Students' Reasoning about Conditional Probability, Samples, and Sampling Procedures

Science.gov (United States)

Prodromou, Theodosia

2016-01-01

In the Australian mathematics curriculum, Year 12 students (aged 16-17) are asked to solve conditional probability problems that involve the representation of the problem situation with two-way tables or three-dimensional diagrams and consider sampling procedures that result in different correct answers. In a small exploratory study, we…

Influence of Freezing and Storage Procedure on Human Urine Samples in NMR-Based Metabolomics

OpenAIRE

Rist, Manuela; Muhle-Goll, Claudia; Görling, Benjamin; Bub, Achim; Heissler, Stefan; Watzl, Bernhard; Luy, Burkhard

2013-01-01

It is consensus in the metabolomics community that standardized protocols should be followed for sample handling, storage and analysis, as it is of utmost importance to maintain constant measurement conditions to identify subtle biological differences. The aim of this work, therefore, was to systematically investigate the influence of freezing procedures and storage temperatures and their effect on NMR spectra as a potentially disturbing aspect for NMR-based metabolomics studies. Urine sample...

Procedures for multielement analysis using high-flux fast-neutron activation

International Nuclear Information System (INIS)

Williams, R.E.; Hopke, P.K.; Meyer, R.A.

1981-06-01

Improvements have been made in the rabbit system used for multi-element fast-neutron activation analysis at the Lawrence Livermore National Laboratory Rotating Target Neutron Source, RTNS-I. Procedures have been developed for the analysis of 20 to 25 elements in samples with an inorganic matrix and 10 to 15 elements in biological samples, without the need for prohibitively expensive, long irradiations. Results are presented for the analysis of fly ash, orchard leaves, and bovine liver

Inverse sampled Bernoulli (ISB) procedure for estimating a population proportion, with nuclear material applications

International Nuclear Information System (INIS)

Wright, T.

1982-01-01

A new sampling procedure is introduced for estimating a population proportion. The procedure combines the ideas of inverse binomial sampling and Bernoulli sampling. An unbiased estimator is given with its variance. The procedure can be viewed as a generalization of inverse binomial sampling

14CO2 analysis of soil gas: Evaluation of sample size limits and sampling devices

Science.gov (United States)

Wotte, Anja; Wischhöfer, Philipp; Wacker, Lukas; Rethemeyer, Janet

2017-12-01

Radiocarbon (14C) analysis of CO2 respired from soils or sediments is a valuable tool to identify different carbon sources. The collection and processing of the CO2, however, is challenging and prone to contamination. We thus continuously improve our handling procedures and present a refined method for the collection of even small amounts of CO2 in molecular sieve cartridges (MSCs) for accelerator mass spectrometry 14C analysis. Using a modified vacuum rig and an improved desorption procedure, we were able to increase the CO2 recovery from the MSC (95%) as well as the sample throughput compared to our previous study. By processing series of different sample size, we show that our MSCs can be used for CO2 samples of as small as 50 μg C. The contamination by exogenous carbon determined in these laboratory tests, was less than 2.0 μg C from fossil and less than 3.0 μg C from modern sources. Additionally, we tested two sampling devices for the collection of CO2 samples released from soils or sediments, including a respiration chamber and a depth sampler, which are connected to the MSC. We obtained a very promising, low process blank for the entire CO2 sampling and purification procedure of ∼0.004 F14C (equal to 44,000 yrs BP) and ∼0.003 F14C (equal to 47,000 yrs BP). In contrast to previous studies, we observed no isotopic fractionation towards lighter δ13C values during the passive sampling with the depth samplers.

Procedure for determination of alpha emitters in urine and dregs samples

International Nuclear Information System (INIS)

Serdeiro, Nelida H.

2005-01-01

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

Partial report and other sampling procedures overestimate the duration of iconic memory.

Science.gov (United States)

Appelman, I B

1980-03-01

In three experiments, subjects estimated the duration of a brief visual image (iconic memory) either directly by adjusting onset of a click to offset of the visual image, or indirectly with a Sperling partial report (sampling) procedure. The results indicated that partial report and other sampling procedures may reflect other brief phenomena along with iconic memory. First, the partial report procedure yields a greater estimate of the duration of iconic memory than the more direct click method. Second, the partial report estimate of the duration of iconic memory is affected if the subject is required to simultaneously retain a list of distractor items (memory load), while the click method estimate of the duration of iconic memory is not affected by a memory load. Finally, another sampling procedure based on visual cuing yields different estimates of the duration of iconic memory depending on how many items are cued. It was concluded that partial report and other sampling procedures overestimate the duration of iconic memory.

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

Recommended operating procedure number 56: Collection of gaseous grab samples from combustion sources for nitrous oxide measurement. Final report, Jan-Dec 91

International Nuclear Information System (INIS)

Ryan, J.V.; Karns, S.A.

1992-07-01

The document is a recommended operating procedure (ROP), prepared for use in research activities conducted by EPA's Air and Energy Engineering Research Laboratory (AEERL). The procedure applies to the collection of gaseous grab samples from fossil fuel combustion sources for subsequent analysis of nitrous oxide. The procedure details only the grab sampling methodology and associated equipment

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)

Cluster analysis of commercial samples of Bauhinia spp. using HPLC-UV/PDA and MCR-ALS/PCA without peak alignment procedure.

Science.gov (United States)

Ardila, Jorge Armando; Funari, Cristiano Soleo; Andrade, André Marques; Cavalheiro, Alberto José; Carneiro, Renato Lajarim

2015-01-01

Bauhinia forficata Link. is recognised by the Brazilian Health Ministry as a treatment of hypoglycemia and diabetes. Analytical methods are useful to assess the plant identity due the similarities found in plants from Bauhinia spp. HPLC-UV/PDA in combination with chemometric tools is an alternative widely used and suitable for authentication of plant material, however, the shifts of retention times for similar compounds in different samples is a problem. To perform comparisons between the authentic medicinal plant (Bauhinia forficata Link.) and samples commercially available in drugstores claiming to be "Bauhinia spp. to treat diabetes" and to evaluate the performance of multivariate curve resolution - alternating least squares (MCR-ALS) associated to principal component analysis (PCA) when compared to pure PCA. HPLC-UV/PDA data obtained from extracts of leaves were evaluated employing a combination of MCR-ALS and PCA, which allowed the use of the full chromatographic and spectrometric information without the need of peak alignment procedures. The use of MCR-ALS/PCA showed better results than the conventional PCA using only one wavelength. Only two of nine commercial samples presented characteristics similar to the authentic Bauhinia forficata spp., considering the full HPLC-UV/PDA data. The combination of MCR-ALS and PCA is very useful when applied to a group of samples where a general alignment procedure could not be applied due to the different chromatographic profiles. This work also demonstrates the need of more strict control from the health authorities regarding herbal products available on the market. Copyright © 2015 John Wiley & Sons, Ltd.

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

Bio-Oil Analysis Laboratory Procedures | Bioenergy | NREL

Science.gov (United States)

Bio-Oil Analysis Laboratory Procedures Bio-Oil Analysis Laboratory Procedures NREL develops laboratory analytical procedures (LAPs) for the analysis of raw and upgraded pyrolysis bio-oils. These standard procedures have been validated and allow for reliable bio-oil analysis. Procedures Determination

Transuranic waste characterization sampling and analysis methods manual. Revision 1

International Nuclear Information System (INIS)

Suermann, J.F.

1996-04-01

This Methods Manual provides a unified source of information on the sampling and analytical techniques that enable Department of Energy (DOE) facilities to comply with the requirements established in the current revision of the Transuranic Waste Characterization Quality Assurance Program Plan (QAPP) for the Waste Isolation Pilot Plant (WIPP) Transuranic (TRU) Waste Characterization Program (the Program) and the WIPP Waste Analysis Plan. This Methods Manual includes all of the testing, sampling, and analytical methodologies accepted by DOE for use in implementing the Program requirements specified in the QAPP and the WIPP Waste Analysis Plan. The procedures in this Methods Manual are comprehensive and detailed and are designed to provide the necessary guidance for the preparation of site-specific procedures. With some analytical methods, such as Gas Chromatography/Mass Spectrometry, the Methods Manual procedures may be used directly. With other methods, such as nondestructive characterization, the Methods Manual provides guidance rather than a step-by-step procedure. Sites must meet all of the specified quality control requirements of the applicable procedure. Each DOE site must document the details of the procedures it will use and demonstrate the efficacy of such procedures to the Manager, National TRU Program Waste Characterization, during Waste Characterization and Certification audits

Sampling and sample handling procedures for priority pollutants in surface coal mining wastewaters. [Detailed list to be analyzed for

Energy Technology Data Exchange (ETDEWEB)

Hayden, R. S.; Johnson, D. O.; Henricks, J. D.

1979-03-01

The report describes the procedures used by Argonne National Laboratory to sample surface coal mine effluents in order to obtain field and laboratory data on 110 organic compounds or classes of compounds and 14 metals and minerals that are known as priority pollutants, plus 5-day biochemical oxygen demand (BOD/sub 5/), total organic carbon (TOC), chemical oxygen demand (COD), total dissolved solids (TDS), and total suspended solids (TSS). Included are directions for preparation of sampling containers and equipment, methods of sampling and sample preservation, and field and laboratory protocols, including chain-of-custody procedures. Actual analytical procedures are not described, but their sources are referenced.

Guideline for Sampling and Analysis of Tar and Particles in Biomass Producer Gases. Version 3.3

Energy Technology Data Exchange (ETDEWEB)

Neeft, J.P.A.; Knoef, H.A.M.; Zielke, U.; Sjoestroem, K.; Hasler, P.; Simell, P.A.; Dorrington, M.A.; Thomas, L.; Abatzoglou, N.; Deutch, S.; Greil, C.; Buffinga, G.J.; Brage, C.; Suomalainen, M.

2002-07-01

This Guideline provides a set of procedures for the measurement of organic contaminants and particles in producer gases from biomass gasifiers. The procedures are designed to cover different gasifier types (updraft or downdraft fixed bed or fluidised bed gasifiers), operating conditions (0 - 900C and 0.6-60 bars) and concentration ranges (1 mg/m{sub n}{sup 3} to 300 g/m{sub n}{sup 3}). The Guideline describes a modular sampling train, and a set of procedures, which include: planning and preparation of the sampling, sampling and post-sampling, analysis, calculations, error analysis and reporting. The modular sampling train consists of 4 modules. Module 1 is a preconditioning module for isokinetic sampling and gas cooling. Module 2 is a particle collection module including a heated filter. Module 3 is a tar collection module with a gas quench (optionally by circulating a liquid), impinger bottles and a backup adsorber. Module 4 is a volume-sampling module consisting of a pump, a rotameter, a gas flow meter and pressure and temperature indicators. The equipment and materials that are required for procuring this modular sampling train are given in the Guideline. The sampling procedures consist of a description for isokinetic sampling, a leakage test prior to sampling, the actual sampling and its duration, how the equipment is cleaned after the sampling, and how the samples are prepared and stored. Analysis of the samples is performed via three procedures. Prior to these procedures, the sample is prepared by Soxhlet extraction of the tars on the particle filter and by collection of all tars in one bulk solution. The first procedure describes the weighing of the particle filter to obtain the concentration of particles in the biomass producer gas. The bulk tar solution is used for two purposes: for determination of gravimetric tar and for analysis of individual compounds. The second procedure describes how to determine the gravimetric tar mass from the bulk solution. The

Direct methylation procedure for converting fatty amides to fatty acid methyl esters in feed and digesta samples.

Science.gov (United States)

Jenkins, T C; Thies, E J; Mosley, E E

2001-05-01

Two direct methylation procedures often used for the analysis of total fatty acids in biological samples were evaluated for their application to samples containing fatty amides. Methylation of 5 mg of oleamide (cis-9-octadecenamide) in a one-step (methanolic HCl for 2 h at 70 degrees C) or a two-step (sodium methoxide for 10 min at 50 degrees C followed by methanolic HCl for 10 min at 80 degrees C) procedure gave 59 and 16% conversions of oleamide to oleic acid, respectively. Oleic acid recovery from oleamide was increased to 100% when the incubation in methanolic HCl was lengthened to 16 h and increased to 103% when the incubation in methoxide was modified to 24 h at 100 degrees C. However, conversion of oleamide to oleic acid in an animal feed sample was incomplete for the modified (24 h) two-step procedure but complete for the modified (16 h) one-step procedure. Unsaturated fatty amides in feed and digesta samples can be converted to fatty acid methyl esters by incubation in methanolic HCl if the time of exposure to the acid catalyst is extended from 2 to 16 h.

Procedures for sampling and sample reduction within quality assurance systems for solid biofuels

Energy Technology Data Exchange (ETDEWEB)

NONE

2005-07-01

The objective of this experimental study on sampling was to determine the size and number of samples of biofuels required (taken at two sampling points in each case) and to compare two methods of sampling. The first objective of the sample-reduction exercise was to compare the reliability of various sampling methods, and the second objective was to measure the variations introduced as a result of reducing the sample size to form suitable test portions. The materials studied were sawdust, wood chips, wood pellets and bales of straw, and these were analysed for moisture, ash, particle size and chloride. The sampling procedures are described. The study was conducted in Scandinavia. The results of the study were presented in Leipzig in October 2004. The work was carried out as part of the UK's DTI Technology Programme: New and Renewable Energy.

Sampling and Analysis Plan for the 216-A-29 Ditch

International Nuclear Information System (INIS)

Petersen, S.W.

1998-06-01

This sampling and analysis plan defines procedures to be used for collecting and handling samples to be obtained from the 216-A-29 Ditch, and identifies requirements for field and laboratory measurements. The sampling strategy describes here is derived from a Data Quality Objectives workshop conducted in January 1997 to support sampling to assure worker safety during construction and to assess the validity of a 1988 ditch sampling campaign and the effectiveness of subsequent stabilization. The purpose of the proposed sampling and analysis activities is to characterize soil contamination in the vicinity of a proposed road over the 216-A-29 Ditch

UMTRA project water sampling and analysis plan, Maybell, Colorado

International Nuclear Information System (INIS)

1994-06-01

This water sampling and analysis plan (WSAP) describes planned water sampling activities and provides the regulatory and technical basis for ground water sampling in 1994 at the US Department of Energy's (DOE) Uranium Mill Tailings Remedial Action (UMTRA) Project site in Maybell, Colorado. The WSAP identifies and justifies sampling locations, analytical parameters, and sampling frequencies at the site. The ground water data will be used for site characterization and risk assessment. The regulatory basis for the ground water and surface water monitoring activities is derived from the EPA regulations in 40 CFR Part 192 (1993) and the proposed EPA standards of 1987 (52 FR 36000). Sampling procedures are guided by the UMTRA Project standard operating procedures (SOP) (JEG, n.d.), the Technical Approach Document (TAD) (DOE, 1989), and the most effective technical approach for the site. This WSAP also includes a summary and the results of water sampling activities from 1989 through 1992 (no sampling was performed in 1993)

Modified FlowCAM procedure for quantifying size distribution of zooplankton with sample recycling capacity.

Directory of Open Access Journals (Sweden)

Esther Wong

Full Text Available We have developed a modified FlowCAM procedure for efficiently quantifying the size distribution of zooplankton. The modified method offers the following new features: 1 prevents animals from settling and clogging with constant bubbling in the sample container; 2 prevents damage to sample animals and facilitates recycling by replacing the built-in peristaltic pump with an external syringe pump, in order to generate negative pressure, creates a steady flow by drawing air from the receiving conical flask (i.e. vacuum pump, and transfers plankton from the sample container toward the main flowcell of the imaging system and finally into the receiving flask; 3 aligns samples in advance of imaging and prevents clogging with an additional flowcell placed ahead of the main flowcell. These modifications were designed to overcome the difficulties applying the standard FlowCAM procedure to studies where the number of individuals per sample is small, and since the FlowCAM can only image a subset of a sample. Our effective recycling procedure allows users to pass the same sample through the FlowCAM many times (i.e. bootstrapping the sample in order to generate a good size distribution. Although more advanced FlowCAM models are equipped with syringe pump and Field of View (FOV flowcells which can image all particles passing through the flow field; we note that these advanced setups are very expensive, offer limited syringe and flowcell sizes, and do not guarantee recycling. In contrast, our modifications are inexpensive and flexible. Finally, we compared the biovolumes estimated by automated FlowCAM image analysis versus conventional manual measurements, and found that the size of an individual zooplankter can be estimated by the FlowCAM image system after ground truthing.

Biomass Compositional Analysis Laboratory Procedures | Bioenergy | NREL

Science.gov (United States)

Biomass Compositional Analysis Laboratory Procedures Biomass Compositional Analysis Laboratory Procedures NREL develops laboratory analytical procedures (LAPs) for standard biomass analysis. These procedures help scientists and analysts understand more about the chemical composition of raw biomass

Sampling procedures for inventory of commercial volume tree species in Amazon Forest.

Science.gov (United States)

Netto, Sylvio P; Pelissari, Allan L; Cysneiros, Vinicius C; Bonazza, Marcelo; Sanquetta, Carlos R

2017-01-01

The spatial distribution of tropical tree species can affect the consistency of the estimators in commercial forest inventories, therefore, appropriate sampling procedures are required to survey species with different spatial patterns in the Amazon Forest. For this, the present study aims to evaluate the conventional sampling procedures and introduce the adaptive cluster sampling for volumetric inventories of Amazonian tree species, considering the hypotheses that the density, the spatial distribution and the zero-plots affect the consistency of the estimators, and that the adaptive cluster sampling allows to obtain more accurate volumetric estimation. We use data from a census carried out in Jamari National Forest, Brazil, where trees with diameters equal to or higher than 40 cm were measured in 1,355 plots. Species with different spatial patterns were selected and sampled with simple random sampling, systematic sampling, linear cluster sampling and adaptive cluster sampling, whereby the accuracy of the volumetric estimation and presence of zero-plots were evaluated. The sampling procedures applied to species were affected by the low density of trees and the large number of zero-plots, wherein the adaptive clusters allowed concentrating the sampling effort in plots with trees and, thus, agglutinating more representative samples to estimate the commercial volume.

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.

A random sampling procedure for anisotropic distributions

International Nuclear Information System (INIS)

Nagrajan, P.S.; Sethulakshmi, P.; Raghavendran, C.P.; Bhatia, D.P.

1975-01-01

A procedure is described for sampling the scattering angle of neutrons as per specified angular distribution data. The cosine of the scattering angle is written as a double Legendre expansion in the incident neutron energy and a random number. The coefficients of the expansion are given for C, N, O, Si, Ca, Fe and Pb and these elements are of interest in dosimetry and shielding. (author)

Procedure for conducting a human-reliability analysis for nuclear power plants. Final report

International Nuclear Information System (INIS)

Bell, B.J.; Swain, A.D.

1983-05-01

This document describes in detail a procedure to be followed in conducting a human reliability analysis as part of a probabilistic risk assessment when such an analysis is performed according to the methods described in NUREG/CR-1278, Handbook for Human Reliability Analysis with Emphasis on Nuclear Power Plant Applications. An overview of the procedure describing the major elements of a human reliability analysis is presented along with a detailed description of each element and an example of an actual analysis. An appendix consists of some sample human reliability analysis problems for further study

Phosphorus analysis in milk samples by neutron activation analysis method

International Nuclear Information System (INIS)

Oliveira, R.M. de; Cunha, I.I.L.

1991-01-01

The determination of phosphorus in milk samples by instrumental thermal neutron activation analysis is described. The procedure involves a short irradiation in a nuclear reactor and measurement of the beta radiation emitted by phosphorus - 32 after a suitable decay period. The sources of error were studied and the established method was applied to standard reference materials of known phosphorus content. (author)

Sampling methodology and PCB analysis

International Nuclear Information System (INIS)

Dominelli, N.

1995-01-01

As a class of compounds PCBs are extremely stable and resist chemical and biological decomposition. Diluted solutions exposed to a range of environmental conditions will undergo some preferential degradation and the resulting mixture may differ considerably from the original PCB used as insulating fluid in electrical equipment. The structure of mixtures of PCBs (synthetic compounds prepared by direct chlorination of biphenyl with chlorine gas) is extremely complex and presents a formidable analytical problem, further complicated by the presence of PCBs as contaminants in oils to soils to water. This paper provides some guidance into sampling and analytical procedures; it also points out various potential problems encountered during these processes. The guidelines provided deal with sample collection, storage and handling, sample stability, laboratory analysis (usually gas chromatography), determination of PCB concentration, calculation of total PCB content, and quality assurance. 1 fig

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

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.

Development of SRC-I product analysis. Volume 3. Documentation of procedures

Energy Technology Data Exchange (ETDEWEB)

Schweighardt, F.K.; Kingsley, I.S.; Cooper, F.E.; Kamzelski, A.Z.; Parees, D.M.

1983-09-01

This section documents the BASIC computer program written to simulate Wilsonville's GC-simulated distillation (GCSD) results at APCI-CRSD Trexlertown. The GC conditions used at APCI for the Wilsonville GCSD analysis of coal-derived liquid samples were described in the SRC-I Quarterly Technical Report, April-June 1981. The approach used to simulate the Wilsonville GCSD results is also from an SRC-I Quarterly Technical Report and is reproduced in Appendix VII-A. The BASIC computer program is described in the attached Appendix VII-B. Analysis of gases produced during coal liquefaction generates key information needed to determine product yields for material balance and process control. Gas samples from the coal process development unit (CPDU) and tubing bombs are the primary samples analyzed. A Carle gas chromatographic system was used to analyze coal liquefaction gas samples. A BASIC computer program was written to calculate the gas chromatographic peak area results into mole percent results. ICRC has employed several analytical workup procedures to determine the amount of distillate, oils, asphaltenes, preasphaltenes, and residue in SRC-I process streams. The ASE procedure was developed using Conoco's liquid column fractionation (LC/F) method as a model. In developing the ASE procedure, ICRC was able to eliminate distillation, and therefore quantify the oils fraction in one extraction step. ASE results were shown to be reproducible within +- 2 wt %, and to yield acceptable material balances. Finally, the ASE method proved to be the least affected by sample composition.

Sampling design and procedures for fixed surface-water sites in the Georgia-Florida coastal plain study unit, 1993

Science.gov (United States)

Hatzell, H.H.; Oaksford, E.T.; Asbury, C.E.

1995-01-01

The implementation of design guidelines for the National Water-Quality Assessment (NAWQA) Program has resulted in the development of new sampling procedures and the modification of existing procedures commonly used in the Water Resources Division of the U.S. Geological Survey. The Georgia-Florida Coastal Plain (GAFL) study unit began the intensive data collection phase of the program in October 1992. This report documents the implementation of the NAWQA guidelines by describing the sampling design and procedures for collecting surface-water samples in the GAFL study unit in 1993. This documentation is provided for agencies that use water-quality data and for future study units that will be entering the intensive phase of data collection. The sampling design is intended to account for large- and small-scale spatial variations, and temporal variations in water quality for the study area. Nine fixed sites were selected in drainage basins of different sizes and different land-use characteristics located in different land-resource provinces. Each of the nine fixed sites was sampled regularly for a combination of six constituent groups composed of physical and chemical constituents: field measurements, major ions and metals, nutrients, organic carbon, pesticides, and suspended sediments. Some sites were also sampled during high-flow conditions and storm events. Discussion of the sampling procedure is divided into three phases: sample collection, sample splitting, and sample processing. A cone splitter was used to split water samples for the analysis of the sampling constituent groups except organic carbon from approximately nine liters of stream water collected at four fixed sites that were sampled intensively. An example of the sample splitting schemes designed to provide the sample volumes required for each sample constituent group is described in detail. Information about onsite sample processing has been organized into a flowchart that describes a pathway for each of

Proteome profiling analysis of human ovarian cancer serum samples

International Nuclear Information System (INIS)

Cognetti, F.; Citro, G.

2009-01-01

Mass Spectrometry represents a powerful tool in cancer research to discovery of potential bio markers through peak identification from serum profiling. By using high resolution MALDITOF and bioinformatic analysis almost 400 serum sample homogeneously distributed between biopsy confirmed ovarian cancer and high risk serum samples were analyzed. Each serum sample run in duplicate and whole serum sample preparation procedure has been performed by Hamilton Star Robot in order to reduce bias and the replicates with a low Pearson coefficient are removed. After automated reverse phase magnetic beads separation the samples were tested in MALDI-TOF

A highly rationalized procedure of neutron activation analysis for routine applications in dairy science

International Nuclear Information System (INIS)

Heine, K.; Wiechen, A.

1976-01-01

A rational procedure was developed for the multi-element analysis by neutron activation for applications in dairy science. The preparation of samples prior to irradiation consists of drying, weighing, and welding in quartz ampoules. The neutron flux, samples are exposed to during reactor irradiation , is determined by the mono-comparator technique for which the Co-content of a commercial aluminium foil was chosen as the flux monitor. Constancy of the Co-content and uncomplicated handling of the foil essentially simplify the determination of flux. The samples are irradiated for 72 h, dissolved in HNO 3 /H 2 SO 4 and measured in the liquid state after waiting times of 1-2, 4 and 8 weeks by a Ge(Li)-detector and a 4,096 channel spectrometer. The procedure was confirmed by investigations of the biological KALE standard and by participation in inter-comparisons of biological substances of the Analytical Quality Control Service of the IAEA for the analysis of the elements Na, Ca, Cr, Fe, Co, Zn, Se, Rb, and Cs. So a procedure was developed suitable for routine multi-element analysis of biologic samples by optimizing and rationalizing all analytical steps. (orig./MG) [de

A headspace solid-phase microextraction procedure coupled with gas chromatography-mass spectrometry for the analysis of volatile polycyclic aromatic hydrocarbons in milk samples

Energy Technology Data Exchange (ETDEWEB)

Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

2008-06-15

A sensitive and solvent-free method for the determination of ten polycyclic aromatic hydrocarbons, namely, naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene and chrysene, with up to four aromatic rings, in milk samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry detection has been developed. A polydimethylsiloxane-divinylbenzene fiber was chosen and used at 75 C for 60 min. Detection limits ranging from 0.2 to 5 ng L{sup -1} were attained at a signal-to-noise ratio of 3, depending on the compound and the milk sample under analysis. The proposed method was applied to ten different milk samples and the presence of six of the analytes studied in a skimmed milk with vegetal fiber sample was confirmed. The reliability of the procedure was verified by analyzing two different certified reference materials and by recovery studies. (orig.)

UMTRA project water sampling and analysis plan, Tuba City, Arizona

International Nuclear Information System (INIS)

1996-02-01

Planned, routine ground water sampling activities at the U.S. Department of Energy (DOE) Uranium Mill Tailings Remedial Action (UMTRA) Project site in Tuba City, Arizona, are described in the following sections of this water sampling and analysis plan (WSAP). This plan identifies and justifies the sampling locations, analytical parameters, detection limits, and sampling frequency for the stations routinely monitored at the site. The ground water data are used for site characterization and risk assessment. The regulatory basis for routine ground water monitoring at UMTRA Project sites is derived from the U.S. Environmental Protection Agency (EPA) regulations in 40 CFR Part 192 (1994) and the final EPA standards of 1995 (60 FR 2854). Sampling procedures are guided by the UMTRA Project standard operating procedures (SOP) (JEG, n.d.), and the most effective technical approach for the site

Experimental design technique applied to the validation of an instrumental Neutron Activation Analysis procedure

International Nuclear Information System (INIS)

Santos, Uanda Paula de M. dos; Moreira, Edson Gonçalves

2017-01-01

In this study optimization of procedures and standardization of Instrumental Neutron Activation Analysis (INAA) method were carried out for the determination of the elements bromine, chlorine, magnesium, manganese, potassium, sodium and vanadium in biological matrix materials using short irradiations at a pneumatic system. 2 k experimental designs were applied for evaluation of the individual contribution of selected variables of the analytical procedure in the final mass fraction result. The chosen experimental designs were the 2 3 and the 2 4 , depending on the radionuclide half life. Different certified reference materials and multi-element comparators were analyzed considering the following variables: sample decay time, irradiation time, counting time and sample distance to detector. Comparator concentration, sample mass and irradiation time were maintained constant in this procedure. By means of the statistical analysis and theoretical and experimental considerations, it was determined the optimized experimental conditions for the analytical methods that will be adopted for the validation procedure of INAA methods in the Neutron Activation Analysis Laboratory (LAN) of the Research Reactor Center (CRPq) at the Nuclear and Energy Research Institute (IPEN /CNEN-SP). Optimized conditions were estimated based on the results of z-score tests, main effect, interaction effects and better irradiation conditions. (author)

Experimental design technique applied to the validation of an instrumental Neutron Activation Analysis procedure

Energy Technology Data Exchange (ETDEWEB)

Santos, Uanda Paula de M. dos; Moreira, Edson Gonçalves, E-mail: uandapaula@gmail.com, E-mail: emoreira@ipen.br [Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP), São Paulo, SP (Brazil)

2017-07-01

In this study optimization of procedures and standardization of Instrumental Neutron Activation Analysis (INAA) method were carried out for the determination of the elements bromine, chlorine, magnesium, manganese, potassium, sodium and vanadium in biological matrix materials using short irradiations at a pneumatic system. 2{sup k} experimental designs were applied for evaluation of the individual contribution of selected variables of the analytical procedure in the final mass fraction result. The chosen experimental designs were the 2{sup 3} and the 2{sup 4}, depending on the radionuclide half life. Different certified reference materials and multi-element comparators were analyzed considering the following variables: sample decay time, irradiation time, counting time and sample distance to detector. Comparator concentration, sample mass and irradiation time were maintained constant in this procedure. By means of the statistical analysis and theoretical and experimental considerations, it was determined the optimized experimental conditions for the analytical methods that will be adopted for the validation procedure of INAA methods in the Neutron Activation Analysis Laboratory (LAN) of the Research Reactor Center (CRPq) at the Nuclear and Energy Research Institute (IPEN /CNEN-SP). Optimized conditions were estimated based on the results of z-score tests, main effect, interaction effects and better irradiation conditions. (author)

9 CFR 147.8 - Procedures for preparing egg yolk samples for diagnostic tests.

Science.gov (United States)

2010-01-01

... samples for diagnostic tests. 147.8 Section 147.8 Animals and Animal Products ANIMAL AND PLANT HEALTH... IMPROVEMENT PLAN Blood Testing Procedures § 147.8 Procedures for preparing egg yolk samples for diagnostic... for diagnostic testing. (b) The authorized laboratory must identify each egg as to the breeding flock...

CARVEDILOL POPULATION PHARMACOKINETIC ANALYSIS – APPLIED VALIDATION PROCEDURE

Directory of Open Access Journals (Sweden)

Aleksandra Catić-Đorđević

2013-09-01

Full Text Available Carvedilol is a nonselective beta blocker/alpha-1 blocker, which is used for treatment of essential hypertension, chronic stable angina, unstable angina and ischemic left ventricular dysfunction. The aim of this study was to describe carvedilol population pharmacokinetic (PK analysis as well as the validation of analytical procedure, which is an important step regarding this approach. In contemporary clinical practice, population PK analysis is often more important than standard PK approach in setting a mathematical model that describes the PK parameters. Also, it includes the variables that have particular importance in the drugs pharmacokinetics such as sex, body mass, dosage, pharmaceutical form, pathophysiological state, disease associated with the organism or the presence of a specific polymorphism in the isoenzyme important for biotransformation of the drug. One of the most frequently used approach in population PK analysis is the Nonlinear Modeling of Mixed Effects - NONMEM modeling. Analytical methods used in the data collection period is of great importance for the implementation of a population PK analysis of carvedilol in order to obtain reliable data that can be useful in clinical practice. High performance liquid chromatography (HPLC analysis of carvedilol is used to confirm the identity of a drug and provide quantitative results and also to monitor the efficacy of the therapy. Analytical procedures used in other studies could not be fully implemented in our research as it was necessary to perform certain modification and validation of the method with the aim of using the obtained results for the purpose of a population pharmacokinetic analysis. Validation process is a logical terminal phase of analytical procedure development that provides applicability of the procedure itself. The goal of validation is to ensure consistency of the method and accuracy of results or to confirm the selection of analytical method for a given sample

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.

Remarks on the sampling procedures for polycyclic aromatic hydrocarbons from the atmosphere

Energy Technology Data Exchange (ETDEWEB)

Tomingas, R [Duesseldorf Univ. (Germany, F.R.). Inst. fuer Lufthygiene und Silikoseforschung

1979-01-01

Despite all efforts to optimize the sampling procedure for polycyclic aromatic hydrocarbons (PAH) a part of the PAH is lost during the sampling period. The amount of loss depends on the vapour pressure, the air flow rate, the oxidants in the suspended matter and on the sampling time. The sampling time in return is determined by the PAH concentration in the atmosphere and cannot be shortened infinitely, at least not at the expense of the air flow rate. When the concentration of the PAH is extremely low, a repeated change of the filters is advisable. Losses of PAH even occur when filters are stored in the dark. An evaluation of these losses is difficult for many reasons. There is no relationship between the amount of loss and time unit; the decrease of each PAH is different and seems to depend on the composition of the particulate matter collected on the filter. The disappearance of the PAH from the filter is a continual process, therefore a rapid performance of the analysis is inevitable.

On the assessment of extremely low breakdown probabilities by an inverse sampling procedure [gaseous insulation

DEFF Research Database (Denmark)

Thyregod, Poul; Vibholm, Svend

1991-01-01

the flashover probability function and the corresponding distribution of first breakdown voltages under the inverse sampling procedure, and show how this relation may be utilized to assess the single-shot flashover probability corresponding to the observed average first breakdown voltage. Since the procedure......First breakdown voltages obtained under the inverse sampling procedure assuming a double exponential flashover probability function are discussed. An inverse sampling procedure commences the voltage application at a very low level, followed by applications at stepwise increased levels until...... is based on voltage applications in the neighbourhood of the quantile under investigation, the procedure is found to be insensitive to the underlying distributional assumptions...

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)

Relations among conceptual knowledge, procedural knowledge, and procedural flexibility in two samples differing in prior knowledge.

Science.gov (United States)

Schneider, Michael; Rittle-Johnson, Bethany; Star, Jon R

2011-11-01

Competence in many domains rests on children developing conceptual and procedural knowledge, as well as procedural flexibility. However, research on the developmental relations between these different types of knowledge has yielded unclear results, in part because little attention has been paid to the validity of the measures or to the effects of prior knowledge on the relations. To overcome these problems, we modeled the three constructs in the domain of equation solving as latent factors and tested (a) whether the predictive relations between conceptual and procedural knowledge were bidirectional, (b) whether these interrelations were moderated by prior knowledge, and (c) how both constructs contributed to procedural flexibility. We analyzed data from 2 measurement points each from two samples (Ns = 228 and 304) of middle school students who differed in prior knowledge. Conceptual and procedural knowledge had stable bidirectional relations that were not moderated by prior knowledge. Both kinds of knowledge contributed independently to procedural flexibility. The results demonstrate how changes in complex knowledge structures contribute to competence development.

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

Comparison of two sample preparation procedures for HPLC determination of ochratoxin A

Directory of Open Access Journals (Sweden)

Vuković Gorica L.

2009-01-01

Full Text Available In preparation of samples for chromatographic determination of ochratoxin A, two types of columns were used for sample cleanup (SPE and immunoaffinity columns. The first method consisted of liquid-liquid extraction with a mixture of chloroform and phosphoric acid, followed by ion-exchange cleanup on Waters Oasis MAX columns. The sec­ond method consisted of extraction with a mixture of water and methanol, followed by LCTech OtaCLEAN immunoaf­finity column cleanup. Recoveries of the methods were determined at three levels in three repetitions for maize flour, and they were 84% (%RSD = 19.2 for the first method of sample preparation and 101% (%RSD = 2.2 for the second method. Values of LOQ for OTA were 0.25 and 1.00 μg/kg for the IAC and SPE clean-up procedures, respectively. Both methods comply with present regulations, but the MAX sample clean-up procedure should be used as an alternative, since the immunoaffinity column clean-up procedure is characterized by better reproducibility, accuracy, and efficiency.

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

Membrane biofouling characterization: effects of sample preparation procedures on biofilm structure and the microbial community

KAUST Repository

Xue, Zheng

2014-07-15

Ensuring the quality and reproducibility of results from biofilm structure and microbial community analysis is essential to membrane biofouling studies. This study evaluated the impacts of three sample preparation factors (ie number of buffer rinses, storage time at 4°C, and DNA extraction method) on the downstream analysis of nitrifying biofilms grown on ultrafiltration membranes. Both rinse and storage affected biofilm structure, as suggested by their strong correlation with total biovolume, biofilm thickness, roughness and the spatial distribution of EPS. Significant variations in DNA yields and microbial community diversity were also observed among samples treated by different rinses, storage and DNA extraction methods. For the tested biofilms, two rinses, no storage and DNA extraction with both mechanical and chemical cell lysis from attached biofilm were the optimal sample preparation procedures for obtaining accurate information about biofilm structure, EPS distribution and the microbial community. © 2014 © 2014 Taylor & Francis.

Double-Shell Tank (DST) Ventilation System Vapor Sampling and Analysis Plan

International Nuclear Information System (INIS)

SASAKI, L.M.

2000-01-01

This sampling and analysis plan (SAP) identifies characterization objectives pertaining to sample collection, laboratory analytical evaluation, and reporting requirements for vapor samples from the primary ventilation systems of the AN, AP, AW, and AY/AZ tank farms. Sampling will be performed in accordance with Data Quality Objectives for Regulatory Requirements for Hazardous and Radioactive Air Emissions Sampling and Analysis (Air DQO) (Mulkey 1999). The sampling will verify if current air emission estimates used in the permit application are correct and provide information for future air permit applications. Vapor samples will be obtained from tank farm ventilation systems, downstream from the tanks and upstream of any filtration. Samples taken in support of the DQO will consist of SUMMA(trademark) canisters, triple sorbent traps (TSTs), sorbent tube trains (STTs), polyurethane foam (PUF) samples. Particulate filter samples and tritium traps will be taken for radiation screening to allow the release of the samples for analysis. The following sections provide the general methodology and procedures to be used in the preparation, retrieval, transport, analysis, and reporting of results from the vapor samples

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.

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

Multielemental analysis of 18 essential and toxic elements in amniotic fluid samples by ICP-MS: Full procedure validation and estimation of measurement uncertainty.

Science.gov (United States)

Markiewicz, B; Sajnóg, A; Lorenc, W; Hanć, A; Komorowicz, I; Suliburska, J; Kocyłowski, R; Barałkiewicz, D

2017-11-01

Amniotic fluid is the substantial factor in the development of an embryo and fetus due to the fact that water and solutes contained in it penetrate the fetal membranes in an hydrostatic and osmotic way as well as being swallowed by the fetus. Elemental composition of amniotic fluid influences the growth and health of the fetus, therefore, an analysis of amniotic fluid is important because the results would indicate abnormal levels of minerals or toxic elements. Inductively coupled plasma mass spectroscopy (ICP-MS) is often used for determination of trace and ultra-trace level elements in a wide range of matrices including biological samples because of its unique analytical capabilities. In the case of trace and ultra-trace level analysis detailed characteristics of analytical procedure as well as properties of the analytical result are particularly important. The purpose of this study was to develop a new analytical procedure for multielemental analysis of 18 elements (Al, As, Ba, Ca, Cd, Co, Cr, Cu, Mg, Mn, Ni, Pb, Sb, Se, Sr, U, V and Zn) in amniotic fluid samples using ICP-MS. Dynamic reaction cell (DRC) with two reaction gases, ammonia and oxygen, was involved in the experiment to eliminate spectral interferences. Detailed validation was conducted using 3 certified reference mterials (CRMs) and real amniotic fluid samples collected from patients. Repeatability for all analyzed analytes was found to range from 0.70% to 8.0% and for intermediate precision results varied from 1.3% to 15%. Trueness expressed as recovery ranged from 80% to 125%. Traceability was assured through the analyses of CRMs. Uncertainty of the results was also evaluated using single-laboratory validation approach. The obtained expanded uncertainty (U) results for CRMs, expressed as a percentage of the concentration of an analyte, were found to be between 8.3% for V and 45% for Cd. Standard uncertainty of the precision was found to have a greater influence on the combined standard uncertainty

Biomass Thermogravimetric Analysis: Uncertainty Determination Methodology and Sampling Maps Generation

Science.gov (United States)

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

2010-01-01

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

BEAMGAA. A chance for high precision analysis of big samples

International Nuclear Information System (INIS)

Goerner, W.; Berger, A.; Haase, O.; Segebade, Chr.; Alber, D.; Monse, G.

2005-01-01

In activation analysis of traces in small samples, the non-equivalence of the activating radiation doses of sample and calibration material gives rise to sometimes tolerable systematic errors. Conversely, analysis of major components usually demands high trueness and precision. To meet this, beam geometry activation analysis (BEAMGAA) procedures have been developed for instrumental photon (IPAA) and neutron activation analysis (INAA) in which the activating neutron/photon beam exhibits broad, flat-topped characteristics. This results in a very low lateral activating flux gradient compared to known radiation facilities, however, at significantly lower flux density. The axial flux gradient can be accounted for by a monitor-sample-monitor assembly. As a first approach, major components were determined in high purity substances as well as selenium in a cattle fodder additive. (author)

Sampling and analysis methods for geothermal fluids and gases

Energy Technology Data Exchange (ETDEWEB)

Watson, J.C.

1978-07-01

The sampling procedures for geothermal fluids and gases include: sampling hot springs, fumaroles, etc.; sampling condensed brine and entrained gases; sampling steam-lines; low pressure separator systems; high pressure separator systems; two-phase sampling; downhole samplers; and miscellaneous methods. The recommended analytical methods compiled here cover physical properties, dissolved solids, and dissolved and entrained gases. The sequences of methods listed for each parameter are: wet chemical, gravimetric, colorimetric, electrode, atomic absorption, flame emission, x-ray fluorescence, inductively coupled plasma-atomic emission spectroscopy, ion exchange chromatography, spark source mass spectrometry, neutron activation analysis, and emission spectrometry. Material on correction of brine component concentrations for steam loss during flashing is presented. (MHR)

40 CFR 90.413 - Exhaust sample procedure-gaseous components.

Science.gov (United States)

2010-07-01

...-analysis values. (3) Measure and record HC, CO, CO2, and NOX concentrations in the exhaust sample bag(s...-analysis values. (7) Collect background HC, CO, CO2, and NOX in a sample bag (for dilute exhaust sampling...: (1) For dilute grab (“bag”) sample analysis, the analyzer response must be stable at greater than 99...

Gas chromatographic-mass spectrometric analysis of urinary volatile organic metabolites: Optimization of the HS-SPME procedure and sample storage conditions.

Science.gov (United States)

Živković Semren, Tanja; Brčić Karačonji, Irena; Safner, Toni; Brajenović, Nataša; Tariba Lovaković, Blanka; Pizent, Alica

2018-01-01

Non-targeted metabolomics research of human volatile urinary metabolome can be used to identify potential biomarkers associated with the changes in metabolism related to various health disorders. To ensure reliable analysis of urinary volatile organic metabolites (VOMs) by gas chromatography-mass spectrometry (GC-MS), parameters affecting the headspace-solid phase microextraction (HS-SPME) procedure have been evaluated and optimized. The influence of incubation and extraction temperatures and times, coating fibre material and salt addition on SPME efficiency was investigated by multivariate optimization methods using reduced factorial and Doehlert matrix designs. The results showed optimum values for temperature to be 60°C, extraction time 50min, and incubation time 35min. The proposed conditions were applied to investigate urine samples' stability regarding different storage conditions and freeze-thaw processes. The sum of peak areas of urine samples stored at 4°C, -20°C, and -80°C up to six months showed a time dependent decrease over time although storage at -80°C resulted in a slight non-significant reduction comparing to the fresh sample. However, due to the volatile nature of the analysed compounds, more than two cycles of freezing/thawing of the sample stored for six months at -80°C should be avoided whenever possible. Copyright © 2017 Elsevier B.V. All rights reserved.

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

International Nuclear Information System (INIS)

Markert, B.

1992-01-01

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

Recommended practice for process sampling for partial pressure analysis

International Nuclear Information System (INIS)

Blessing, James E.; Ellefson, Robert E.; Raby, Bruce A.; Brucker, Gerardo A.; Waits, Robert K.

2007-01-01

This Recommended Practice describes and recommends various procedures and types of apparatus for obtaining representative samples of process gases from >10 -2 Pa (10 -4 Torr) for partial pressure analysis using a mass spectrometer. The document was prepared by a subcommittee of the Recommended Practices Committee of the American Vacuum Society. The subcommittee was comprised of vacuum users and manufacturers of mass spectrometer partial pressure analyzers who have practical experience in the sampling of process gas atmospheres

Quality-assurance procedures: Method 5G determination of particulate emissions from wood heaters from a dilution tunnel sampling location

Energy Technology Data Exchange (ETDEWEB)

Ward, T.E.; Hartman, M.W.; Olin, R.C.; Rives, G.D.

1989-06-01

Quality-assurance procedures are contained in this comprehensive document intended to be used as an aid for wood-heater manufacturers and testing laboratories in performing particulate matter sampling of wood heaters according to EPA protocol, Method 5G. These procedures may be used in research and development, and as an aid in auditing and certification testing. A detailed, step-by-step quality assurance guide is provided to aid in the procurement and assembly of testing apparatus, to clearly describe the procedures, and to facilitate data collection and reporting. Suggested data sheets are supplied that can be used as an aid for both recordkeeping and certification applications. Throughout the document, activity matrices are provided to serve as a summary reference. Checklists are also supplied that can be used by testing personnel. Finally, for the purposes of ensuring data quality, procedures are outlined for apparatus operation, maintenance, and traceability. These procedures combined with the detailed description of the sampling and analysis protocol will help ensure the accuracy and reliability of Method 5G emission-testing results.

A radiochemical procedure for a low-level measurement of ''241Am in environmental samples using a supported functional organo phosphorus extractant

International Nuclear Information System (INIS)

Gasco, C.; Anton, M. P.; Alvarez, A.; Navarro, N.; Salvador, S.

1994-01-01

The transuranides analysis in environmental samples is carried out by CIEMAT using standardized methods based on sequential separation with ionic-exchange resins. The americium fraction is purified through a two-layer ion exchange column and lately in an anion-exchange column in nitric acid methanol medium. The technique is time consuming and the results are not completely satisfactory (low recovery and loss of a-resolution) for some samples. The chemical compound CMPO (octyl(phenyl)-N,N-diisobutyl carbomoylmethyiphosphine oxide) dissolved in TPB (tributyl phosphate) and supported on an inert substrate has been tested directly for ''241Am analysis by a large number of laboratories. A new method that combines both procedures has been developed. The details of the improved procedure are described in this paper. The advantages of its application to environmental samples (urine, faeces and sediments) are discussed. The utilization of standard samples, with americium certified concentrations confirms the reliability of our measurements. (Author) 8 refs

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

UMTRA Project water sampling and analysis plan, Durango, Colorado. Revision 1

International Nuclear Information System (INIS)

1995-09-01

Planned, routine ground water sampling activities at the US Department of Energy (DOE) Uranium Mill Tailings Remedial Action (UMTRA) Project site in Durango, Colorado, are described in this water sampling and analysis plan. The plan identifies and justifies the sampling locations, analytical parameters, detection limits, and sampling frequency for the routine monitoring stations at the site. The ground water data are used to characterize the site ground water compliance strategies and to monitor contaminants of potential concern identified in the baseline risk assessment (DOE, 1995a). Regulatory basis for routine ground water monitoring at UMTRA Project sites is derived from the US EPA regulations in 40 CFR Part 192 (1994) and EPA standards of 1995 (60 FR 2854). Sampling procedures are guided by the UMTRA Project standard operating procedures (SOP) (JEG, n.d.), the Technical Approach Document (TAD) (DOE, 1989), and the most effective technical approach for the site

Safety analysis procedures for PHWR

International Nuclear Information System (INIS)

Min, Byung Joo; Kim, Hyoung Tae; Yoo, Kun Joong

2004-03-01

The methodology of safety analyses for CANDU reactors in Canada, a vendor country, uses a combination of best-estimate physical models and conservative input parameters so as to minimize the uncertainty of the plant behavior predictions. As using the conservative input parameters, the results of the safety analyses are assured the regulatory requirements such as the public dose, the integrity of fuel and fuel channel, the integrity of containment and reactor structures, etc. However, there is not the comprehensive and systematic procedures for safety analyses for CANDU reactors in Korea. In this regard, the development of the safety analyses procedures for CANDU reactors is being conducted not only to establish the safety analyses system, but also to enhance the quality assurance of the safety assessment. In the first phase of this study, the general procedures of the deterministic safety analyses are developed. The general safety procedures are covered the specification of the initial event, selection of the methodology and accident sequences, computer codes, safety analysis procedures, verification of errors and uncertainties, etc. Finally, These general procedures of the safety analyses are applied to the Large Break Loss Of Coolant Accident (LBLOCA) in Final Safety Analysis Report (FSAR) for Wolsong units 2, 3, 4

The method of Sample Management in Neutron Activation Analysis Laboratory-Serpong

International Nuclear Information System (INIS)

Elisabeth-Ratnawati

2005-01-01

In the testing laboratory used by neutron activation analysis method, sample preparation is the main factor and it can't be neglect. The error in the sample preparation can give result with lower accuracy. In this article is explained the scheme of sample preparation i.e sample receive administration, the separate of sample, fluid and solid sample preparation, sample grouping, irradiation, sample counting and holding the sample post irradiation. If the management of samples were good application based on Standard Operation Procedure, therefore each samples has good traceability. To optimize the management of samples is needed the trained and skilled personal and good facility. (author)

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

Science.gov (United States)

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

2017-08-13

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

Development of Radioanalytical and Microanalytical Procedures for the Determination of Actinides in Environmental Samples

International Nuclear Information System (INIS)

Macsik, Zsuzsanna; Vajda, Nora; Bene, Balazs; Varga, Zsolt

2008-01-01

A radio-analytical procedure has been developed for the simultaneous determination of actinides in swipe samples by alpha-spectrometry after the separation of the actinides by extraction chromatography. The procedure is based on the complete decomposition of the sample by destruction with microwave digestion or ashing in furnace. Actinides are separated on an extraction chromatographic column filled with TRU resin (product of Eichrom Industries Inc.). Alpha sources prepared from the separated fractions of americium, plutonium, thorium and uranium are counted by alpha spectrometry. Micro-analytical procedure is being developed for the location and identification of individual particles containing fissile material using solid state nuclear track detectors. The parameters of alpha and fission track detection have been optimized and a procedure has been elaborated to locate the particles on the sample by defining the coordinates of the tracks created by the particles on the track detector. Development of a procedure is planned to separate the located particles using micromanipulator and these particles will be examined individually by different micro- and radio-analytical techniques. (authors)

Development of Radioanalytical and Microanalytical Procedures for the Determination of Actinides in Environmental Samples

Energy Technology Data Exchange (ETDEWEB)

Macsik, Zsuzsanna [Institute of Nuclear Techniques, Moegyetem rakpart 9, H-1111 Budapest (Hungary); Vajda, Nora [RadAnal Ltd., Bimbo ut 119/a, H-1026 Budapest (Hungary); Bene, Balazs [National Institute of Standards and Technology, Gaithersburg, MD 20899 (United States); Varga, Zsolt [Institute of Isotopes, Konkoly-Thege M. ut 29-33, H-1121 Budapest (Hungary)

2008-07-01

A radio-analytical procedure has been developed for the simultaneous determination of actinides in swipe samples by alpha-spectrometry after the separation of the actinides by extraction chromatography. The procedure is based on the complete decomposition of the sample by destruction with microwave digestion or ashing in furnace. Actinides are separated on an extraction chromatographic column filled with TRU resin (product of Eichrom Industries Inc.). Alpha sources prepared from the separated fractions of americium, plutonium, thorium and uranium are counted by alpha spectrometry. Micro-analytical procedure is being developed for the location and identification of individual particles containing fissile material using solid state nuclear track detectors. The parameters of alpha and fission track detection have been optimized and a procedure has been elaborated to locate the particles on the sample by defining the coordinates of the tracks created by the particles on the track detector. Development of a procedure is planned to separate the located particles using micromanipulator and these particles will be examined individually by different micro- and radio-analytical techniques. (authors)

Tank 241-U-106 vapor sampling and analysis tank characterization report

International Nuclear Information System (INIS)

Huckaby, J.L.

1995-01-01

This report presents the details of the Hanford waste tank characterization study for tank 241-U-106. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected to determine the potential risks to tank farm workers due to fugitive emissions from the tank

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.

PIXE analysis of Nigerian flour and bread samples

Science.gov (United States)

Olise, Felix S.; Fernandes, Adriana M.; Cristina Chaves, P.; Taborda, Ana; Reis, Miguel A.

2014-01-01

The alleged use of potassium bromate (KBrO3) in bread baking led a few authors to report on the chemical methods for the determination of KBrO3 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.

Evaluation of some procedures relevant to the determination of trace elemental components in biological materials by destructive neutron activation analysis

International Nuclear Information System (INIS)

Berry, D.L.

1979-01-01

The development of a simplified procedure for the analysis of biological materials by destructive neutron activation analysis (DNAA) is described. The sample manipulations preceding gamma ray assay were investigated as five specific stages of processing: (1) pre-irradiation treatment; (2) sample irradiation; (3) removal of the organic matrix; (4) removal of interfering radioactivities; and (5) concentration and separation of analyte activities. Each stage was evaluated with respect to susceptibility to sample contamination, loss of trace elemental components, and compatibility with other operations in the overall DNAA procedures. A complete DNAA procedure was proposed and evaluated for the analysis of standard bovine liver and blood samples. The DNAA system was effective for the determination of As, Cu, Fe, Hg, Mo, Rb, Sb, Se, and Zn without yield determinations and with a minimum turn-around time of approximately 3 days

Evaluation of some procedures relevant to the determination of trace elemental components in biological materials by destructive neutron activation analysis

Energy Technology Data Exchange (ETDEWEB)

Berry, D.L.

1979-01-01

The development of a simplified procedure for the analysis of biological materials by destructive neutron activation analysis (DNAA) is described. The sample manipulations preceding gamma ray assay were investigated as five specific stages of processing: (1) pre-irradiation treatment; (2) sample irradiation; (3) removal of the organic matrix; (4) removal of interfering radioactivities; and (5) concentration and separation of analyte activities. Each stage was evaluated with respect to susceptibility to sample contamination, loss of trace elemental components, and compatibility with other operations in the overall DNAA procedures. A complete DNAA procedure was proposed and evaluated for the analysis of standard bovine liver and blood samples. The DNAA system was effective for the determination of As, Cu, Fe, Hg, Mo, Rb, Sb, Se, and Zn without yield determinations and with a minimum turn-around time of approximately 3 days.

Determination of calcium, potassium, manganese, iron, copper and zinc levels in representative samples of two onion cultivars using total reflection X-ray fluorescence and ultrasound extraction procedure

International Nuclear Information System (INIS)

Alvarez, J.; Marco, L.M.; Arroyo, J.; Greaves, E.D.; Rivas, R.

2003-01-01

The chemical characterization of onion cultivar samples is an important tool for the enhancement of their productivity due to the fact that chemical composition is closed related to the quality of the products. A new sample preparation procedure for elemental characterization is proposed, involving the acid extraction of the analytes from crude samples by means of an ultrasonic bath, avoiding the required digestion of samples in vegetable tissue analysis. The technique of total reflection X-ray fluorescence (TXRF) was successfully applied for the simultaneous determination of the elements Ca, K, Mn, Fe, Cu and Zn. The procedure was compared with the wet ashing and dry ashing procedures for all the elements using multivariate analysis and the Scheffe test. The technique of flame atomic absorption spectrometry (FAAS) was employed for comparison purposes and accuracy evaluation of the proposed analysis method. A good agreement between the two techniques was found when using the dry ashing and ultrasound leaching procedures. The levels of each element found for representative samples of two onion cultivars (Yellow Granex PRR 502 and 438 Granex) were also compared by the same method. Levels of K, Mn and Zn were significantly higher in the 438 Granex cultivar, while levels of Ca, Fe and Cu were significantly higher in the Yellow Granex PRR 502 cultivar

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.

Sampling and analysis plan for the consolidated sludge samples from the canisters and floor of the 105-K East basin

International Nuclear Information System (INIS)

BAKER, R.B.

1999-01-01

This Sampling and Analysis Plan (SAP) provides direction for sampling of fuel canister and floor Sludge from the K East Basin to complete the inventory of samples needed for Sludge treatment process testing. Sample volumes and sources consider recent reviews made by the Sludge treatment subproject. The representative samples will be characterized to the extent needed for the material to be used effectively for testing. Sampling equipment used allows drawing of large volume sludge samples and consolidation of sample material from a number of basin locations into one container. Once filled, the containers will be placed in a cask and transported to Hanford laboratories for recovery and evaluation. Included in the present SAP are the logic for sample location selection, laboratory analysis procedures required, and reporting needed to meet the Data Quality Objectives (DQOs) for this initiative

Polychlorinated biphenyls (PCB) analysis report for solid sample for 219S tank 102

International Nuclear Information System (INIS)

Ross, G.A.

1997-01-01

One waste sample was analyzed (with duplicate, matrix spike, and matrix spike duplicate) for PCBs as Aroclor mixtures by the Inorganic/Organic Chemistry Group. A soxhlet extraction procedure was used for extraction of the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). Extraction follows closely method 354 C of SW-846, analysis follows SW-846 method 8082. A cross reference of laboratory sample number to the customer identification is given in a table

Tank 241-TY-101 vapor sampling and analysis tank characterization report

International Nuclear Information System (INIS)

Huckaby, J.L.

1995-01-01

This report presents the details of the Hanford waste tank characterization study for tank 241-TY-101. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedure that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

Tank 241-C-107 vapor sampling and analysis tank characterization report

International Nuclear Information System (INIS)

Huckaby, J.L.

1995-01-01

This report presents the details of the Hanford waste tank characterization study for tank 241-C-107. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

Tank 241-C-102 vapor sampling and analysis tank characterization report

International Nuclear Information System (INIS)

Huckaby, J.L.

1995-01-01

This report presents the details of the Hanford waste tank characterization study for tank 241-C-102. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

Tank 241-B-103 vapor sampling and analysis tank characterization report

International Nuclear Information System (INIS)

Huckaby, J.L.

1995-01-01

This report presents the details of the Hanford waste tank characterization study for tank 241-B-103. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedure that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

Tank 241-BX-104 vapor sampling and analysis tank characterization report

International Nuclear Information System (INIS)

Huckaby, J.L.

1995-01-01

This report presents the details of the Hanford waste tank characterization study for tank 241-BX-104. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedure that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

Tank 241-SX-106 vapor sampling and analysis tank characterization report

International Nuclear Information System (INIS)

Huckaby, J.L.

1995-01-01

This report presents the details of the Hanford waste tank characterization study for tank 241-SX-106. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedure that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

Tank 241-T-107 vapor sampling and analysis tank characterization report

International Nuclear Information System (INIS)

Huckaby, J.L.

1995-01-01

This report presents the details of the Hanford waste tank characterization study for tank 241-T-107. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedure that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

Implementation guide for turbidity threshold sampling: principles, procedures, and analysis

Science.gov (United States)

Jack Lewis; Rand Eads

2009-01-01

Turbidity Threshold Sampling uses real-time turbidity and river stage information to automatically collect water quality samples for estimating suspended sediment loads. The system uses a programmable data logger in conjunction with a stage measurement device, a turbidity sensor, and a pumping sampler. Specialized software enables the user to control the sampling...

Operability test procedure for PFP wastewater sampling facility

International Nuclear Information System (INIS)

Hirzel, D.R.

1995-01-01

Document provides instructions for performing the Operability Test of the 225-WC Wastewater Sampling Station which monitors the discharge to the Treated Effluent Disposal Facility from the Plutonium Finishing Plant. This Operability Test Procedure (OTP) has been prepared to verify correct configuration and performance of the PFP Wastewater sampling system installed in Building 225-WC located outside the perimeter fence southeast of the Plutonium Finishing Plant (PFP). The objective of this test is to ensure the equipment in the sampling facility operates in a safe and reliable manner. The sampler consists of two Manning Model S-5000 units which are rate controlled by the Milltronics Ultrasonic flowmeter at manhole No.C4 and from a pH measuring system with the sensor in the stream adjacent to the sample point. The intent of the dual sampling system is to utilize one unit to sample continuously at a rate proportional to the wastewater flow rate so that the aggregate tests are related to the overall flow and thereby eliminate isolated analyses. The second unit will only operate during a high or low pH excursion of the stream (hence the need for a pH control). The major items in this OTP include testing of the Manning Sampler System and associated equipment including the pH measuring and control system, the conductivity monitor, and the flow meter

Elemental hair analysis: A review of procedures and applications

International Nuclear Information System (INIS)

Pozebon, D.; Scheffler, G.L.; Dressler, V.L.

2017-01-01

Although exogenous contamination and unreliable reference values have limited the utility of scalp hair as a biomarker of chemical elements exposure, its use in toxicological, clinical, environmental and forensic investigations is growing and becoming more extensive. Therefore, hair elemental analysis is reviewed in the current manuscript which spans articles published in the last 10 years. It starts with a general discussion of history, morphology and possible techniques for elemental analysis, where inductively coupled plasma-mass spectrometry (ICP-MS) is clearly highlighted since this technique is leading quantitative ultra-trace elemental analysis. Emphasis over sampling, quality assurance, washing procedures and sample decomposition is given with detailed protocols compiled in tables as well as the utility of hair to identify human gender, age, diseases, healthy conditions, nutrition status and contamination sites. Isotope ratio information, chemical speciation analysis and analyte preconcentration are also considered for hair. Finally, the potential of laser ablation ICP-MS (LA-ICP-MS) to provide spatial resolution and time-track the monitoring of elements in hair strands instead of conventional bulk analysis is spotlighted as a real future trend in the field. - Highlights: • Elemental analysis of hair is critically reviewed, with focus on ICP-MS employment. • Standards protocols of hair washing and sample decomposition are compiled. • The usefulness of elemental and/or isotopic analysis of hair is demonstrated. • The potential of LA-ICP-MS for elemental time tracking in hair is highlighted.

Generalized procedures for determining inspection sample sizes (related to quantitative measurements). Vol. 1: Detailed explanations

International Nuclear Information System (INIS)

Jaech, J.L.; Lemaire, R.J.

1986-11-01

Generalized procedures have been developed to determine sample sizes in connection with the planning of inspection activities. These procedures are based on different measurement methods. They are applied mainly to Bulk Handling Facilities and Physical Inventory Verifications. The present report attempts (i) to assign to appropriate statistical testers (viz. testers for gross, partial and small defects) the measurement methods to be used, and (ii) to associate the measurement uncertainties with the sample sizes required for verification. Working papers are also provided to assist in the application of the procedures. This volume contains the detailed explanations concerning the above mentioned procedures

Derivative activation analysis of phosphorus at ppb levels in water samples

International Nuclear Information System (INIS)

Arunachalam, J.; John, A.; Gangadharan, S.

1991-01-01

A neutron activation analysis procedure has been developed for the indirect determination of phosphorus as orthophosphate at ppb levels, via the formation of antimonyl phosphomolybdic acid. The complex is adsorbed on Sephadex G-25 resin and the antimony is estimated through NAA, allowing the determination of phosphorus. The procedure provides an easy method to adopt for the routine determination of phosphorus at ≥ 10 ng ml -1 levels with good precision, in water samples. (author) 6 refs.; 5 tabs

A radiochemical procedure for a low-level measurement of ''241 Am in environmental samples using a supported functional organo phosphorus extractant

International Nuclear Information System (INIS)

Gasco, C.; Anton, M.A.; Alvarez, A.; Navarro, N.; Salvador, S.

1994-01-01

The transuranides analysis in environmental samples is carried out by CIEMAT using standardized methods based on sequential separation with ionic-exchange resins. The americium fraction is purified through a two-layer ion exchange column and lately in an anion-exchange column in nitric acid methanol medium. The technique is time-consuming and the results are not completely satisfactory (low recovery and loss of alpha-resolution) for some samples. The chemical compound CMPO (octyl(phenyl).N,N-diisobutyl carbomoylmethyiphosphine oxide) dissolved in TPB (tributyl phosphate) and supported on an inert substrate has been tested directly for ''241 Am analysis by a large number of laboratories. A new method that combines both procedures has been developed. The details of the improved procedure are described in this paper. The advantages of its application to environmental samples (urine, faeces and sediments) are discussed. The utilization of standard, with americium certified concentrations confirms the reliability of our measurements

Develpoment of a procedure for the determination of chromium in samples of urine and serum by neutron activation analysis

International Nuclear Information System (INIS)

Buettner, I.; Hamm, V.; Knoechel, A.; Sen Gupta, R.

1993-01-01

Since the mid-fifties the possibility of a causal relationship between deficient chromium and insulin metabolism and the manifestation of certain varieties of diabetes mellitus has been presumed. The determination of the chromium status under pathophysiological conditions may be helpful for the study of this problem. For these purposes an analytical procedure as reference system was developed which allows the determination of chromium in biological matrices down to the concentration of 0.33 ng/ml. It is based on NAA and is used in the framework of a commonly used procedure based on GF-AAS. For its application blood and urine samples are freeze-dried and irradiated. After wet digestion with HNO 3 in a microwave combustion system chromium is separated for measurement from the matrix nuclides with the help of the ion-exchanger Cellex-P. THe individual steps of the procedure were evaluated by means of tracer experiments. (orig.)

Develpoment of a procedure for the determination of chromium in samples of urine and serum by neutron activation analysis

Energy Technology Data Exchange (ETDEWEB)

Buettner, I [Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry; Hamm, V [Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry; Knoechel, A [Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry; Sen Gupta, R [Hamburg Univ. (Germany). Inst. for Inorganic and Applied Chemistry

1993-06-01

Since the mid-fifties the possibility of a causal relationship between deficient chromium and insulin metabolism and the manifestation of certain varieties of diabetes mellitus has been presumed. The determination of the chromium status under pathophysiological conditions may be helpful for the study of this problem. For these purposes an analytical procedure as reference system was developed which allows the determination of chromium in biological matrices down to the concentration of 0.33 ng/ml. It is based on NAA and is used in the framework of a commonly used procedure based on GF-AAS. For its application blood and urine samples are freeze-dried and irradiated. After wet digestion with HNO[sub 3] in a microwave combustion system chromium is separated for measurement from the matrix nuclides with the help of the ion-exchanger Cellex-P. THe individual steps of the procedure were evaluated by means of tracer experiments. (orig.)

Procedure of trace element analysis in oyster tissues by using X-ray fluorescence

International Nuclear Information System (INIS)

Vo Thi Tuong Hanh; Dinh Thi Bich Lieu; Dinh Thien Lam and Nguyen Manh Hung

2004-01-01

The procedure of trace element analysis such as Ca, Mn, Fe, Zn, Cu, Pb in molluscs (oyster tissues) was established by using X-ray fluorescence techniques. The procedure was investigated from the sample collection, drying, ashing ratio to the analytical techniques by using Cd-109, detector Si (Li) and the peak processing MCAPLUS program was applied for this study. The procedure is based on direct comparison with certified concentrations of international standard reference SRM 1566b Oyster Tissue of National Institute of Standards and Technology, Department of commerce, United States of America for Ca, Mn, Fe, Zn, Cu and the Standard Addition Methods for Pb. The accuracy of the Standard Addition Methods was estimated by CRM281 Rye Grass of Community Bureau of Reference-BCR, European Commission. The results of 10 samples which were collected from several markets in Hanoi are shown. (author)

Analysis of polonium-210 in food samples

International Nuclear Information System (INIS)

Bueno, Luciana; Cunha, Ieda Irma Lamas

1999-01-01

This paper presents the polonium levels in food products. The analysis procedure consisted of acid leaching of the samples, solution evaporation, addition of hydrochloric acid, spontaneous deposition of polonium on a silver disk counting by alpha spectroscopy. The method was applied in reference materials and in foodstuffs, resulting in the following values: tea samples 0.4 to 1.7 Bq/unit; fish = 0.17 to 0.40 Bq/Kg, fruits = 0.048 to 0.067 Bq/kg, vegetables = 0.12 to 0.31 Bq/kg, cereal = 0.036 to 0.042 Bq/kg and legumes = 0.024 to 0.51 Bq/kg. The results are very important for public health due to the possible effects to the human organism by the ingestion of contaminated foodstuffs. (author)

Continuous quality control of the blood sampling procedure using a structured observation scheme

DEFF Research Database (Denmark)

Seemann, T. L.; Nybo, M.

2015-01-01

Background: An important preanalytical factor is the blood sampling procedure and its adherence to the guidelines, i.e. CLSI and ISO 15189, in order to ensure a consistent quality of the blood collection. Therefore, it is critically important to introduce quality control on this part of the process....... As suggested by the EFLM working group on the preanalytical phase we introduced continuous quality control of the blood sampling procedure using a structured observation scheme to monitor the quality of blood sampling performed on an everyday basis. Materials and methods: Based on our own routines the EFLM....... Conclusion: It is possible to establish a continuous quality control on blood sampling. It has been well accepted by the staff and we have already been able to identify critical areas in the sampling process. We find that continuous auditing increase focus on the quality of blood collection which ensures...

A procedure for partitioning bulk sediments into distinct grain-size fractions for geochemical analysis

Science.gov (United States)

Barbanti, A.; Bothner, Michael H.

1993-01-01

A method to separate sediments into discrete size fractions for geochemical analysis has been tested. The procedures were chosen to minimize the destruction or formation of aggregates and involved gentle sieving and settling of wet samples. Freeze-drying and sonication pretreatments, known to influence aggregates, were used for comparison. Freeze-drying was found to increase the silt/clay ratio by an average of 180 percent compared to analysis of a wet sample that had been wet sieved only. Sonication of a wet sample decreased the silt/clay ratio by 51 percent. The concentrations of metals and organic carbon in the separated fractions changed depending on the pretreatment procedures in a manner consistent with the hypothesis that aggregates consist of fine-grained organic- and metal-rich particles. The coarse silt fraction of a freeze-dried sample contained 20–44 percent higher concentrations of Zn, Cu, and organic carbon than the coarse silt fraction of the wet sample. Sonication resulted in concentrations of these analytes that were 18–33 percent lower in the coarse silt fraction than found in the wet sample. Sonication increased the concentration of lead in the clay fraction by an average of 40 percent compared to an unsonicated sample. Understanding the magnitude of change caused by different analysis protocols is an aid in designing future studies that seek to interpret the spatial distribution of contaminated sediments and their transport mechanisms.

A pre-concentration procedure using coprecipitation for determination of lead and iron in several samples using flame atomic absorption spectrometry

International Nuclear Information System (INIS)

Saracoglu, S.; Soylak, M.; Peker, D.S. Kacar; Elci, L.; Santos, W.N.L. dos; Lemos, V.A.; Ferreira, S.L.C.

2006-01-01

The present paper proposes a pre-concentration procedure for determination of lead and iron in several samples by flame atomic absorption spectrometry. In it, lead(II) and iron(III) ions are coprecipitated using the violuric acid-copper(II) system as collector. Afterwards, the precipitate is dissolved with 1 M HNO 3 solution and the metal ions are determined. The optimization step was performed using factorial design involving the variables: pH, violuric acid mass (VA) and copper concentration (Cu). Using the optimized experimental conditions, the proposed procedure allows the determination these metals with detection limits of 0.18 μg L -1 for iron and 0.16 μg L -1 for lead. The effects of foreign ions on the pre-concentration procedure were also evaluated and the results demonstrated that this method could be applied for determination of iron and lead in several real samples. The proposed method was successfully applied to the analysis of seawater, urine, mineral water, soil and physiological solution samples. The concentrations of lead and iron achieved in these samples agree well with others data reported in the literature

Standard operating procedure for combustion of 14C - samples with OX-500 biological material oxidizer

International Nuclear Information System (INIS)

Nashriyah Mat.

1995-01-01

This procedure is for the purpose of safe operation of OX-500 biological material oxidizer. For ease of operation, the operation flow chart (including testing the system and sample combustion) and end of day maintenance flow chart were simplified. The front view, diagrams and switches are duly copied from operating manual. Steps on sample preparation are also included for biotic and a biotic samples. This operating procedure is subjected to future reviews

Influence of rice sample preparation and milling procedures on milling quality appraisals

Science.gov (United States)

The objective of this research was to investigate the effect of sample preparation and milling procedure on milling quality appraisals of rough rice. Samples of freshly harvested medium-grain rice (M202) with different initial moisture contents (MCs) ranging from 20.2% to 25.1% (w.b.) were used for...

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.).

Nonradioactive Dangerous Waste Landfill sampling and analysis plan and data quality objectives process summary report

International Nuclear Information System (INIS)

Smith, R.C.

1997-08-01

This sampling and analysis plan defines the sampling and analytical activities and associated procedures that will be used to support the Nonradioactive Dangerous Waste Landfill soil-gas investigation. This SAP consists of three sections: this introduction, the field sampling plan, and the quality assurance project plan. The field sampling plan defines the sampling and analytical methodologies to be performed

Sample preparation for semivolatile organics analysis of Hanford single-shell tank waste with high nitrate/nitrite and water content

International Nuclear Information System (INIS)

Stromatt, R.W.; Hoppe, E.W.; Steele, M.J.

1993-11-01

This report describes research work carried out to solve sample preparation problems associated with applying gas chromatography with mass spectrometric detection (GC/MS) to the analysis of single shell tank (SST) samples from Hanford for semivolatile organic compounds. Poor performance was found when applying the procedures based on the U.S. Environmental Protection Agency (EPA), Contract Laboratory Program, Statement of Work (CLP SOW). Analysis work was carried out on simulated drainable liquid modeled after the SST core samples which had evidenced analysis problems. Some work was also conducted on true SST samples. It was found that the pH range was too broad in the original procedure. It was also found that by decreasing the amount of methanol used in the extraction process, problems associated with the formation of an azeotrope phase could be avoided. The authors suggest a new procedure, whose eventual application to a wide array of SST samples will lend itself to better quality control limits

Human Reliability Analysis For Computerized Procedures

International Nuclear Information System (INIS)

Boring, Ronald L.; Gertman, David I.; Le Blanc, Katya

2011-01-01

This paper provides a characterization of human reliability analysis (HRA) issues for computerized procedures in nuclear power plant control rooms. It is beyond the scope of this paper to propose a new HRA approach or to recommend specific methods or refinements to those methods. Rather, this paper provides a review of HRA as applied to traditional paper-based procedures, followed by a discussion of what specific factors should additionally be considered in HRAs for computerized procedures. Performance shaping factors and failure modes unique to computerized procedures are highlighted. Since there is no definitive guide to HRA for paper-based procedures, this paper also serves to clarify the existing guidance on paper-based procedures before delving into the unique aspects of computerized procedures.

Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 104

International Nuclear Information System (INIS)

Ross, G.A.

1998-01-01

A sample of solids was obtained from tank 104 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprenel tubing (Phthalate free). The sample obtained in a glass jar with Teflon 2 lid, was analyzed for PCBs as Aroclor mixtures. A soxhlet extraction procedure was used to extract the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). The extraction method closely follows SW-846 method 3540C and the analysis follows SW-846 method

Tank 241-AP-104 Grab Sampling and Analysis Plan

International Nuclear Information System (INIS)

TEMPLETON, A.M.

2000-01-01

This sampling and analysis plan (SAP) identifies characterization objectives pertaining to sample collection, laboratory analytical evaluation, and reporting requirements for samples obtained from tank 241-AP-104. The purpose of this sampling event is to obtain information about the characteristics of the contents of 241-AP-104 required to provide sample material to the Waste Treatment Contractor. Grab samples will be obtained from riser 001 to provide sufficient material for the chemical analyses and tests required to satisfy these data quality objectives and ICD-23. The 222-S Laboratory will receive samples; composite the samples; perform chemical analyses on composite samples; and provide samples to the Waste Treatment Contractor and the Process Chemistry Laboratory. The Process Chemistry Laboratory at the 222-S Laboratory Complex will perform process tests to evaluate the behavior of the 241-AP-104 waste undergoing the retrieval and treatment scenarios defined in the applicable DQOs. The Waste Treatment Contractor will perform process verification and waste form qualification tests. Requirements for analyses of samples originating in the L and H DQO process tests will be documented in the corresponding test plan (Person 2000) and are not within the scope of this SAP. This report provides the general methodology and procedures to be used in the preparation, retrieval, transport, analysis, and reporting of results from grab samples retrieved from tank 241-AP-104

A comparison of various procedures in photon activation analysis with the same irradiation setup

Energy Technology Data Exchange (ETDEWEB)

Sun, Z.J. [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S. Cass Ave., Argonne, IL 60439 (United States); Wells, D. [Physics Department, South Dakota School of Mines and Technology, 501 E. Saint Joseph St., Rapid City, SD 57701 (United States); Segebade, C. [Idaho Accelerator Center, Idaho State University, 921 S. 8th Ave., Pocatello, ID 83209 (United States); Quigley, K.; Chemerisov, S. [Chemical Sciences and Engineering Division, Argonne National Laboratory, 9700 S. Cass Ave., Argonne, IL 60439 (United States)

2014-11-15

A sample of known elemental concentrations was activated in the bremsstrahlung photon beam which was created by a pulsed electron LINAC. Several procedures of photon activation analysis, including those applied with/without reference material and with/without photon flux monitor, were conducted to make a comparison of their precision and accuracy in practice. Experimental results have indicated that: (1) relative procedures usually produce better outcome despite that the absolute measurement is straightforward and eliminate the assistance of reference materials; (2) among relative procedures, the method with internal flux monitor yields higher quality of the analytical results. In the article, the pros and cons of each procedure are discussed as well.

Automatic sample changer control software for automation of neutron activation analysis process in Malaysian Nuclear Agency

Science.gov (United States)

Yussup, N.; Ibrahim, M. M.; Rahman, N. A. A.; Mokhtar, M.; Salim, N. A. A.; Soh@Shaari, S. C.; Azman, A.; Lombigit, L.; Azman, A.; Omar, S. A.

2018-01-01

Most of the procedures in neutron activation analysis (NAA) process that has been established in Malaysian Nuclear Agency (Nuclear Malaysia) since 1980s were performed manually. These manual procedures carried out by the NAA laboratory personnel are time consuming and inefficient especially for sample counting and measurement process. The sample needs to be changed and the measurement software needs to be setup for every one hour counting time. Both of these procedures are performed manually for every sample. Hence, an automatic sample changer system (ASC) that consists of hardware and software is developed to automate sample counting process for up to 30 samples consecutively. This paper describes the ASC control software for NAA process which is designed and developed to control the ASC hardware and call GammaVision software for sample measurement. The software is developed by using National Instrument LabVIEW development package.

Sampling and analysis plan for Wayne Interim Storage Site (WISS), Wayne, New Jersey

International Nuclear Information System (INIS)

Brown, K.S.; Murray, M.E.; Rodriguez, R.E.

1998-10-01

This field sampling plan describes the methodology to perform an independent radiological verification survey and chemical characterization of a remediated area of the subpile at the Wayne Interim Storage Site, Wayne, New Jersey.Data obtained from collection and analysis of systematic and biased soil samples will be used to assess the status of remediation at the site and verify the final radiological status. The objective of this plan is to describe the methods for obtaining sufficient and valid measurements and analytical data to supplement and verify a radiological profile already established by the Project Remediation Management Contractor (PMC). The plan describes the procedure for obtaining sufficient and valid analytical data on soil samples following remediation of the first layer of the subpile. Samples will be taken from an area of the subpile measuring approximately 30 m by 80 m from which soil has been excavated to a depth of approximately 20 feet to confirm that the soil beneath the excavated area does not exceed radiological guidelines established for the site or chemical regulatory limits for inorganic metals. After the WISS has been fully remediated, the Department of Energy will release it for industrial/commercial land use in accordance with the Record of Decision. This plan provides supplemental instructions to guidelines and procedures established for sampling and analysis activities. Procedures will be referenced throughout this plan as applicable, and are available for review if necessary

Organically bound tritium analysis in environmental samples

Energy Technology Data Exchange (ETDEWEB)

Baglan, N. [CEA/DAM/DIF, Arpajon (France); Kim, S.B. [AECL, Chalk River Laboratories, Chalk River, ON (Canada); Cossonnet, C. [IRSN/PRP-ENV/STEME/LMRE, Orsay (France); Croudace, I.W.; Warwick, P.E. [GAU-Radioanalytical, University of Southampton, Southampton (United Kingdom); Fournier, M. [IRSN/DG/DMQ, Fontenay-aux-Roses (France); Galeriu, D. [IFIN-HH, Horia-Hulubei, Inst. Phys. and Nucl. Eng., Bucharest (Romania); Momoshima, N. [Kyushu University, Radioisotope Ctr., Fukuoka (Japan); Ansoborlo, E. [CEA/DEN/DRCP/CETAMA, Bagnols-sur-Ceze (France)

2015-03-15

Organically bound tritium (OBT) has become of increased interest within the last decade, with a focus on its behaviour and also its analysis, which are important to assess tritium distribution in the environment. In contrast, there are no certified reference materials and no standard analytical method through the international organization related to OBT. In order to resolve this issue, an OBT international working group was created in May 2012. Over 20 labs from around the world participated and submitted their results for the first intercomparison exercise results on potato (Sep 2013). The samples, specially-prepared potatoes, were provided in March 2013 to each participant. Technical information and results from this first exercise are discussed here for all the labs which have realised the five replicates necessary to allow a reliable statistical treatment. The results are encouraging as the increased number of participating labs did not degrade the observed dispersion of the results for a similar activity level. Therefore, the results do not seem to depend on the analytical procedure used. From this work an optimised procedure can start to be developed to deal with OBT analysis and will guide subsequent planned OBT trials by the international group.

Sample registration software for process automation in the Neutron Activation Analysis (NAA) Facility in Malaysia nuclear agency

Energy Technology Data Exchange (ETDEWEB)

Rahman, Nur Aira Abd, E-mail: nur-aira@nuclearmalaysia.gov.my; Yussup, Nolida; Ibrahim, Maslina Bt. Mohd; Mokhtar, Mukhlis B.; Soh Shaari, Syirrazie Bin Che; Azman, Azraf B. [Technical Support Division, Malaysian Nuclear Agency, 43000, Kajang, Selangor (Malaysia); Salim, Nazaratul Ashifa Bt. Abdullah [Division of Waste and Environmental Technology, Malaysian Nuclear Agency, 43000, Kajang, Selangor (Malaysia); Ismail, Nadiah Binti [Fakulti Kejuruteraan Elektrik, UiTM Pulau Pinang, 13500 Permatang Pauh, Pulau Pinang (Malaysia)

2015-04-29

Neutron Activation Analysis (NAA) had been established in Nuclear Malaysia since 1980s. Most of the procedures established were done manually including sample registration. The samples were recorded manually in a logbook and given ID number. Then all samples, standards, SRM and blank were recorded on the irradiation vial and several forms prior to irradiation. These manual procedures carried out by the NAA laboratory personnel were time consuming and not efficient. Sample registration software is developed as part of IAEA/CRP project on ‘Development of Process Automation in the Neutron Activation Analysis (NAA) Facility in Malaysia Nuclear Agency (RC17399)’. The objective of the project is to create a pc-based data entry software during sample preparation stage. This is an effective method to replace redundant manual data entries that needs to be completed by laboratory personnel. The software developed will automatically generate sample code for each sample in one batch, create printable registration forms for administration purpose, and store selected parameters that will be passed to sample analysis program. The software is developed by using National Instruments Labview 8.6.

Sample registration software for process automation in the Neutron Activation Analysis (NAA) Facility in Malaysia nuclear agency

Science.gov (United States)

Rahman, Nur Aira Abd; Yussup, Nolida; Salim, Nazaratul Ashifa Bt. Abdullah; Ibrahim, Maslina Bt. Mohd; Mokhtar, Mukhlis B.; Soh@Shaari, Syirrazie Bin Che; Azman, Azraf B.; Ismail, Nadiah Binti

2015-04-01

Neutron Activation Analysis (NAA) had been established in Nuclear Malaysia since 1980s. Most of the procedures established were done manually including sample registration. The samples were recorded manually in a logbook and given ID number. Then all samples, standards, SRM and blank were recorded on the irradiation vial and several forms prior to irradiation. These manual procedures carried out by the NAA laboratory personnel were time consuming and not efficient. Sample registration software is developed as part of IAEA/CRP project on `Development of Process Automation in the Neutron Activation Analysis (NAA) Facility in Malaysia Nuclear Agency (RC17399)'. The objective of the project is to create a pc-based data entry software during sample preparation stage. This is an effective method to replace redundant manual data entries that needs to be completed by laboratory personnel. The software developed will automatically generate sample code for each sample in one batch, create printable registration forms for administration purpose, and store selected parameters that will be passed to sample analysis program. The software is developed by using National Instruments Labview 8.6.

Integrated preservation and sample clean up procedures for studying water ingestion by recreational swimmers via urinary biomarker determination.

Science.gov (United States)

Cantú, Ricardo; Shoemaker, Jody A; Kelty, Catherine A; Wymer, Larry J; Behymer, Thomas D; Dufour, Alfred P; Magnuson, Matthew L

2017-08-22

The use of cyanuric acid as a biomarker for ingestion of swimming pool water may lead to quantitative knowledge of the volume of water ingested during swimming, contributing to a better understanding of disease resulting from ingestion of environmental contaminants. When swimming pool water containing chlorinated cyanurates is inadvertently ingested, cyanuric acid is excreted quantitatively within 24 h as a urinary biomarker of ingestion. Because the volume of water ingested can be quantitatively estimated by calculation from the concentration of cyanuric acid in 24 h urine samples, a procedure for preservation, cleanup, and analysis of cyanuric acid was developed to meet the logistical demands of large scale studies. From a practical stand point, urine collected from swimmers cannot be analyzed immediately, given requirements of sample collection, shipping, handling, etc. Thus, to maintain quality control to allow confidence in the results, it is necessary to preserve the samples in a manner that ensures as quantitative analysis as possible. The preservation and clean-up of cyanuric acid in urine is complicated because typical approaches often are incompatible with the keto-enol tautomerization of cyanuric acid, interfering with cyanuric acid sample preparation, chromatography, and detection. Therefore, this paper presents a novel integration of sample preservation, clean-up, chromatography, and detection to determine cyanuric acid in 24 h urine samples. Fortification of urine with cyanuric acid (0.3-3.0 mg/L) demonstrated accuracy (86-93% recovery) and high reproducibility (RSD urine suggested sufficient cyanuric acid stability for sample collection procedures, while longer holding times suggested instability of the unpreserved urine. Preserved urine exhibited a loss of around 0.5% after 22 days at refrigerated storage conditions of 4 °C. Published by Elsevier B.V.

105-DR Large Sodium Fire Facility decontamination, sampling, and analysis plan

International Nuclear Information System (INIS)

Knaus, Z.C.

1995-01-01

This is the decontamination, sampling, and analysis plan for the closure activities at the 105-DR Large Sodium Fire Facility at Hanford Reservation. This document supports the 105-DR Large Sodium Fire Facility Closure Plan, DOE-RL-90-25. The 105-DR LSFF, which operated from about 1972 to 1986, was a research laboratory that occupied the former ventilation supply room on the southwest side of the 105-DR Reactor facility in the 100-D Area of the Hanford Site. The LSFF was established to investigate fire fighting and safety associated with alkali metal fires in the liquid metal fast breeder reactor facilities. The decontamination, sampling, and analysis plan identifies the decontamination procedures, sampling locations, any special handling requirements, quality control samples, required chemical analysis, and data validation needed to meet the requirements of the 105-DR Large Sodium Fire Facility Closure Plan in compliance with the Resource Conservation and Recovery Act

Shrunken head (tsantsa): a complete forensic analysis procedure.

Science.gov (United States)

Charlier, P; Huynh-Charlier, I; Brun, L; Hervé, C; de la Grandmaison, G Lorin

2012-10-10

Based on the analysis of shrunken heads referred to our forensic laboratory for anthropological expertise, and data from both anthropological and medical literature, we propose a complete forensic procedure for the analysis of such pieces. A list of 14 original morphological criteria has been developed, based on the global aspect, color, physical deformation, anatomical details, and eventual associated material (wood, vegetal fibers, sand, charcoals, etc.). Such criteria have been tested on a control sample of 20 tsantsa (i.e. shrunken heads from the Jivaro or Shuar tribes of South America). Further complementary analyses are described such as CT-scan and microscopic examination. Such expertise is more and more asked to forensic anthropologists and practitioners in a context of global repatriation of human artifacts to native communities. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

Sequential extraction procedure for determination of uranium, thorium, radium, lead and polonium radionuclides by alpha spectrometry in environmental samples

Science.gov (United States)

Oliveira, J. M.; Carvalho, F. P.

2006-01-01

A sequential extraction technique was developed and tested for common naturally-occurring radionuclides. This technique allows the extraction and purification of uranium, thorium, radium, lead, and polonium radionuclides from the same sample. Environmental materials such as water, soil, and biological samples can be analyzed for those radionuclides without matrix interferences in the quality of radioelement purification and in the radiochemical yield. The use of isotopic tracers (232U, 229Th, 224Ra, 209Po, and stable lead carrier) added to the sample in the beginning of the chemical procedure, enables an accurate control of the radiochemical yield for each radioelement. The ion extraction procedure, applied after either complete dissolution of the solid sample with mineral acids or co-precipitation of dissolved radionuclide with MnO2 for aqueous samples, includes the use of commercially available pre-packed columns from Eichrom® and ion exchange columns packed with Bio-Rad resins, in altogether three chromatography columns. All radioactive elements but one are purified and electroplated on stainless steel discs. Polonium is spontaneously plated on a silver disc. The discs are measured using high resolution silicon surface barrier detectors. 210Pb, a beta emitter, can be measured either through the beta emission of 210Bi, or stored for a few months and determined by alpha spectrometry through the in-growth of 210Po. This sequential extraction chromatography technique was tested and validated with the analysis of certified reference materials from the IAEA. Reproducibility was tested through repeated analysis of the same homogeneous material (water sample).

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR COLLECTION, STORAGE, AND SHIPMENT OF URINE SAMPLES FOR METALS AND PESTICIDES ANALYSIS (UA-F-20.1)

Science.gov (United States)

The purpose of this SOP is to guide the collection, storage, and shipment of urine samples collected. This SOP provides a brief description of sample, collection, preservation, storage, shipping, and custody procedures. This procedure was followed to ensure consistent data retri...

Different Analytical Procedures for the Study of Organic Residues in Archeological Ceramic Samples with the Use of Gas Chromatography-mass Spectrometry.

Science.gov (United States)

Kałużna-Czaplińska, Joanna; Rosiak, Angelina; Kwapińska, Marzena; Kwapiński, Witold

2016-01-01

The analysis of the composition of organic residues present in pottery is an important source of information for historians and archeologists. Chemical characterization of the materials provides information on diets, habits, technologies, and original use of the vessels. This review presents the problem of analytical studies of archeological materials with a special emphasis on organic residues. Current methods used in the determination of different organic compounds in archeological ceramics are presented. Particular attention is paid to the procedures of analysis of archeological ceramic samples used before gas chromatography-mass spectrometry. Advantages and disadvantages of different extraction methods and application of proper quality assurance/quality control procedures are discussed.

[Sample preparation methods for chromatographic analysis of organic components in atmospheric particulate matter].

Science.gov (United States)

Hao, Liang; Wu, Dapeng; Guan, Yafeng

2014-09-01

The determination of organic composition in atmospheric particulate matter (PM) is of great importance in understanding how PM affects human health, environment, climate, and ecosystem. Organic components are also the scientific basis for emission source tracking, PM regulation and risk management. Therefore, the molecular characterization of the organic fraction of PM has become one of the priority research issues in the field of environmental analysis. Due to the extreme complexity of PM samples, chromatographic methods have been the chief selection. The common procedure for the analysis of organic components in PM includes several steps: sample collection on the fiber filters, sample preparation (transform the sample into a form suitable for chromatographic analysis), analysis by chromatographic methods. Among these steps, the sample preparation methods will largely determine the throughput and the data quality. Solvent extraction methods followed by sample pretreatment (e. g. pre-separation, derivatization, pre-concentration) have long been used for PM sample analysis, and thermal desorption methods have also mainly focused on the non-polar organic component analysis in PM. In this paper, the sample preparation methods prior to chromatographic analysis of organic components in PM are reviewed comprehensively, and the corresponding merits and limitations of each method are also briefly discussed.

Soil Gas Sampling

Science.gov (United States)

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

Fast derivatization of fatty acids in different meat samples for gas chromatography analysis.

Science.gov (United States)

Figueiredo, Ingrid Lima; Claus, Thiago; Oliveira Santos Júnior, Oscar; Almeida, Vitor Cinque; Magon, Thiago; Visentainer, Jesuí Vergilio

2016-07-22

In order to analyze the composition of fatty acids employing gas chromatography as the separation method, a derivatization of lipids using esterification and transesterification reactions is needed. The methodologies currently available are time consuming and use large amounts of sample and reagents. Thus, this work proposes a new procedure to carry out the derivatization of fatty acids without the need for prior extraction of lipids. The use of small amounts of sample (100mg) allows the analysis to be performed in specific parts of animals, in most cases without having them slaughtered. Another benefit is the use of small amounts of reagents (only 2mL of NaOH/Methanol and H2SO4/Methanol). The use of an experimental design procedure (Design Expert software) allows the optimization of the alkaline and acid reaction times. The procedure was validated for five minutes in both steps. The method was validated for bovine fat, beef, chicken, pork, fish and shrimp meats. The results for the merit figures of accuracy (from 101.07% to 109.18%), precision (RSDintra-day (from 0.65 to 3.93%), RSDinter-day (from 1.57 to 5.22%)), linearity (R(2)=0.9864) and robustness confirmed that the new method is satisfactory within the linear range of 2-30% of lipids in the sample. Besides the benefits of minimizing the amount of samples and reagents, the procedure enables gas chromatography sample preparation in a very short time compared with traditional procedures. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

The Alaska Commercial Fisheries Water Quality Sampling Methods and Procedures Manual

Energy Technology Data Exchange (ETDEWEB)

Folley, G.; Pearson, L.; Crosby, C. [Alaska Dept. of Environmental Conservation, Soldotna, AK (United States); DeCola, E.; Robertson, T. [Nuka Research and Planning Group, Seldovia, AK (United States)

2006-07-01

A comprehensive water quality sampling program was conducted in response to the oil spill that occurred when the M/V Selendang Ayu ship ran aground near a major fishing port at Unalaska Island, Alaska in December 2004. In particular, the sampling program focused on the threat of spilled oil to the local commercial fisheries resources. Spill scientists were unable to confidently model the movement of oil away from the wreck because of limited oceanographic data. In order to determine which fish species were at risk of oil contamination, a real-time assessment of how and where the oil was moving was needed, because the wreck became a continual source of oil release for several weeks after the initial grounding. The newly developed methods and procedures used to detect whole oil during the sampling program will be presented in the Alaska Commercial Fisheries Water Quality Sampling Methods and Procedures Manual which is currently under development. The purpose of the manual is to provide instructions to spill managers while they try to determine where spilled oil has or has not been encountered. The manual will include a meaningful data set that can be analyzed in real time to assess oil movement and concentration. Sections on oil properties and processes will be included along with scientific water quality sampling methods for whole and dissolved phase oil to assess potential contamination of commercial fishery resources and gear in Alaska waters during an oil spill. The manual will present a general discussion of factors that should be considered when designing a sampling program after a spill. In order to implement Alaska's improved seafood safety measures, the spatial scope of spilled oil must be known. A water quality sampling program can provide state and federal fishery managers and food safety inspectors with important information as they identify at-risk fisheries. 11 refs., 7 figs.

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).

Development of Procedures for the Analysis of Components of Dumped Chemical Weapons and Their Principal Transformation Products in Sea Water

International Nuclear Information System (INIS)

Saveleva, E. I.; Koryagina, N. L.; Radilov, A. S.; Khlebnikova, N. S.; Khrustaleva, V. S.

2007-01-01

A package of chemical analytical procedures was developed for the detection of products indicative of the presence of damped chemical weapons in the Baltic Sea. The principal requirements imposed upon the procedures were the following: high sensitivity, reliable identification of target compounds, wide range of components covered by survey analysis, and lack of interferences from sea salts. Thiodiglycol, a product of hydrolysis of sulfur mustard reportedly always detected in the sites of damping chemical weapons in the Baltic Sea, was considered the principal marker. We developed a high-sensitivity procedure for the determination of thiodiglycol in sea water, involving evaporation of samples to dryness in a vacuum concentrator, followed by tert-butyldimethylsilylation of the residue and GCMS analysis in the SIM mode with meta-fluorobenzoic acid as internal reference. The detection limit of thiodiglycol was 0.001 mg/l, and the procedure throughput was up to 30 samples per day. The same procedure, but with BSTFA as derivatizing agent instead of MTBSTFA, was used for preparing samples for survey analysis of nonvolatile components. In this case, full mass spectra were measured in the GCMS analysis. The use of BSTFA was motivated by the fact that trimethylsilyl derivatives are much wider represented in electronic mass spectral databases. The identification of sulfur mustard, volatile transformation products of sulfur mustard and lewisite, as well as chloroacetophenone in sea water was performed by means of GCMS in combination with SPME. The survey GC-MS analysis was focused on the identification of volatile and nonvolatile toxic chemicals whose mass spectra are included in the OPCW database (3219 toxic chemicals, precursors, and transformation products) with the use of AMDIS software (version 2.62). Using 2 GC-MS instruments, we could perform the survey analysis for volatile and nonvolatile components of up to 20 samples per day. Thus, the package of three procedures

Application of CWC analytical procedures for safeguards; Analysis of phosphorus-containing organic chemical signatures from environmental samples; Final report on task FIN A844 on the Finnish support programme to IAEA safeguards

Energy Technology Data Exchange (ETDEWEB)

Rautio, M; Bjoerk, H; Haekkinen, V; Kostiainen, O; Kuitunen, M L; Lehtonen, P; Mesilaakso, M; Soederstroem, M [Finnish Inst. for Verification of the Chemical Weapons Convention, Helsinki (Finland)

1995-03-01

Solvent extraction can be used for the recovery of U and Pu from irradiated fuel. The most potential organic chemical signatures are extractants and solvents used in reprocessing plants. The PUREX process is widely used in reprocessing. It uses tri-n-butyl phosphate (TBP) as extractant in an organic solvent for U and Pu from irradiated fuel and U from its ores. TBP is a strong extractant for tetra and hexavalent actinides from nitric acid media. Stable complexes are formed between actinide nitrate and TBP which are soluble in the organic phase. Sample containing TBP and some radiolysis products can indicate that TBP is used for reprocessing nuclear fuel. The TBP will decompose in the PUREX process to mono-and dibutyl phosphates (MBP and DBP). TBP, DBP and MBP have been analysed from air, water, soil, and sediment samples according to slightly modified procedures presented in Recommended Operating Procedures for Sampling and Analysis in the Verification of Chemical Disarmament. The limits of detection for the phosphates have been determined for air, water and soil samples. (orig.) (12 refs., 8 figs., 4 tabs.).

Microbial ecology laboratory procedures manual NASA/MSFC

Science.gov (United States)

Huff, Timothy L.

1990-01-01

An essential part of the efficient operation of any microbiology laboratory involved in sample analysis is a standard procedures manual. The purpose of this manual is to provide concise and well defined instructions on routine technical procedures involving sample analysis and methods for monitoring and maintaining quality control within the laboratory. Of equal importance is the safe operation of the laboratory. This manual outlines detailed procedures to be followed in the microbial ecology laboratory to assure safety, analytical control, and validity of results.

The effect of sample grinding procedures after processing on gas production profiles and end-product formation in expander processed barley and peas

NARCIS (Netherlands)

Azarfar, A.; Poel, van der A.F.B.; Tamminga, S.

2007-01-01

Grinding is a technological process widely applied in the feed manufacturing industry and is a prerequisite for obtaining representative samples for laboratory procedures (e.g. gas production analysis). When feeds are subjected to technological processes other than grinding (e.g. expander

Preliminary results of scoop samples analysis from reactor pressure vessels of Bohunice V-1 NPP

International Nuclear Information System (INIS)

Kupca, L.

1997-01-01

In the paper are presented the main goals and results from the scoop specimen analysis performed on the both RPVs WWER-440/230 in Jaslovske Bohunice V-1 NPPs. Main tasks of this complex activity were: model experiments for analysis procedures optimisation; chemical analysis; hardness measurements on the RPV and bulk samples; microstructure analysis; scanning electron microscope and microprobe analysis; gamma spectrometry; brittle fracture temperature evaluation; trends of brittle fracture temperature growth after annealing procedure. In conclusions and recommendations are discussed the planned activities in the field of both RPVs integrity evaluation for the future operation of the NPP Jaslovske Bohunice V-1. (author)

Procedures for the collection and preservation of groundwater and surface water samples and for the installation of monitoring wells

International Nuclear Information System (INIS)

Korte, N.; Kearl, P.

1984-01-01

Proper sampling procedures are essential for a successful water-quality monitoring program. It must be emphasized, however, that it is impossible to maintain absolutely in-situ conditions when collecting and preserving a water sample, whether from a flowing stream or an aquifer. Consequently, the most that can reasonably be expected is to collect a best possible sample with minimal disturbance. This document describes procedures for installing monitoring wells and for collecting samples of surface water and groundwater. The discussion of monitoring wells includes mention of multilevel sampling and a general overview of vadose-zone monitoring. Guidelines for well installation are presented in detail. The discussion of water-sample collection contains evaluations of sampling pumps, filtration equipment, and sample containers. Sample-preservation techniques, as published by several government and private sources, are reviewed. Finally, step-by-step procedures for collection of water samples are provided; these procedures address such considerations as necessary equipment, field operations, and written documentation. Separate procedures are also included for the collection of samples for determination of sulfide and for reactive aluminum. The report concludes with a brief discussion of adverse sampling, conditions that may significantly affect the quality of the data. Appendix A presents a rationale for the development and use of statistical considerations in water sampling to ensure a more complete water quality monitoring program. 51 references, 9 figures, 4 tables

A recommended procedure for establishing the source level relationships between heroin case samples of unknown origins

Directory of Open Access Journals (Sweden)

Kar-Weng Chan

2014-06-01

Full Text Available A recent concern of how to reliably establish the source level relationships of heroin case samples is addressed in this paper. Twenty-two trafficking heroin case samples of unknown origins seized from two major regions (Kuala Lumpur and Penang in Malaysia were studied. A procedure containing six major steps was followed to analyze and classify these samples. Subsequently, with the aid of statistical control samples, reliability of the clustering result was assessed. The final outcome reveals that the samples seized from the two regions in 2013 had highly likely originated from two different sources. Hence, the six-step procedure is sufficient for any chemist who attempts to assess the relative source level relationships of heroin samples.

An Alternative View of Some FIA Sample Design and Analysis Issues

Science.gov (United States)

Paul C. Van Deusen

2005-01-01

Sample design and analysis decisions are the result of compromises and inputs from many sources. The end result would likely change if different individuals or groups were involved in the planning process. Discussed here are some alternatives to the procedures that are currently being used for the annual inventory. The purpose is to indicate that alternatives exist and...

Studies and developments for the analysis of products of nuclear reprocessing plants with the help of the X-ray fluorescence analysis on totally reflecting sample holders (TXRF)

International Nuclear Information System (INIS)

Diercks, H.; Eggers, I.; Gibau, F.; Haarich, M.; Hastenteufel, S.; Haurand, M.; Knoechel, A.; Salow, H.

1990-01-01

Studies with inactive and active simulates of products of nuclear reprocessing plants show the suitability of the X-Ray Fluorescence Analysis on Totally Reflecting Sample Holders (TXRF), to detect the available elements simultaneously by direct measurements of specially prepared thin samples. High dilution enables in the most cases, to avoid working in hot cells and to carry out the analysis in glove boxes. The analysis of uranium products and great amounts of matrix elements containing solutions like LAW and MAW demands the separation of the matrix elements before TXRF measurement. Procedures for this task have been developed. The potential of the new analytical procedure was demonstrated by the analysis of two samples of highly diluted high active wastes. (orig.) With 65 refs., 20 tabs., 81 figs [de

An automated sensitivity analysis procedure for the performance assessment of nuclear waste isolation systems

International Nuclear Information System (INIS)

Pin, F.G.; Worley, B.A.; Oblow, E.M.; Wright, R.Q.; Harper, W.V.

1986-01-01

To support an effort in making large-scale sensitivity analyses feasible, cost efficient and quantitatively complete, the authors have developed an automated procedure making use of computer calculus. The procedure, called GRESS (GRadient Enhanced Software System), is embodied in a precompiler that can process Fortran computer codes and add derivative-taking capabilities to the normal calculation scheme. In this paper, the automated GRESS procedure is described and applied to the code UCB-NE-10.2, which simulates the migration through a sorption medium of the radionuclide members of a decay chain. The sensitivity calculations for a sample problem are verified using comparison with analytical and perturbation analysis results. Conclusions are drawn relative to the applicability of GRESS for more general large-scale sensitivity studies, and the role of such techniques in an overall sensitivity and uncertainty analysis program is discussed

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

International Nuclear Information System (INIS)

Godoy, J.M.; Schuettelkopf, H.

1980-07-01

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

Tank 241-C-111 vapor sampling and analysis tank characterization report. Revision 1

International Nuclear Information System (INIS)

Huckaby, J.L.

1995-01-01

This report presents the details of the Hanford waste tank characterization study for tank 241-C-111. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to tank farm workers due to fugitive emissions from the tank

Tank 241-BY-110 vapor sampling and analysis tank characterization report. Revision 1

International Nuclear Information System (INIS)

Huckaby, J.L.

1995-01-01

This report presents the details of the Hanford waste tank characterization study for tank 241-BY-110. The drivers and objectives of the headspace vapor sampling and analysis were in accordance with procedures that were presented in other reports. The vapor and headspace gas samples were collected and analyzed to determine the potential risks to the tank farm workers due to fugitive emissions from the tank

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.

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.

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)

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)

Sampling procedures and tables

International Nuclear Information System (INIS)

Franzkowski, R.

1980-01-01

Characteristics, defects, defectives - Sampling by attributes and by variables - Sample versus population - Frequency distributions for the number of defectives or the number of defects in the sample - Operating characteristic curve, producer's risk, consumer's risk - Acceptable quality level AQL - Average outgoing quality AOQ - Standard ISQ 2859 - Fundamentals of sampling by variables for fraction defective. (RW)

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

International Nuclear Information System (INIS)

2009-01-01

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

Multicriteria decision analysis in ranking of analytical procedures for aldrin determination in water.

Science.gov (United States)

Tobiszewski, Marek; Orłowski, Aleksander

2015-03-27

The study presents the possibility of multi-criteria decision analysis (MCDA) application when choosing analytical procedures with low environmental impact. A type of MCDA, Preference Ranking Organization Method for Enrichment Evaluations (PROMETHEE), was chosen as versatile tool that meets all the analytical chemists--decision makers requirements. Twenty five analytical procedures for aldrin determination in water samples (as an example) were selected as input alternatives to MCDA analysis. Nine different criteria describing the alternatives were chosen from different groups--metrological, economical and the most importantly--environmental impact. The weights for each criterion were obtained from questionnaires that were sent to experts, giving three different scenarios for MCDA results. The results of analysis show that PROMETHEE is very promising tool to choose the analytical procedure with respect to its greenness. The rankings for all three scenarios placed solid phase microextraction and liquid phase microextraction--based procedures high, while liquid-liquid extraction, solid phase extraction and stir bar sorptive extraction--based procedures were placed low in the ranking. The results show that although some of the experts do not intentionally choose green analytical chemistry procedures, their MCDA choice is in accordance with green chemistry principles. The PROMETHEE ranking results were compared with more widely accepted green analytical chemistry tools--NEMI and Eco-Scale. As PROMETHEE involved more different factors than NEMI, the assessment results were only weakly correlated. Oppositely, the results of Eco-Scale assessment were well-correlated as both methodologies involved similar criteria of assessment. Copyright © 2015 Elsevier B.V. All rights reserved.

Accident Sequence Evaluation Program: Human reliability analysis procedure

International Nuclear Information System (INIS)

Swain, A.D.

1987-02-01

This document presents a shortened version of the procedure, models, and data for human reliability analysis (HRA) which are presented in the Handbook of Human Reliability Analysis With emphasis on Nuclear Power Plant Applications (NUREG/CR-1278, August 1983). This shortened version was prepared and tried out as part of the Accident Sequence Evaluation Program (ASEP) funded by the US Nuclear Regulatory Commission and managed by Sandia National Laboratories. The intent of this new HRA procedure, called the ''ASEP HRA Procedure,'' is to enable systems analysts, with minimal support from experts in human reliability analysis, to make estimates of human error probabilities and other human performance characteristics which are sufficiently accurate for many probabilistic risk assessments. The ASEP HRA Procedure consists of a Pre-Accident Screening HRA, a Pre-Accident Nominal HRA, a Post-Accident Screening HRA, and a Post-Accident Nominal HRA. The procedure in this document includes changes made after tryout and evaluation of the procedure in four nuclear power plants by four different systems analysts and related personnel, including human reliability specialists. The changes consist of some additional explanatory material (including examples), and more detailed definitions of some of the terms. 42 refs

Solid-phase extraction procedures in systematic toxicological analysis

NARCIS (Netherlands)

Franke, J.P.; de Zeeuw, R.A

1998-01-01

In systematic toxicological analysis (STA) the substance(s) present is (are) not known at the start of the analysis. in such an undirected search the extraction procedure cannot be directed to a given substance but must be a general procedure where a compromise must be reached in that the substances

A column exchange chromatographic procedure for the automated purification of analytical samples in nuclear spent fuel reprocessing and plutonium fuel fabrication

International Nuclear Information System (INIS)

Zahradnik, P.; Swietly, H.; Doubek, N.; Bagliano, G.

1992-11-01

A Column Exchange Chromatographic procedure using Tri-n-Octyl-Phosphine-Oxide (TOPO) as stationary phase, is in routine use at SAL since 1984 on nuclear spent fuel reprocessing and on Pu product samples, prior to alpha and mass spectrometric analysis. This standard procedure was further on modified in view of its automation in a glove box; the resulting new procedure is described in this paper. Laboratory Robot Compatible (LRC) disposable columns were selected because their dimensions are particularly favorable and reproducible. A less corrosive HNO 3 -HI mixture substituted the former HC1-HI plutonium eluant. The inorganic support of the stationary phase used to test the above mentioned changes was unexpectedly withdrawn from the market so that another support had to be selected and the procedure reoptimized accordingly. The resulting procedure was tested with the robot and validated against the manual procedure taken as reference: the comparison showed that the modified procedure meets the analytical requirements and has the same performance than the original procedure. (author). Refs, figs and tabs

Application of Fourier analysis to the study of roughness profiles of eroded samples

International Nuclear Information System (INIS)

Bethencourt, M.; Botana, F.J.; Calvino, J.J.; Marcos, M.; Rodriguez-Chacon, M.A.

1998-01-01

Fourier transforms are applied to analyse surface roughness profiles recorded on samples coming from erosion-corrosion essays. The information retrieved using this method clearly complements that revealed by the more classical roughness amplitude parameters. The analysis procedure here proposed can be applied not only to characterise the surface of corroded samples but, in general, to evaluate the quality of any surface after application of finishing treatments. (Author) 7 refs

Automated Sampling and Extraction of Krypton from Small Air Samples for Kr-85 Measurement Using Atom Trap Trace Analysis

International Nuclear Information System (INIS)

Hebel, S.; Hands, J.; Goering, F.; Kirchner, G.; Purtschert, R.

2015-01-01

Atom-Trap-Trace-Analysis (ATTA) provides the capability of measuring the Krypton-85 concentration in microlitre amounts of krypton extracted from air samples of about 1 litre. This sample size is sufficiently small to allow for a range of applications, including on-site spot sampling and continuous sampling over periods of several hours. All samples can be easily handled and transported to an off-site laboratory for ATTA measurement, or stored and analyzed on demand. Bayesian sampling methodologies can be applied by blending samples for bulk measurement and performing in-depth analysis as required. Prerequisite for measurement is the extraction of a pure krypton fraction from the sample. This paper introduces an extraction unit able to isolate the krypton in small ambient air samples with high speed, high efficiency and in a fully automated manner using a combination of cryogenic distillation and gas chromatography. Air samples are collected using an automated smart sampler developed in-house to achieve a constant sampling rate over adjustable time periods ranging from 5 minutes to 3 hours per sample. The smart sampler can be deployed in the field and operate on battery for one week to take up to 60 air samples. This high flexibility of sampling and the fast, robust sample preparation are a valuable tool for research and the application of Kr-85 measurements to novel Safeguards procedures. (author)

Research And Establishment Of The Analytical Procedure For/Of Sr-90 In Milk Samples

International Nuclear Information System (INIS)

Tran Thi Tuyet Mai; Duong Duc Thang; Nguyen Thi Linh; Bui Thi Anh Duong

2014-01-01

Sr-90 is an indicator for the transfer radionuclides from environment to human. This work was setup to build a procedure for Sr-90 determination in main popular foodstuff and focus to fresh milk. The deal of this work was establish procedure for Sr-90 , assessment for chemical yield and test sample of Vietnam fresh milk, also in this work, the QA, QC for the procedure was carried out using standard sample of IAEA. The work has been completed for the procedure of determination Sr-90 in milk. The chemical yield of recovery for Y-90 and Sr-90 were at 46.76 % ±1.25% and 0.78 ± 0.086, respectively. The QA & QC program was carried out using reference material IAEA-373. The result parse is appropriate equally and well agreement with the certificate value. Three reference samples were analyses with 15 measurements. The results of Sr-90 concentration after processing statistics given a value at 3.69 Bq/kg with uncertainty of 0.23 Bq/kg. The certificate of IAEA-154 for Sr-90 (half live 28.8 year) is the 6.9 Bq/kg, with the range 95% Confidence Interval as (6.0 -8.0 ) Bq/kg at 31st August 1987. After adjusting decay, the radioactivity at this time is 3.67 Bq/kg. It means that such the result of this work was perfect matching the value of stock index IAEA. Five Vietnam fresh milk samples were analyzed for Sr-90, the specific radioactivity of Sr-90 in milk were in a range from 0.032 to 0.041 Bq/l. (author)

Supplement to the UMTRA Project water sampling and analysis plan, Maybell, Colorado

International Nuclear Information System (INIS)

1995-09-01

This water sampling and analysis plan (WSAP) supplement supports the regulatory and technical basis for water sampling at the Maybell, Colorado, Uranium Mill Tailings Remedial Action (UMTRA) Project site, as defined in the 1994 WSAP document for Maybell (DOE, 1994a). Further, this supplement serves to confirm our present understanding of the site relative to the hydrogeology and contaminant distribution as well as our intention to continue to use the sampling strategy as presented in the 1994 WSAP document for Maybell. Ground water and surface water monitoring activities are derived from the US Environmental Protection Agency regulations in 40 CFR Part 192 (1994) and 60 CFR 2854 (1 995). Sampling procedures are guided by the UMTRA Project standard operating procedures (JEG, n.d.), the Technical Approach Document (DOE, 1989), and the most effective technical approach for the site. Additional site-specific documents relevant to the Maybell site are the Maybell Baseline Risk Assessment (currently in progress), the Maybell Remedial Action Plan (RAP) (DOE, 1994b), and the Maybell Environmental Assessment (DOE, 1995)

Supplement to the UMTRA Project water sampling and analysis plan, Monument Valley, Arizona

International Nuclear Information System (INIS)

1995-09-01

This water sampling and analysis plan (WSAP) supplement supports the regulatory and technical basis for water sampling at the Riverton, Wyoming, Uranium Mill Tailings Remedial Action (UMTRA) Project site, as defined in the 1994 WSAP document for Riverton (DOE, 1994). Further, the supplement serves to confirm the Project's present understanding of the site relative to the hydrogeology and contaminant distribution as well as the intent to continue to use the sampling strategy as presented in the 1994 WSAP document for Riverton. Ground water and surface water monitoring activities are derived from the US Environmental Protection Agency regulations in 40 CFR Part 192 and 60 FR 2854. Sampling procedures are guided by the UMTRA Project standard operating procedures (JEG, n.d.), the Technical Approach Document (DOE, 1989), and the most effective technical approach for the site. Additional site-specific documents relevant to the Riverton site are the Riverton Baseline Risk Assessment (BLRA) (DOE, 1995a) and the Riverton Site Observational Work Plan (SOWP) (DOE, 1995b)

Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites

International Nuclear Information System (INIS)

2012-01-01

This plan incorporates U.S. Department of Energy (DOE) Office of Legacy Management (LM) standard operating procedures (SOPs) into environmental monitoring activities and will be implemented at all sites managed by LM. This document provides detailed procedures for the field sampling teams so that samples are collected in a consistent and technically defensible manner. Site-specific plans (e.g., long-term surveillance and maintenance plans, environmental monitoring plans) document background information and establish the basis for sampling and monitoring activities. Information will be included in site-specific tabbed sections to this plan, which identify sample locations, sample frequencies, types of samples, field measurements, and associated analytes for each site. Additionally, within each tabbed section, program directives will be included, when developed, to establish additional site-specific requirements to modify or clarify requirements in this plan as they apply to the corresponding site. A flowchart detailing project tasks required to accomplish routine sampling is displayed in Figure 1. LM environmental procedures are contained in the Environmental Procedures Catalog (LMS/PRO/S04325), which incorporates American Society for Testing and Materials (ASTM), DOE, and U.S. Environmental Protection Agency (EPA) guidance. Specific procedures used for groundwater and surface water monitoring are included in Appendix A. If other environmental media are monitored, SOPs used for air, soil/sediment, and biota monitoring can be found in the site-specific tabbed sections in Appendix D or in site-specific documents. The procedures in the Environmental Procedures Catalog are intended as general guidance and require additional detail from planning documents in order to be complete; the following sections fulfill that function and specify additional procedural requirements to form SOPs. Routine revision of this Sampling and Analysis Plan will be conducted annually at the

Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites

Energy Technology Data Exchange (ETDEWEB)

None

2012-10-24

This plan incorporates U.S. Department of Energy (DOE) Office of Legacy Management (LM) standard operating procedures (SOPs) into environmental monitoring activities and will be implemented at all sites managed by LM. This document provides detailed procedures for the field sampling teams so that samples are collected in a consistent and technically defensible manner. Site-specific plans (e.g., long-term surveillance and maintenance plans, environmental monitoring plans) document background information and establish the basis for sampling and monitoring activities. Information will be included in site-specific tabbed sections to this plan, which identify sample locations, sample frequencies, types of samples, field measurements, and associated analytes for each site. Additionally, within each tabbed section, program directives will be included, when developed, to establish additional site-specific requirements to modify or clarify requirements in this plan as they apply to the corresponding site. A flowchart detailing project tasks required to accomplish routine sampling is displayed in Figure 1. LM environmental procedures are contained in the Environmental Procedures Catalog (LMS/PRO/S04325), which incorporates American Society for Testing and Materials (ASTM), DOE, and U.S. Environmental Protection Agency (EPA) guidance. Specific procedures used for groundwater and surface water monitoring are included in Appendix A. If other environmental media are monitored, SOPs used for air, soil/sediment, and biota monitoring can be found in the site-specific tabbed sections in Appendix D or in site-specific documents. The procedures in the Environmental Procedures Catalog are intended as general guidance and require additional detail from planning documents in order to be complete; the following sections fulfill that function and specify additional procedural requirements to form SOPs. Routine revision of this Sampling and Analysis Plan will be conducted annually at the

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

Science.gov (United States)

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

2016-08-22

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

Sampling procedure in a willow plantation for estimation of moisture content

DEFF Research Database (Denmark)

Nielsen, Henrik Kofoed; Lærke, Poul Erik; Liu, Na

2015-01-01

Heating value and fuel quality of wood is closely connected to moisture content. In this work the variation of moisture content (MC) of short rotation coppice (SRC) willow shoots is described for five clones during one harvesting season. Subsequently an appropriate sampling procedure minimising...... labour costs and sampling uncertainty is proposed, where the MC of a single stem section with the length of 10–50 cm corresponds to the mean shoot moisture content (MSMC) with a bias of maximum 11 g kg−1. This bias can be reduced by selecting the stem section according to the particular clone...

Accident Sequence Evaluation Program: Human reliability analysis procedure

Energy Technology Data Exchange (ETDEWEB)

Swain, A.D.

1987-02-01

This document presents a shortened version of the procedure, models, and data for human reliability analysis (HRA) which are presented in the Handbook of Human Reliability Analysis With emphasis on Nuclear Power Plant Applications (NUREG/CR-1278, August 1983). This shortened version was prepared and tried out as part of the Accident Sequence Evaluation Program (ASEP) funded by the US Nuclear Regulatory Commission and managed by Sandia National Laboratories. The intent of this new HRA procedure, called the ''ASEP HRA Procedure,'' is to enable systems analysts, with minimal support from experts in human reliability analysis, to make estimates of human error probabilities and other human performance characteristics which are sufficiently accurate for many probabilistic risk assessments. The ASEP HRA Procedure consists of a Pre-Accident Screening HRA, a Pre-Accident Nominal HRA, a Post-Accident Screening HRA, and a Post-Accident Nominal HRA. The procedure in this document includes changes made after tryout and evaluation of the procedure in four nuclear power plants by four different systems analysts and related personnel, including human reliability specialists. The changes consist of some additional explanatory material (including examples), and more detailed definitions of some of the terms. 42 refs.

Initial analysis and curation plans for MUSES-C asteroidal samples

Science.gov (United States)

Yano, H.; Kushiro, I.; Fujiwara, A.

that there are a few more areas of expertise still lacked within the recommended members. Thus, the competition shall be repeated one or two more times (in early 2003 after the launch, and possibly in 2005 after in-situ data is obtained) in order to collect the best Japanese experts in the whole range of different types of analyses at the time of the sample return. The final members of the MASPET will be appointed about 2 years prior to the Earth return. Then they will conduct a Stest runT of the whole initial analysis procedures at the ISAS asteromaterial curation facility, to be newly created in next a few years, and their respective analysis facilities. This talk also covers the current concepts of the facility and plans of analysis procedure flow.

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)

A very sensitive LSC procedure to determine Ni-63 in environmental samples, steel and concrete

International Nuclear Information System (INIS)

Scheuerer, C.; Schupfner, R.; Schuettelkopf, H.

1995-01-01

This procedure to determine Ni-63 contributes to a safe and economically reasonable decommissioning of nuclear power plants. Co-60, Fe-55 and Ni-63 are the most abundant long-lived radionuclides associated with contaminated piping, hardware and concrete for a period of several decades of years after shutdown. Samples are carefully ashed leached, or dissolved by suitable mixtures of acids. The analysis starts with the absorption Ni 2+ on the chelating resin CHELEX 100. The next purification steps include an anionic exchange column and a precipitation as Ni-dimethyl-glyoxime, which is extracted into chloroform. After reextraction with sulfuric acid the solution containing Ni 2+ is mixed with a scintillation cocktail and counted in an anticoincidence shielded LSC. The decontamination factors are determined for all important artificially and naturally occurring radionuclides ranging form above 10 4 to 10 9 . The chemical yield adopts a value of (95±5)%. Up to maximum sample amounts of 0.4 g steel, 5 g concrete and about 100 g of environmental samples the detection limits are about 5 mBq per sample or 12 mBq/g steel, 1 mBq/g concrete and 0.05 mBq/g environmental sample at a counting time of 1000 minutes. (author) 16 refs.; 2 figs.; 2 tabs

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

Science.gov (United States)

Mullett, Wayne M

2007-03-10

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

Analysis of multiple single nucleotide polymorphisms (SNP) on DNA traces from plasma and dried blood samples

NARCIS (Netherlands)

Catsburg, Arnold; van der Zwet, Wil C.; Morre, Servaas A.; Ouburg, Sander; Vandenbroucke-Grauls, Christina M. J. E.; Savelkoul, Paul H. M.

2007-01-01

Reliable analysis of single nucleotide polymorphisms (SNPs) in DNA derived from samples containing low numbers of cells or from suboptimal sources can be difficult. A new procedure to characterize multiple SNPs in traces of DNA from plasma and old dried blood samples was developed. Six SNPs in the

Sampling procedure for lake or stream surface water chemistry

Science.gov (United States)

Robert Musselman

2012-01-01

Surface waters collected in the field for chemical analyses are easily contaminated. This research note presents a step-by-step detailed description of how to avoid sample contamination when field collecting, processing, and transporting surface water samples for laboratory analysis.

Experimental procedure for the determination of counting efficiency and sampling flow rate of a grab-sampling working level meter

International Nuclear Information System (INIS)

Grenier, M.; Bigu, J.

1982-07-01

The calibration procedures used for a working level meter (WLM) of the grab-sampling type are presented in detail. The WLM tested is a Pylon WL-1000C working level meter and it was calibrated for radon/thoron daughter counting efficiency (E), for sampling pump flow rate (Q) and other variables of interest. For the instrument calibrated at the Elliot Lake Laboratory, E was 0.22 +- 0.01 while Q was 4.50 +- 0.01 L/min

Analysis and optimization of blood-testing procedures.

NARCIS (Netherlands)

Bar-Lev, S.K.; Boxma, O.J.; Perry, D.; Vastazos, L.P.

2017-01-01

This paper is devoted to the performance analysis and optimization of blood testing procedures. We present a queueing model of two queues in series, representing the two stages of a blood-testing procedure. Service (testing) in stage 1 is performed in batches, whereas it is done individually in

Optimization of instrumental neutron activation analysis method by means of 2k experimental design technique aiming the validation of analytical procedures

International Nuclear Information System (INIS)

Petroni, Robson; Moreira, Edson G.

2013-01-01

In this study optimization of procedures and standardization of Instrumental Neutron Activation Analysis (INAA) methods were carried out for the determination of the elements arsenic, chromium, cobalt, iron, rubidium, scandium, selenium and zinc in biological materials. The aim is to validate the analytical methods for future accreditation at the National Institute of Metrology, Quality and Technology (INMETRO). The 2 k experimental design was applied for evaluation of the individual contribution of selected variables of the analytical procedure in the final mass fraction result. Samples of Mussel Tissue Certified Reference Material and multi-element standards were analyzed considering the following variables: sample decay time, counting time and sample distance to detector. The standard multi-element concentration (comparator standard), mass of the sample and irradiation time were maintained constant in this procedure. By means of the statistical analysis and theoretical and experimental considerations it was determined the optimized experimental conditions for the analytical methods that will be adopted for the validation procedure of INAA methods in the Neutron Activation Analysis Laboratory (LAN) of the Research Reactor Center (CRPq) at the Nuclear and Energy Research Institute (IPEN - CNEN/SP). Optimized conditions were estimated based on the results of z-score tests, main effect and interaction effects. The results obtained with the different experimental configurations were evaluated for accuracy (precision and trueness) for each measurement. (author)

Clinical procedure for colon carcinoma tissue sampling directly affects the cancer marker-capacity of VEGF family members

International Nuclear Information System (INIS)

Pringels, Sarah; Van Damme, Nancy; De Craene, Bram; Pattyn, Piet; Ceelen, Wim; Peeters, Marc; Grooten, Johan

2012-01-01

mRNA levels of members of the Vascular Endothelial Growth Factor family (VEGF-A, -B, -C, -D, Placental Growth Factor/PlGF) have been investigated as tissue-based markers of colon cancer. These studies, which used specimens obtained by surgical resection or colonoscopic biopsy, yielded contradictory results. We studied the effect of the sampling method on the marker accuracy of VEGF family members. Comparative RT-qPCR analysis was performed on healthy colon and colon carcinoma samples obtained by biopsy (n = 38) or resection (n = 39) to measure mRNA expression levels of individual VEGF family members. mRNA levels of genes encoding the eicosanoid enzymes cyclooxygenase 2 (COX2) and 5-lipoxygenase (5-LOX) and of genes encoding the hypoxia markers glucose transporter 1 (GLUT-1) and carbonic anhydrase IX (CAIX) were included as markers for cellular stress and hypoxia. Expression levels of COX2, 5-LOX, GLUT-1 and CAIX revealed the occurrence in healthy colon resection samples of hypoxic cellular stress and a concurrent increment of basal expression levels of VEGF family members. This increment abolished differential expression of VEGF-B and VEGF-C in matched carcinoma resection samples and created a surgery-induced underexpression of VEGF-D. VEGF-A and PlGF showed strong overexpression in carcinoma samples regardless of the sampling method. Sampling-induced hypoxia in resection samples but not in biopsy samples affects the marker-reliability of VEGF family members. Therefore, biopsy samples provide a more accurate report on VEGF family mRNA levels. Furthermore, this limited expression analysis proposes VEGF-A and PlGF as reliable, sampling procedure insensitive mRNA-markers for molecular diagnosis of colon cancer

An Integrated Solution-Based Rapid Sample Preparation Procedure for the Analysis of N-Glycans From Therapeutic Monoclonal Antibodies.

Science.gov (United States)

Aich, Udayanath; Liu, Aston; Lakbub, Jude; Mozdzanowski, Jacek; Byrne, Michael; Shah, Nilesh; Galosy, Sybille; Patel, Pramthesh; Bam, Narendra

2016-03-01

Consistent glycosylation in therapeutic monoclonal antibodies is a major concern in the biopharmaceutical industry as it impacts the drug's safety and efficacy and manufacturing processes. Large numbers of samples are created for the analysis of glycans during various stages of recombinant proteins drug development. Profiling and quantifying protein N-glycosylation is important but extremely challenging due to its microheterogeneity and more importantly the limitations of existing time-consuming sample preparation methods. Thus, a quantitative method with fast sample preparation is crucial for understanding, controlling, and modifying the glycoform variance in therapeutic monoclonal antibody development. Presented here is a rapid and highly quantitative method for the analysis of N-glycans from monoclonal antibodies. The method comprises a simple and fast solution-based sample preparation method that uses nontoxic reducing reagents for direct labeling of N-glycans. The complete work flow for the preparation of fluorescently labeled N-glycans takes a total of 3 h with less than 30 min needed for the release of N-glycans from monoclonal antibody samples. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

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.

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

International Nuclear Information System (INIS)

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

2006-01-01

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

Quantitative analysis of light elements in thick samples by PIGE

International Nuclear Information System (INIS)

Mateus, R.; Jesus, A.P.; Ribeiro, J.P.

2004-01-01

PIGE analysis of thick and intermediate samples is usually performed with the help of standards, but this method gives only good results when the standard is very similar to the sample to be analysed. In this work, we present an alternative method for PIGE analysis of light elements in thick samples. This method is based on a code that integrates the nuclear reaction excitation function along the depth of the sample. For the integration procedure the sample is divided in sublayers, defined by the energy steps that were used to measure accurately the excitation function. This function is used as input. Within each sublayer the stopping power cross-sections may be assumed as constant. With these two conditions the calculus of the contribution of each sublayer for the total yield becomes an easy task. This work presents results for the analysis of lithium, boron, fluorine and sodium in thick samples. For this purpose, excitation functions of the reactions 7 Li(p,p ' γ) 7 Li, 19 F(p,p ' γ) 19 F, 10 B(p,αγ) 7 Be and 23 Na(p,p ' γ) 23 Na were employed. Calculated γ-ray yields were compared, at several proton energy values, with experimental yields for thick samples made of inorganic compounds of the referred elements. The agreement is better than 7.5%. Taking into consideration the experimental uncertainty of the measured yields and the errors related to the stopping power values used, this agreement shows that effects as the beam energy straggling, ignored in the calculation, seem to play a minor role

Method to determine trace elements in water samples by neutron activation analysis

International Nuclear Information System (INIS)

Kueppers, G.; Erdtmann, G.

1981-05-01

For the determination of trace elements in water by neutron activation analysis irradiation porcedures and chemical separation procedures have been developed. Irradiation in melted quarz glass ampoules in the presence of a platinum wire (for recombination of the oxyhydrogen gas produced by radiolysis) proved successfull with different variants of the irradiation methods, as long irradiation periods without pressure build-up could be achieved. Possible falsifications of the analysis results were investigated in detail (losses by absorption on vessel walls etc.). The irradiated samples can be measured directly with a gamma ray spectrometer and from the radionuclides found the trace element contents may be calculated. More sensitive determinations are possible if the radionuclides are chemically separated. Procedures for removing the matrix activities, for the separation of the radionuclides in groups of elements and for the isolation of single elements have been developed. For especially sensitive determination of some elements selective separation procedures for antimony, cadmium, selenium, mercury and uranium have been developed. The analytical procedures described have been applied to trace element determinations in river water, glacier ice and water solutions from technical processes. (orig./RB) [de

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.

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.)

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

241-Z-361 Sludge Characterization Sampling and Analysis Plan

Energy Technology Data Exchange (ETDEWEB)

BANNING, D.L.

1999-08-05

This sampling and analysis plan (SAP) identifies the type, quantity, and quality of data needed to support characterization of the sludge that remains in Tank 241-2-361. The procedures described in this SAP are based on the results of the 241-2-361 Sludge Characterization Data Quality Objectives (DQO) (BWHC 1999) process for the tank. The primary objectives of this project are to evaluate the contents of Tank 241-2-361 in order to resolve safety and safeguards issues and to assess alternatives for sludge removal and disposal.

241-Z-361 Sludge Characterization Sampling and Analysis Plan

Energy Technology Data Exchange (ETDEWEB)

BANNING, D.L.

1999-07-29

This sampling and analysis plan (SAP) identifies the type, quantity, and quality of data needed to support characterization of the sludge that remains in Tank 241-2-361. The procedures described in this SAP are based on the results of the 241-2-361 Sludge Characterization Data Quality Objectives (DQO) (BWHC 1999) process for the tank. The primary objectives of this project are to evaluate the contents of Tank 241-2-361 in order to resolve safety and safeguards issues and to assess alternatives for sludge removal and disposal.

A DNA fingerprinting procedure for ultra high-throughput genetic analysis of insects.

Science.gov (United States)

Schlipalius, D I; Waldron, J; Carroll, B J; Collins, P J; Ebert, P R

2001-12-01

Existing procedures for the generation of polymorphic DNA markers are not optimal for insect studies in which the organisms are often tiny and background molecular information is often non-existent. We have used a new high throughput DNA marker generation protocol called randomly amplified DNA fingerprints (RAF) to analyse the genetic variability in three separate strains of the stored grain pest, Rhyzopertha dominica. This protocol is quick, robust and reliable even though it requires minimal sample preparation, minute amounts of DNA and no prior molecular analysis of the organism. Arbitrarily selected oligonucleotide primers routinely produced approximately 50 scoreable polymorphic DNA markers, between individuals of three independent field isolates of R. dominica. Multivariate cluster analysis using forty-nine arbitrarily selected polymorphisms generated from a single primer reliably separated individuals into three clades corresponding to their geographical origin. The resulting clades were quite distinct, with an average genetic difference of 37.5 +/- 6.0% between clades and of 21.0 +/- 7.1% between individuals within clades. As a prelude to future gene mapping efforts, we have also assessed the performance of RAF under conditions commonly used in gene mapping. In this analysis, fingerprints from pooled DNA samples accurately and reproducibly reflected RAF profiles obtained from individual DNA samples that had been combined to create the bulked samples.

Northern Marshall Islands radiological survey: sampling and analysis summary

Energy Technology Data Exchange (ETDEWEB)

Robison, W.L.; Conrado, C.L.; Eagle, R.J.; Stuart, M.L.

1981-07-23

A radiological survey was conducted in the Northern Marshall Islands to document reamining external gamma exposures from nuclear tests conducted at Enewetak and Bikini Atolls. An additional program was later included to obtain terrestrial and marine samples for radiological dose assessment for current or potential atoll inhabitants. This report is the first of a series summarizing the results from the terrestrial and marine surveys. The sample collection and processing procedures and the general survey methodology are discussed; a summary of the collected samples and radionuclide analyses is presented. Over 5400 samples were collected from the 12 atolls and 2 islands and prepared for analysis including 3093 soil, 961 vegetation, 153 animal, 965 fish composite samples (average of 30 fish per sample), 101 clam, 50 lagoon water, 15 cistern water, 17 groundwater, and 85 lagoon sediment samples. A complete breakdown by sample type, atoll, and island is given here. The total number of analyses by radionuclide are 8840 for /sup 241/Am, 6569 for /sup 137/Cs, 4535 for /sup 239 +240/Pu, 4431 for /sup 90/Sr, 1146 for /sup 238/Pu, 269 for /sup 241/Pu, and 114 each for /sup 239/Pu and /sup 240/Pu. A complete breakdown by sample category, atoll or island, and radionuclide is also included.

Northern Marshall Islands radiological survey: sampling and analysis summary

International Nuclear Information System (INIS)

Robison, W.L.; Conrado, C.L.; Eagle, R.J.; Stuart, M.L.

1981-01-01

A radiological survey was conducted in the Northern Marshall Islands to document reamining external gamma exposures from nuclear tests conducted at Enewetak and Bikini Atolls. An additional program was later included to obtain terrestrial and marine samples for radiological dose assessment for current or potential atoll inhabitants. This report is the first of a series summarizing the results from the terrestrial and marine surveys. The sample collection and processing procedures and the general survey methodology are discussed; a summary of the collected samples and radionuclide analyses is presented. Over 5400 samples were collected from the 12 atolls and 2 islands and prepared for analysis including 3093 soil, 961 vegetation, 153 animal, 965 fish composite samples (average of 30 fish per sample), 101 clam, 50 lagoon water, 15 cistern water, 17 groundwater, and 85 lagoon sediment samples. A complete breakdown by sample type, atoll, and island is given here. The total number of analyses by radionuclide are 8840 for 241 Am, 6569 for 137 Cs, 4535 for 239+240 Pu, 4431 for 90 Sr, 1146 for 238 Pu, 269 for 241 Pu, and 114 each for 239 Pu and 240 Pu. A complete breakdown by sample category, atoll or island, and radionuclide is also included

Sampling and Analysis Plan for N-Springs ERA pump-and-treat waste media

International Nuclear Information System (INIS)

Stankovich, M.T.

1996-07-01

This Sampling and Analysis Plan details the administrative procedures to be used to conduct sampling activities for characterization of spent ion-exchange resin, clinoptilolite, generated from the N-Springs pump-and-treat expedited response action. N-Springs (riverbank seeps) is located in the 100-N Area of the Hanford Site. Groundwater contained in the 100-NR-2 Operable Unit is contaminated with various radionuclides derived from wastewater disposal practices and spills associated with 100-N Reactor Operations

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.

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

Directory of Open Access Journals (Sweden)

Maria Hernandez-Valladares

2016-08-01

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

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

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.

Procedure manual for the estimation of average indoor radon-daughter concentrations using the radon grab-sampling method

International Nuclear Information System (INIS)

George, J.L.

1986-04-01

The US Department of Energy (DOE) Office of Remedial Action and Waste Technology established the Technical Measurements Center to provide standardization, calibration, comparability, verification of data, quality assurance, and cost-effectiveness for the measurement requirements of DOE remedial action programs. One of the remedial-action measurement needs is the estimation of average indoor radon-daughter concentration. One method for accomplishing such estimations in support of DOE remedial action programs is the radon grab-sampling method. This manual describes procedures for radon grab sampling, with the application specifically directed to the estimation of average indoor radon-daughter concentration (RDC) in highly ventilated structures. This particular application of the measurement method is for cases where RDC estimates derived from long-term integrated measurements under occupied conditions are below the standard and where the structure being evaluated is considered to be highly ventilated. The radon grab-sampling method requires that sampling be conducted under standard maximized conditions. Briefly, the procedure for radon grab sampling involves the following steps: selection of sampling and counting equipment; sample acquisition and processing, including data reduction; calibration of equipment, including provisions to correct for pressure effects when sampling at various elevations; and incorporation of quality-control and assurance measures. This manual describes each of the above steps in detail and presents an example of a step-by-step radon grab-sampling procedure using a scintillation cell

GeLC-MS: A Sample Preparation Method for Proteomics Analysis of Minimal Amount of Tissue.

Science.gov (United States)

Makridakis, Manousos; Vlahou, Antonia

2017-10-10

Application of various proteomics methodologies have been implemented for the global and targeted proteome analysis of many different types of biological samples such as tissue, urine, plasma, serum, blood, and cell lines. Among the aforementioned biological samples, tissue has an exceptional role into clinical research and practice. Disease initiation and progression is usually located at the tissue level of different organs, making the analysis of this material very important for the understanding of the disease pathophysiology. Despite the significant advances in the mass spectrometry instrumentation, tissue proteomics still faces several challenges mainly due to increased sample complexity and heterogeneity. However, the most prominent challenge is attributed to the invasive procedure of tissue sampling which restricts the availability of fresh frozen tissue to minimal amounts and limited number of samples. Application of GeLC-MS sample preparation protocol for tissue proteomics analysis can greatly facilitate making up for these difficulties. In this chapter, a step by step guide for the proteomics analysis of minute amounts of tissue samples using the GeLC-MS sample preparation protocol, as applied by our group in the analysis of multiple different types of tissues (vessels, kidney, bladder, prostate, heart) is provided.

Procedures monitoring and MAAP analysis

International Nuclear Information System (INIS)

May, R.S.

1991-01-01

Numerous studies of severe accidents in light water reactors have shown that operator response can play a crucial role in the predicted outcomes of dominant accident scenarios. MAAP provides the capability to specify certain operator actions as input data. However, making reasonable assumptions about the nature and timing of operator response requires substantial knowledge about plant practices and procedures and what they imply for the event being analyzed. The appearance of knowledge based software technology in the mid-1980s provided a natural format for representing and maintaining procedures as IF-THEN rules. The boiling water reactor (BWR) Emergency Operating Procedures Tracking System (EOPTS) was composed of a rule base of procedures and a dedicated inference engine (problem-solver). Based on the general approach and experience of EOPTS, the authors have developed a prototype procedures monitoring system that reads MAAP transient output files and evaluate the EOP messages and instructions that would be implied during each transient time interval. The prototype system was built using the NEXPERT OBJECT expert system development system, running on a 386-class personal computer with 4 MB of memory. The limited scope prototype includes a reduced set of BWR6 EOPs procedures evaluation on a coarse time interval, a simple text-based user interface, and a summary-report generator. The prototype, which is limited to batch-mode analysis of MAAP output, is intended to demonstrate the concept and aid in the design of a production system, which will involve a direct link to MAAP and interactive capabilities

Studies on thermal neutron perturbation factor needed for bulk sample activation analysis

CERN Document Server

Csikai, J; Sanami, T; Michikawa, T

2002-01-01

The spatial distribution of thermal neutrons produced by an Am-Be source in a graphite pile was measured via the activation foil method. The results obtained agree well with calculated data using the MCNP-4B code. A previous method used for the determination of the average neutron flux within thin absorbing samples has been improved and extended for a graphite moderator. A procedure developed for the determination of the flux perturbation factor renders the thermal neutron activation analysis of bulky samples of unknown composition possible both in hydrogenous and graphite moderators.

Optimization of instrumental neutron activation analysis method by means of 2{sup k} experimental design technique aiming the validation of analytical procedures

Energy Technology Data Exchange (ETDEWEB)

Petroni, Robson; Moreira, Edson G., E-mail: rpetroni@ipen.br, E-mail: emoreira@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

2013-07-01

In this study optimization of procedures and standardization of Instrumental Neutron Activation Analysis (INAA) methods were carried out for the determination of the elements arsenic, chromium, cobalt, iron, rubidium, scandium, selenium and zinc in biological materials. The aim is to validate the analytical methods for future accreditation at the National Institute of Metrology, Quality and Technology (INMETRO). The 2{sup k} experimental design was applied for evaluation of the individual contribution of selected variables of the analytical procedure in the final mass fraction result. Samples of Mussel Tissue Certified Reference Material and multi-element standards were analyzed considering the following variables: sample decay time, counting time and sample distance to detector. The standard multi-element concentration (comparator standard), mass of the sample and irradiation time were maintained constant in this procedure. By means of the statistical analysis and theoretical and experimental considerations it was determined the optimized experimental conditions for the analytical methods that will be adopted for the validation procedure of INAA methods in the Neutron Activation Analysis Laboratory (LAN) of the Research Reactor Center (CRPq) at the Nuclear and Energy Research Institute (IPEN - CNEN/SP). Optimized conditions were estimated based on the results of z-score tests, main effect and interaction effects. The results obtained with the different experimental configurations were evaluated for accuracy (precision and trueness) for each measurement. (author)

Failure mode analysis in adrenal vein sampling: a single-center experience.

Science.gov (United States)

Trerotola, Scott O; Asmar, Melissa; Yan, Yan; Fraker, Douglas L; Cohen, Debbie L

2014-10-01

To analyze failure modes in a high-volume adrenal vein sampling (AVS) practice in an effort to identify preventable causes of nondiagnostic sampling. A retrospective database was constructed containing 343 AVS procedures performed over a 10-year period. Each nondiagnostic AVS procedure was reviewed for failure mode and correlated with results of any repeat AVS. Data collected included selectivity index, lateralization index, adrenalectomy outcomes if performed, and details of AVS procedure. All AVS procedures were performed after cosyntropin stimulation, using sequential technique. AVS was nondiagnostic in 12 of 343 (3.5%) primary procedures and 2 secondary procedures. Failure was right-sided in 8 (57%) procedures, left-sided in 4 (29%) procedures, bilateral in 1 procedure, and neither in 1 procedure (laboratory error). Failure modes included diluted sample from correctly identified vein (n = 7 [50%]; 3 right and 4 left), vessel misidentified as adrenal vein (n = 3 [21%]; all right), failure to locate an adrenal vein (n = 2 [14%]; both right), cosyntropin stimulation failure (n = 1 [7%]; diagnostic by nonstimulated criteria), and laboratory error (n = 1 [7%]; specimen loss). A second AVS procedure was diagnostic in three of five cases (60%), and a third AVS procedure was diagnostic in one of one case (100%). Among the eight patients in whom AVS ultimately was not diagnostic, four underwent adrenalectomy based on diluted AVS samples, and one underwent adrenalectomy based on imaging; all five experienced improvement in aldosteronism. A substantial percentage of AVS failures occur on the left, all related to dilution. Even when technically nondiagnostic per strict criteria, some "failed" AVS procedures may be sufficient to guide therapy. Repeat AVS has a good yield. Copyright © 2014 SIR. Published by Elsevier Inc. All rights reserved.

The Influence of Sample Drying Procedures on Mercury Concentrations Analyzed in Soils

Czech Academy of Sciences Publication Activity Database

Hojdová, Maria; Rohovec, Jan; Chrastný, V.; Penížek, V.; Navrátil, Tomáš

2015-01-01

Roč. 94, č. 5 (2015), s. 570-576 ISSN 0007-4861 R&D Projects: GA ČR GP526/09/P404; GA ČR(CZ) GAP210/11/1369 Institutional support: RVO:67985831 Keywords : sample preparation * drying procedures * microbial activity * freeze-drying * contamination Subject RIV: DD - Geochemistry Impact factor: 1.191, year: 2015

Supplement to the UMTRA Project water sampling and analysis plan, Mexican Hat, Utah

International Nuclear Information System (INIS)

1995-09-01

This water sampling and analysis plan (WSAP) supplement supports the regulatory and technical basis for water sampling at the Mexican Hat, Utah, Uranium Mill Tailings Remedial Action (UMTRA) Project site, as defined in the 1994 WSAP document for Mexican Hat (DOE, 1994). Further, the supplement serves to confirm our present understanding of the site relative to the hydrogeology and contaminant distribution as well as our intention to continue to use the sampling strategy as presented in the 1994 WSAP document for Mexican Hat. Ground water and surface water monitoring activities are derived from the US Environmental Protection Agency regulations in 40 CFR Part 192 (1991) and 60 FR 2854 (1995). Sampling procedures are guided by the UMTRA Project standard operating procedures (JEG, n.d.), the Technical Approach Document (DOE, 1989), and the most effective technical approach for the site. Additional site-specific documents relevant to the Mexican Hat site are the Mexican Hat Long-Term Surveillance Plan (currently in progress), and the Mexican Hat Site Observational Work Plan (currently in progress)

Development of a simple extraction procedure for chlorpyrifos determination in food samples by immunoassay.

Science.gov (United States)

Gabaldón, J A; Maquieira, A; Puchades, R

2007-02-28

The suitability of immunoassay methodology for rapid and accurate determination of chlorpyrifos in vegetables was tested. The optimised ELISA detection limit was 0.32ng/ml, with a working range from 0.69 to 6.21ng/ml and an immunoassay test-mid point (IC(50)) of 2.08ng/ml. A rapid sample preparation procedure considering different parameters such as the amount of sample, volume of extractant, extraction time and dilution factor was optimised. The developed direct extraction (DE) and multiresidue (ME) standard procedures were performed in different fortified fresh and processed vegetable samples (tomato, bonnet pepper, bean, pea, asparagus, broccoli, watermelon, melon, lettuce, cucumber, celery and red pepper). Recoveries were in all cases in the whole range 85.2-108.9% for both DE and ME extracts. Also, the comparison of the results obtained by both immunochemical and chromatographic methods for spiked fruits and vegetables were good with a correlation coefficient (r) of 0.97.

Ultrasound extraction and thin layer chromatography-flame ionization detection analysis of the lipid fraction in marine mucilage samples.

Science.gov (United States)

Mecozzi, M; Amici, M; Romanelli, G; Pietrantonio, E; Deluca, A

2002-07-19

This paper reports an analytical procedure based on ultrasound to extract lipids in marine mucilage samples. The experimental conditions of the ultrasound procedure (solvent and time) were identified by a FT-IR study performed on different standard samples of lipids and of a standard humic sample, before and after the sonication treatment. This study showed that diethyl ether was a more suitable solvent than methanol for the ultrasonic extraction of lipids from environmental samples because it allowed to minimize the possible oxidative modifications of lipids due to the acoustic cavitation phenomena. The optimized conditions were applied to the extraction of total lipid amount in marine mucilage samples and TLC-flame ionization detection analysis was used to identify the relevant lipid sub-fractions present in samples.

Metrological approach to quantitative analysis of clinical samples by LA-ICP-MS: A critical review of recent studies.

Science.gov (United States)

Sajnóg, Adam; Hanć, Anetta; Barałkiewicz, Danuta

2018-05-15

Analysis of clinical specimens by imaging techniques allows to determine the content and distribution of trace elements on the surface of the examined sample. In order to obtain reliable results, the developed procedure should be based not only on the properly prepared sample and performed calibration. It is also necessary to carry out all phases of the procedure in accordance with the principles of chemical metrology whose main pillars are the use of validated analytical methods, establishing the traceability of the measurement results and the estimation of the uncertainty. This review paper discusses aspects related to sampling, preparation and analysis of clinical samples by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) with emphasis on metrological aspects, i.e. selected validation parameters of the analytical method, the traceability of the measurement result and the uncertainty of the result. This work promotes the introduction of metrology principles for chemical measurement with emphasis to the LA-ICP-MS which is the comparative method that requires studious approach to the development of the analytical procedure in order to acquire reliable quantitative results. Copyright © 2018 Elsevier B.V. All rights reserved.

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)

Operability test procedure for the Rotary Mode Core Sampling System Exhausters 3 and 4

International Nuclear Information System (INIS)

WSaldo, E.J.

1995-01-01

This document provides a procedure for performing operability testing of the Rotary Mode Core Sampling System Exhausters 3 ampersand 4. Upon completion of testing activities an operability testing report will be issued

Comparison of different methods for activation analysis of geological and pedological samples: Reactor and epithermal neutron activation, relative and monostandard method

International Nuclear Information System (INIS)

Alian, A.; Sansoni, B.

1980-04-01

Using purely instrumental methods, a comparative study is presented on neutron activation analysis of rock and soil samples by whole reactor neutron spectrum and epithermal neutrons with both relative and monostandard procedures. The latter procedure used with epithermal neutron activation analysis of soil samples necessitated the use of the 'effective resonance integrals' which were determined experimentally. The incorporation of the #betta# factor, representing deviation of reactor epithermal neutron flux from 1/E law, is developed in the present work. The main criteria for the choice of one or more of the procedures studied for a given purpose are also indicated. Analysis of 15 trace elements, Ca and Fe in the standard Japanese granite JG-1 using monostandard epithermal neutron activation gave results in good agreement with the average literature values. (orig./RB) [de

Quantification procedures in micro X-ray fluorescence analysis

International Nuclear Information System (INIS)

Kanngiesser, Birgit

2003-01-01

For the quantification in micro X-ray fluorescence analysis standardfree quantification procedures have become especially important. An introduction to the basic concepts of these quantification procedures is given, followed by a short survey of the procedures which are available now and what kind of experimental situations and analytical problems are addressed. The last point is extended by the description of an own development for the fundamental parameter method, which renders the inclusion of nonparallel beam geometries possible. Finally, open problems for the quantification procedures are discussed

System analysis procedures for conducting PSA of nuclear power plants

International Nuclear Information System (INIS)

Lee, Yoon Hwan; Jeong, Won Dae; Kim, Tae Un; Kim, Kil You; Han, Sang Hoon; Chang, Seung Chul; Sung, Tae Yong; Yang, Jun Eon; Kang, Dae Il; Park, Jin Hee; Hwang, Mi Jeong; Jin, Young Ho.

1997-03-01

This document, the Probabilistic Safety Assessment(PSA) procedures guide for system analysis, is intended to provide the guidelines to analyze the target of system consistently and technically in the performance of PSA for nuclear power plants(NPPs). The guide has been prepared in accordance with the procedures and techniques for fault tree analysis(FTA) used in system analysis. Normally the main objective of system analysis is to assess the reliability of system modeled by Event Tree Analysis(ETA). A variety of analytical techniques can be used for the system analysis, however, FTA method is used in this procedures guide. FTA is the method used for representing the failure logic of plant systems deductively using AND, OR or NOT gates. The fault tree should reflect all possible failure modes that may contribute to the system unavailability. This should include contributions due to the mechanical failures of the components, Common Cause Failures (CCFs), human errors and outages for testing and maintenance. After the construction of fault tree is completed, system unavailability is calculated with the CUT module of KIRAP, and the qualitative and quantitative analysis is performed through the process as above stated. As above mentioned, the procedures for system analysis is based on PSA procedures and methods which has been applied to the safety assessments of constructing NPPs in the country. Accordingly, the method of FTA stated in this procedures guide will be applicable to PSA for the NPPs to be constructed in the future. (author). 6 tabs., 11 figs., 7 refs

System analysis procedures for conducting PSA of nuclear power plants

Energy Technology Data Exchange (ETDEWEB)

Lee, Yoon Hwan; Jeong, Won Dae; Kim, Tae Un; Kim, Kil You; Han, Sang Hoon; Chang, Seung Chul; Sung, Tae Yong; Yang, Jun Eon; Kang, Dae Il; Park, Jin Hee; Hwang, Mi Jeong; Jin, Young Ho

1997-03-01

This document, the Probabilistic Safety Assessment(PSA) procedures guide for system analysis, is intended to provide the guidelines to analyze the target of system consistently and technically in the performance of PSA for nuclear power plants(NPPs). The guide has been prepared in accordance with the procedures and techniques for fault tree analysis(FTA) used in system analysis. Normally the main objective of system analysis is to assess the reliability of system modeled by Event Tree Analysis(ETA). A variety of analytical techniques can be used for the system analysis, however, FTA method is used in this procedures guide. FTA is the method used for representing the failure logic of plant systems deductively using AND, OR or NOT gates. The fault tree should reflect all possible failure modes that may contribute to the system unavailability. This should include contributions due to the mechanical failures of the components, Common Cause Failures (CCFs), human errors and outages for testing and maintenance. After the construction of fault tree is completed, system unavailability is calculated with the CUT module of KIRAP, and the qualitative and quantitative analysis is performed through the process as above stated. As above mentioned, the procedures for system analysis is based on PSA procedures and methods which has been applied to the safety assessments of constructing NPPs in the country. Accordingly, the method of FTA stated in this procedures guide will be applicable to PSA for the NPPs to be constructed in the future. (author). 6 tabs., 11 figs., 7 refs.

Radiochemical procedures and techniques

International Nuclear Information System (INIS)

Flynn, K.

1975-04-01

A summary is presented of the radiochemical procedures and techniques currently in use by the Chemistry Division Nuclear Chemistry Group at Argonne National Laboratory for the analysis of radioactive samples. (U.S.)

Sample size calculation while controlling false discovery rate for differential expression analysis with RNA-sequencing experiments.

Science.gov (United States)

Bi, Ran; Liu, Peng

2016-03-31

RNA-Sequencing (RNA-seq) experiments have been popularly applied to transcriptome studies in recent years. Such experiments are still relatively costly. As a result, RNA-seq experiments often employ a small number of replicates. Power analysis and sample size calculation are challenging in the context of differential expression analysis with RNA-seq data. One challenge is that there are no closed-form formulae to calculate power for the popularly applied tests for differential expression analysis. In addition, false discovery rate (FDR), instead of family-wise type I error rate, is controlled for the multiple testing error in RNA-seq data analysis. So far, there are very few proposals on sample size calculation for RNA-seq experiments. In this paper, we propose a procedure for sample size calculation while controlling FDR for RNA-seq experimental design. Our procedure is based on the weighted linear model analysis facilitated by the voom method which has been shown to have competitive performance in terms of power and FDR control for RNA-seq differential expression analysis. We derive a method that approximates the average power across the differentially expressed genes, and then calculate the sample size to achieve a desired average power while controlling FDR. Simulation results demonstrate that the actual power of several popularly applied tests for differential expression is achieved and is close to the desired power for RNA-seq data with sample size calculated based on our method. Our proposed method provides an efficient algorithm to calculate sample size while controlling FDR for RNA-seq experimental design. We also provide an R package ssizeRNA that implements our proposed method and can be downloaded from the Comprehensive R Archive Network ( http://cran.r-project.org ).

Study on different pre-treatment procedures for metal determination in Orujo spirit samples by ICP-AES

International Nuclear Information System (INIS)

Barciela, Julia; Vilar, Manuela; Garcia-Martin, Sagrario; Pena, Rosa M.; Herrero, Carlos

2008-01-01

In this work several pre-treatment methods were studied for metal (Na, K, Mg, Cu and Ca) determination in Orujo spirit samples using inductively coupled plasma atomic emission spectrometry (ICP-AES). Dilution, digestion, evaporation, and cryogenic desolvatation techniques were comparatively evaluated. Because of their analytical characteristics, digestion and evaporation with nitrogen current were found to be appropriate procedures for the determination of metals in alcoholic spirit samples. Yet, if simplicity and application time are to be considered, the latter-evaporation in a water bath with a nitrogen current-stands out as the optimum procedure for any further determinations in Orujo samples by ICP-AES. Low detection levels and wide linear ranges (sufficient to determine these metals in the samples studied) were achieved for each metal. The recoveries (in the 97.5-100.5% range) and the precision (R.S.D. lower than 5.6%) obtained were also satisfactory. The selected procedure was applied to determine the content of metals in 80 representative Galician Orujo spirit samples with and without a Certified Brand of Origin (CBO) which had been produced using different distillation systems. The metal concentrations ranged between 0.37 and 79.7 mg L -1 for Na, -1 for K, 0.02-4.83 mg L -1 for Mg content, -1 for Cu and 0.03-13.10 mg L -1 for Ca

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

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

International Nuclear Information System (INIS)

1994-05-01

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

Critical evaluation of distillation procedure for the determination of methylmercury in soil samples.

Science.gov (United States)

Perez, Pablo A; Hintelman, Holger; Quiroz, Waldo; Bravo, Manuel A

2017-11-01

In the present work, the efficiency of distillation process for extracting monomethylmercury (MMHg) from soil samples was studied and optimized using an experimental design methodology. The influence of soil composition on MMHg extraction was evaluated by testing of four soil samples with different geochemical characteristics. Optimization suggested that the acid concentration and the duration of the distillation process were most significant and the most favorable conditions, established as a compromise for the studied soils, were determined to be a 70 min distillation using an 0.2 M acid. Corresponding limits of detection (LOD) and quantification (LOQ) were 0.21 and 0.7 pg absolute, respectively. The optimized methodology was applied with satisfactory results to soil samples and was compared to a reference methodology based on isotopic dilution analysis followed by gas chromatography-inductively coupled plasma mass spectrometry (IDA-GC-ICP-MS). Using the optimized conditions, recoveries ranged from 82 to 98%, which is an increase of 9-34% relative to the previously used standard operating procedure. Finally, the validated methodology was applied to quantify MMHg in soils collected from different sites impacted by coal fired power plants in the north-central zone of Chile, measuring MMHg concentrations ranging from 0.091 to 2.8 ng g -1 . These data are to the best of our knowledge the first MMHg measurements reported for Chile. Copyright © 2017 Elsevier Ltd. All rights reserved.

Optimization conditions of samples saponification for tocopherol analysis.

Science.gov (United States)

Souza, Aloisio Henrique Pereira; Gohara, Aline Kirie; Rodrigues, Ângela Claudia; Ströher, Gisely Luzia; Silva, Danielle Cristina; Visentainer, Jesuí Vergílio; Souza, Nilson Evelázio; Matsushita, Makoto

2014-09-01

A full factorial design 2(2) (two factors at two levels) with duplicates was performed to investigate the influence of the factors agitation time (2 and 4 h) and the percentage of KOH (60% and 80% w/v) in the saponification of samples for the determination of α, β and γ+δ-tocopherols. The study used samples of peanuts (cultivar armadillo), produced and marketed in Maringá, PR. The factors % KOH and agitation time were significant, and an increase in their values contributed negatively to the responses. The interaction effect was not significant for the response δ-tocopherol, and the contribution of this effect to the other responses was positive, but less than 10%. The ANOVA and response surfaces analysis showed that the most efficient saponification procedure was obtained using a 60% (w/v) solution of KOH and with an agitation time of 2 h. Copyright © 2014 Elsevier Ltd. All rights reserved.

RECOMMENDED OPERATING PROCEDURE NO. 56: COLLECTION OF GASEOUS GRAB SAMPLES FROM COMBUSTION SOURCES FOR NITROUS OXIDE MEASUREMENT

Science.gov (United States)

The document is a recommended operating procedure, prepare or use in research activities conducted by EPA's Air and Energy Engineering Research Laboratory (AEERL). The procedure applies to the collection of gaseous grab samples from fossil fuel combustion sources for subsequent a...

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)

Fractionation of metals in street sediment samples by using the BCR sequential extraction procedure and multivariate statistical elucidation of the data

International Nuclear Information System (INIS)

Kartal, Senol; Aydin, Zeki; Tokalioglu, Serife

2006-01-01

The concentrations of metals (Cd, Co, Cr, Cu, Fe, Mn, Ni, Pb, and Zn) in street sediment samples were determined by flame atomic absorption spectrometry (FAAS) using the modified BCR (the European Community Bureau of Reference) sequential extraction procedure. According to the BCR protocol for extracting the metals from the relevant target phases, 1.0 g of specimen of the sample was treated with 0.11 M acetic acid (exchangeable and bound to carbonates), 0.5 M hydroxylamine hydrochloride (bound to iron- and manganese-oxides), and 8.8 M hydrogen peroxide plus 1 M ammonium acetate (bound to sulphides and organics), sequentially. The residue was treated with aqua regia solution for recovery studies, although this step is not part of the BCR procedure. The mobility sequence based on the sum of the BCR sequential extraction stages was: Cd ∼ Zn (∼90%) > Pb (∼84%) > Cu (∼75%) > Mn (∼70%) > Co (∼57%) > Ni (∼43%) > Cr (∼40%) > Fe (∼17%). Enrichment factors as the criteria for examining the impact of the anthropogenic emission sources of heavy metals were calculated, and it was observed that the highest enriched elements were Cd, Pb, and Zn in the dust samples, average 190, 111, and 20, respectively. Correlation analysis (CA) and principal component analysis (PCA) were applied to the data matrix to evaluate the analytical results and to identify the possible pollution sources of metals. PCA revealed that the sampling area was mainly influenced from three pollution sources, namely; traffic, industrial, and natural sources. The results show that chemical sequential extraction is a precious operational tool. Validation of the analytical results was checked by both recovery studies and analysis of the standard reference material (NIST SRM 2711 Montana Soil)

Uranium tailings sampling manual

International Nuclear Information System (INIS)

Feenstra, S.; Reades, D.W.; Cherry, J.A.; Chambers, D.B.; Case, G.G.; Ibbotson, B.G.

1985-01-01

The purpose of this manual is to describe the requisite sampling procedures for the application of uniform high-quality standards to detailed geotechnical, hydrogeological, geochemical and air quality measurements at Canadian uranium tailings disposal sites. The selection and implementation of applicable sampling procedures for such measurements at uranium tailings disposal sites are complicated by two primary factors. Firstly, the physical and chemical nature of uranium mine tailings and effluent is considerably different from natural soil materials and natural waters. Consequently, many conventional methods for the collection and analysis of natural soils and waters are not directly applicable to tailings. Secondly, there is a wide range in the physical and chemical nature of uranium tailings. The composition of the ore, the milling process, the nature of tailings depositon, and effluent treatment vary considerably and are highly site-specific. Therefore, the definition and implementation of sampling programs for uranium tailings disposal sites require considerable evaluation, and often innovation, to ensure that appropriate sampling and analysis methods are used which provide the flexibility to take into account site-specific considerations. The following chapters describe the objective and scope of a sampling program, preliminary data collection, and the procedures for sampling of tailings solids, surface water and seepage, tailings pore-water, and wind-blown dust and radon

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

International Nuclear Information System (INIS)

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

1978-01-01

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

New experimental procedure for measuring volume magnetostriction on powder samples

International Nuclear Information System (INIS)

Rivero, G.; Multigner, M.; Valdes, J.; Crespo, P.; Martinez, A.; Hernando, A.

2005-01-01

Conventional techniques used for volume magnetostriction measurements, as strain gauge or cantilever method, are very useful for ribbons or thin films but cannot be applied when the samples are in powder form. To overcome this problem a new experimental procedure has been developed. In this work, the experimental set-up is described, together with the results obtained in amorphous FeCuZr powders, which exhibit a strong dependence of the magnetization on the strength of the applied magnetic field. The magnetostriction measurements presented in this work point out that this dependence is related to a magnetovolume effect

Beef, chicken and lamb fatty acid analysis--a simplified direct bimethylation procedure using freeze-dried material.

Science.gov (United States)

Lee, M R F; Tweed, J K S; Kim, E J; Scollan, N D

2012-12-01

When fractionation of meat lipids is not required, procedures such as saponification can be used to extract total fatty acids, reducing reliance on toxic organic compounds. However, saponification of muscle fatty acids is laborious, and requires extended heating times, and a second methylation step to convert the extracted fatty acids to fatty acid methyl esters prior to gas chromatography. Therefore the development of a more rapid direct methylation procedure would be of merit. The use of freeze-dried material for analysis is common and allows for greater homogenisation of the sample. The present study investigated the potential of using freeze-dried muscle samples and a direct bimethylation to analyse total fatty acids of meat (beef, chicken and lamb) in comparison with a saponification procedure followed by bimethylation. Both methods compared favourably for all major fatty acids measured. There was a minor difference in relation to the C18:1 trans 10 isomer with a greater (Psaponification. However, numerically the difference was small and likely as a result of approaching the limits of isomer identification by single column gas chromatography. Differences (Psaponification to analyse total fatty acids from muscle samples. Copyright © 2012 Elsevier Ltd. All rights reserved.

ORNL-PWR BDHT analysis procedure: an overview

International Nuclear Information System (INIS)

Cliff, S.B.

1978-01-01

The key computer programs currently used by the analysis procedure of the ORNL-PWR Blowdown Heat Transfer Separate Effects Program are overviewed with particular emphasis placed on their interrelationships. The major modeling and calculational programs, COBRA, ORINC, ORTCAL, PINSIM, and various versions of RELAP4, are summarized and placed into the perspective of the procedure. The supportive programs, REDPLT, ORCPLT, BDHTPLOT, OXREPT, and OTOCI, and their uses are described

A novel procedure on next generation sequencing data analysis using text mining algorithm.

Science.gov (United States)

Zhao, Weizhong; Chen, James J; Perkins, Roger; Wang, Yuping; Liu, Zhichao; Hong, Huixiao; Tong, Weida; Zou, Wen

2016-05-13

Next-generation sequencing (NGS) technologies have provided researchers with vast possibilities in various biological and biomedical research areas. Efficient data mining strategies are in high demand for large scale comparative and evolutional studies to be performed on the large amounts of data derived from NGS projects. Topic modeling is an active research field in machine learning and has been mainly used as an analytical tool to structure large textual corpora for data mining. We report a novel procedure to analyse NGS data using topic modeling. It consists of four major procedures: NGS data retrieval, preprocessing, topic modeling, and data mining using Latent Dirichlet Allocation (LDA) topic outputs. The NGS data set of the Salmonella enterica strains were used as a case study to show the workflow of this procedure. The perplexity measurement of the topic numbers and the convergence efficiencies of Gibbs sampling were calculated and discussed for achieving the best result from the proposed procedure. The output topics by LDA algorithms could be treated as features of Salmonella strains to accurately describe the genetic diversity of fliC gene in various serotypes. The results of a two-way hierarchical clustering and data matrix analysis on LDA-derived matrices successfully classified Salmonella serotypes based on the NGS data. The implementation of topic modeling in NGS data analysis procedure provides a new way to elucidate genetic information from NGS data, and identify the gene-phenotype relationships and biomarkers, especially in the era of biological and medical big data. The implementation of topic modeling in NGS data analysis provides a new way to elucidate genetic information from NGS data, and identify the gene-phenotype relationships and biomarkers, especially in the era of biological and medical big data.

Indirect Electrochemical Analysis of Crocin in Phytochemical Sample

Directory of Open Access Journals (Sweden)

Riyaz Ahmad Dar

2012-01-01

Full Text Available A new electroanalytical method has been developed for the quantitative determination of crocin in a sample of stigmas of saffron (Crocus sativus L.. Crocin is polarographically inactive. However, cysteine in 0.02 M NaCl, pH=5.2±0.01 produces a well defined wave/peak with E1/2/Ep= –0.47/–0.45 V vs. Ag/AgCl. On recording polarograms of a set of solution containing a fixed concentration of cysteine and varying concentrations of crocin under aforesaid experimental conditions a gradual decrease in peak height/diffusion current and a negative shift in peak potential was observed. Thus, indicating cysteine-crocin interaction. Amperometric titration indicated crocin to cysteine ratio of 1:2. The above amperometric titration procedure has been used to determine the concentration of crocin in a sample of saffron. Crystallization process was carried out for the extraction of crocin from dried powder of saffron stigmas. The crystallized crocin was identified by UV-Visible spectrophotometry(at 255 nm and 442 nm and the quantitative analysis by the developed amperometric method. The concentration of crocin in saffron was found to be 2.13% and purity of isolated crocin 96.81%. The percent recovery varied from 98.56–100.31% and RSD (n=5 of 2.17%.The validation of the proposed procedure for the quantitative assay of crocin was examined via an evaluation of the repeatability, recovery, selectivity and relative standard deviation.

UMTRA project water sampling and analysis plan, Falls City, Texas. Revision 1

International Nuclear Information System (INIS)

1995-09-01

Planned, routine ground water sampling activities at the US Department of Energy (DOE) Uranium Mill Tailings Remedial Action (UMTRA) Project site near Falls City, Texas, are described in this water sampling and analysis plan (WSAP). The following plan identifies and justifies the sampling locations, analytical parameters, and sampling frequency for the routine monitoring stations at the site. The ground water data are used for site characterization and risk assessment. The regulatory basis for routine ground water monitoring at UMTRA Project sites is derived from the US Environmental Protection Agency (EPA) regulations in 40 CFR Part 192. Sampling procedures are guided by the UMTRA Project standard operating procedures (SOP) (JEG, n.d.), the Technical Approach Document (TAD) (DOE, 1989), and the most effective technical approach for the site. The Falls City site is in Karnes County, Texas, approximately 8 miles [13 kilometers southwest of the town of Falls City and 46 mi (74 km) southeast of San Antonio, Texas. Before surface remedial action, the tailings site consisted of two parcels. Parcel A consisted of the mill site, one mill building, five tailings piles, and one tailings pond south of Farm-to-Market (FM) Road 1344 and west of FM 791. A sixth tailings pile designated Parcel B was north of FM 791 and east of FM 1344

External quality control in ground-water sampling and analysis at the Hanford Site

International Nuclear Information System (INIS)

Hall, S.H.; Juracich, S.P.

1991-11-01

At the US Department of Energy's Hanford Site, external Quality Control (QC) for ground-water monitoring is extensive and has included routine submittal of intra- and interlaboratory duplicate samples, blind samples, and several kinds of blank samples. Examination of the resulting QC data for nine of the constituents found in ground water at the Hanford Site shows that the quality of analysis has generally been within the expectations of precision and accuracy that have been established by the US Environmental Protection Agency (EPA). The constituents subjected to review were nitrate, chromium, sodium, fluoride, carbon tetrachloride, tritium, ammonium, trichloroethylene, and cyanide. Of these, the fluoride measurements were notable exceptions and were poor by EPA standards. The review has shown that interlaboratory analysis of duplicate samples yields the most useful QC data for evaluating laboratory performance in determining commonly encountered constituents. For rarely encountered constituents, interlaboratory comparisons may be augmented with blind samples (synthetic samples of known composition). Intralaboratory comparisons, blanks, and spikes should be generally restricted to studies of suspected or known sample contamination and to studies of the adequacy of sampling and analytical procedures

Microwave-Assisted Sample Treatment in a Fully Automated Flow-Based Instrument: Oxidation of Reduced Technetium Species in the Analysis of Total Technetium-99 in Caustic Aged Nuclear Waste Samples

International Nuclear Information System (INIS)

Egorov, Oleg B.; O'Hara, Matthew J.; Grate, Jay W.

2004-01-01

An automated flow-based instrument for microwave-assisted treatment of liquid samples has been developed and characterized. The instrument utilizes a flow-through reaction vessel design that facilitates the addition of multiple reagents during sample treatment, removal of the gaseous reaction products, and enables quantitative removal of liquids from the reaction vessel for carryover-free operations. Matrix modification and speciation control chemistries that are required for the radiochemical determination of total 99Tc in caustic aged nuclear waste samples have been investigated. A rapid and quantitative oxidation procedure using peroxydisulfate in acidic solution was developed to convert reduced technetium species to pertechnetate in samples with high content of reducing organics. The effectiveness of the automated sample treatment procedures has been validated in the radiochemical analysis of total 99Tc in caustic aged nuclear waste matrixes from the Hanford site

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.

Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 101

International Nuclear Information System (INIS)

Diaz, L.A.

1998-01-01

One waste sample that was obtained with solids from tank 101 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprene tubing (Phthalate free) was obtained in a glass jar with teflon lid was analyzed (with duplicate, matrix spike, and matrix spike duplicate) for PCBs as Aroclor mixtures by the Inorganic/Organic Chemistry Group. A soxhlet extraction procedure was used for extraction of the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). Results are presented

Ultra-high performance supercritical fluid chromatography-mass spectrometry procedure for analysis of monosaccharides from plant gum binders.

Science.gov (United States)

Pauk, Volodymyr; Pluháček, Tomáš; Havlíček, Vladimír; Lemr, Karel

2017-10-09

The ultra-high performance supercritical fluid chromatography-mass spectrometry (UHPSFC/MS) procedure for analysis of native monosaccharides was developed. Chromatographic conditions were investigated to separate a mixture of four hexoses, three pentoses, two deoxyhexoses and two uronic acids. Increasing water content in methanol modifier to 5% and formic acid to 4% improved peak shapes of neutral monosaccharides and allowed complete elution of highly polar uronic acids in a single run. An Acquity HSS C18SB column outperformed other three tested stationary phases (BEH (silica), BEH 2-ethylpyridine, CSH Fluoro-Phenyl) in terms of separation of isomers and analysis time (4.5 min). Limits of detection were in the range 0.01-0.12 ng μL -1 . Owing to separation of anomers, identification of critical pairs (arabinose-xylose and glucose-galactose) was possible. Feasibility of the new method was demonstrated on plant-derived polysaccharide binders. Samples of watercolor paints, painted paper and three plant gums widely encountered in painting media (Arabic, cherry and tragacanth) were decomposed prior the analysis by microwave-assisted hydrolysis at 40 bar initial pressure using 2 mol L -1 trifluoroacetic acid. Among tested temperatures, 120 °C ensured appropriate hydrolysis efficiency for different types of gum and avoided excessive degradation of labile monosaccharides. Procedure recovery tested on gum Arabic was 101% with an RSD below 8%. Aqueous hydrolysates containing monosaccharides in different ratios specific to each type of plant gum were diluted or analyzed directly. Filtration of samples before hydrolysis reduced interferences from a paper support and identification of gum Arabic in watercolor-painted paper samples was demonstrated. Successful identification of pure gum Arabic was confirmed for sample quantities as little as 1 μg. Two classification approaches were compared and principal component analysis was superior to analysis based on peak area

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)

Study on different pre-treatment procedures for metal determination in Orujo spirit samples by ICP-AES

Energy Technology Data Exchange (ETDEWEB)

Barciela, Julia; Vilar, Manuela; Garcia-Martin, Sagrario [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain); Pena, Rosa M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain)], E-mail: qarosa@lugo.usc.es; Herrero, Carlos [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias, Universidad de Santiago de Compostela, Campus de Lugo, 27002 Lugo (Spain)], E-mail: cherrero@lugo.usc.es

2008-10-17

In this work several pre-treatment methods were studied for metal (Na, K, Mg, Cu and Ca) determination in Orujo spirit samples using inductively coupled plasma atomic emission spectrometry (ICP-AES). Dilution, digestion, evaporation, and cryogenic desolvatation techniques were comparatively evaluated. Because of their analytical characteristics, digestion and evaporation with nitrogen current were found to be appropriate procedures for the determination of metals in alcoholic spirit samples. Yet, if simplicity and application time are to be considered, the latter-evaporation in a water bath with a nitrogen current-stands out as the optimum procedure for any further determinations in Orujo samples by ICP-AES. Low detection levels and wide linear ranges (sufficient to determine these metals in the samples studied) were achieved for each metal. The recoveries (in the 97.5-100.5% range) and the precision (R.S.D. lower than 5.6%) obtained were also satisfactory. The selected procedure was applied to determine the content of metals in 80 representative Galician Orujo spirit samples with and without a Certified Brand of Origin (CBO) which had been produced using different distillation systems. The metal concentrations ranged between 0.37 and 79.7 mg L{sup -1} for Na,

Recovery of extracellular vesicles from human breast milk is influenced by sample collection and vesicle isolation procedures

Directory of Open Access Journals (Sweden)

Marijke I. Zonneveld

2014-08-01

Full Text Available Extracellular vesicles (EV in breast milk carry immune relevant proteins and could play an important role in the instruction of the neonatal immune system. To further analyze these EV and to elucidate their function it is important that native populations of EV can be recovered from (stored breast milk samples in a reproducible fashion. However, the impact of isolation and storage procedures on recovery of breast milk EV has remained underexposed. Here, we aimed to define parameters important for EV recovery from fresh and stored breast milk. To compare various protocols across different donors, breast milk was spiked with a well-defined murine EV population. We found that centrifugation of EV down into density gradients largely improved density-based separation and isolation of EV, compared to floatation up into gradients after high-force pelleting of EV. Using cryo-electron microscopy, we identified different subpopulations of human breast milk EV and a not previously described population of lipid tubules. Additionally, the impact of cold storage on breast milk EV was investigated. We determined that storing unprocessed breast milk at −80°C or 4°C caused death of cells present in breast milk, leading to contamination of the breast milk EV population with storage-induced EV. Here, an alternative method is proposed to store breast milk samples for EV analysis at later time points. The proposed adaptations to the breast milk storage and EV isolation procedures can be applied for EV-based biomarker profiling of breast milk and functional analysis of the role of breast milk EV in the development of the neonatal immune system.

Analytical Chemistry Laboratory (ACL) procedure compendium

International Nuclear Information System (INIS)

1993-01-01

This volume contains the interim change notice for sample preparation methods. Covered are: acid digestion for metals analysis, fusion of Hanford tank waste solids, water leach of sludges/soils/other solids, extraction procedure toxicity (simulate leach in landfill), sample preparation for gamma spectroscopy, acid digestion for radiochemical analysis, leach preparation of solids for free cyanide analysis, aqueous leach of solids for anion analysis, microwave digestion of glasses and slurries for ICP/MS, toxicity characteristic leaching extraction for inorganics, leach/dissolution of activated metal for radiochemical analysis, extraction of single-shell tank (SST) samples for semi-VOC analysis, preparation and cleanup of hydrocarbon- containing samples for VOC and semi-VOC analysis, receiving of waste tank samples in onsite transfer cask, receipt and inspection of SST samples, receipt and extrusion of core samples at 325A shielded facility, cleaning and shipping of waste tank samplers, homogenization of solutions/slurries/sludges, and test sample preparation for bioassay quality control program

SEM/TIMS analysis trials on hotswipe samples taken from a shielded cell at Harwell

International Nuclear Information System (INIS)

Tushingham, J.; Vatter, I.; Cooke, R.

1998-09-01

The IAEA require advanced techniques and procedures for the detection of traces of actinides to be applied to their environmental sampling programme for nuclear safeguards as a means to detect undeclared activities. 'Swipe' samples taken from within nuclear facilities by IAEA inspectors require analysis to determine their actinide content and composition by bulk and particle measurements. The use of analytical equipment capable of analysing individual particles, particularly of actinides, is essential to optimise the IAEA's aim to monitor Member State's nuclear activities more proficiently. A trial has been undertaken at the Harwell Laboratory of AEA Technology to establish the efficacy of scanning electron microscopy (SEM) and thermal ionisation mass spectrometry (TIMS) for the particle and bulk characterisation, respectively, of actinides on samples taken from within a shielded cell. These measurements were supported by γ-spectrometry and α-spectrometry. 'Hotswipe' samples taken from within a shielded cell with a well-known recent history have been prepared for particle and bulk analysis. SEM has been used to characterise individual particles from the swipe samples and the results have been related to known cell activities. Samples were prepared for SEM using a simple procedure to minimise the potential for sample contamination. The method proved to be capable of identifying 1 μm particles that contained U, Pu, Pa and Np. The measurement of U/Pu ratios was limited to particles that contained >2% Pu in U by weight. TIMS, together with alpha spectrometry, has been used to determine the bulk actinide composition of the samples whilst gamma spectrometry has been used to determine the fission product composition. Further work to improve the potential of SEM, and also secondary ionisation mass spectrometry (SIMS), for the measurement of hotswipe samples has been proposed. (author)

Challenges of sample preparation for cross sectional EBSD analysis of electrodeposited nickel films

DEFF Research Database (Denmark)

Alimadadi, Hossein; Pantleon, Karen

2009-01-01

Thorough microstructure and crystallographic orientation analysis of thin films by means of electron backscatter diffraction requires cross section preparation of the film-substrate compound. During careful preparation, changes of the rather non-stable as-deposited microstructure must be avoided....... Different procedures for sample preparation including mechanical grinding and polishing, electropolishing and focused ion beam milling have been applied to a nickel film electrodeposited on top of an amorphous Ni-P layer on a Cu-substrate. Reliable EBSD analysis of the whole cross section can be obtained...

Flood risk analysis procedure for nuclear power plants

International Nuclear Information System (INIS)

Wagner, D.P.

1982-01-01

This paper describes a methodology and procedure for determining the impact of floods on nuclear power plant risk. The procedures are based on techniques of fault tree and event tree analysis and use the logic of these techniques to determine the effects of a flood on system failure probability and accident sequence occurrence frequency. The methodology can be applied independently or as an add-on analysis for an existing risk assessment. Each stage of the analysis yields useful results such as the critical flood level, failure flood level, and the flood's contribution to accident sequence occurrence frequency. The results of applications show the effects of floods on the risk from nuclear power plants analyzed in the Reactor Safety Study

Minerals sampling: sensibility analysis and correction factors for Pierre Gy's equation

International Nuclear Information System (INIS)

Vallebuona, G.; Niedbalski, F.

2005-01-01

Pierre Gy's equation is widely used in ore sampling. This equation is based in four parameters: shape factor, size distribution factor, mineralogical factor and liberation factor. The usual practice is to consider fixed values for the shape and size distribution factors. This practice does not represent well several important ores. The mineralogical factor considers only one specie of interest and the gangue, leaving out other cases such as polymetallic ores where there are more than one species of interest. A sensibility analysis to the Gy's equation factors was done and a procedure to determine specific values for them was developed and presented in this work. mean ore characteristics, associated with an insecure use of the actual procedure, were determined. finally, for a case study, the effects of using each alternative were evaluated. (Author) 4 refs

Carotenoid determination in recent marine sediments - practical problems during sample preparation and HPLC analysis

Directory of Open Access Journals (Sweden)

Magdalena Krajewska

2017-05-01

Full Text Available An analytical procedure for the analysis of carotenoids in marine sediments rich in organic matter has been developed. Analysis of these compounds is difficult; the application of methods used by other authors required optimization for the samples studied here. The analytical procedure involved multiple ultrasound-assisted extraction with acetone followed by liquid-liquid extraction (acetone extract:benzene:water - 15:1:10 v/v/v and HPLC analysis. The influence of column temperature on pigment separation and the quantification method were investigated – a temperature of 5 °C was selected for the Lichrospher 100 RP-18e column. The pigments in the sediment extract were quantified using a method based on HPLC analysis (at 450 nm and spectrophotometric measurements (at 450 nm, and extinction coefficients were determined for standard solutions at this wavelength. It is very important to use the value of the extinction coefficient appropriate to the wavelength at which the detection of carotenoids was carried out.

Comparative analysis of diagnostic accuracy of different brain biopsy procedures.

Science.gov (United States)

Jain, Deepali; Sharma, Mehar Chand; Sarkar, Chitra; Gupta, Deepak; Singh, Manmohan; Mahapatra, A K

2006-12-01

Image-guided procedures such as computed tomography (CT) guided, neuronavigator-guided and ultrasound-guided methods can assist neurosurgeons in localizing the intraparenchymal lesion of the brain. However, despite improvements in the imaging techniques, an accurate diagnosis of intrinsic lesion requires tissue sampling and histological verification. The present study was carried out to examine the reliability of the diagnoses made on tumor sample obtained via different stereotactic and ultrasound-guided brain biopsy procedures. A retrospective analysis was conducted of all brain biopsies (frame-based and frameless stereotactic and ultrasound-guided) performed in a single tertiary care neurosciences center between 1995 and 2005. The overall diagnostic accuracy achieved on histopathology and correlation with type of biopsy technique was evaluated. A total of 130 cases were included, which consisted of 82 males and 48 females. Age ranged from 4 to 75 years (mean age 39.5 years). Twenty per cent (27 patients) were in the pediatric age group, while 12% (16 patients) were >or= 60-years of age. A definitive histological diagnosis was established in 109 cases (diagnostic yield 80.2%), which encompassed 101 neoplastic and eight nonneoplastic lesions. Frame-based, frameless stereotactic and ultrasound-guided biopsies were done in 95, 15 and 20 patients respectively. Although the numbers of cases were small there was trend for better yield with frameless image-guided stereotactic biopsy and maximum diagnostic yield was obtained i.e, 87% (13/15) in comparison to conventional frame-based CT-guided stereotactic biopsy and ultrasound-guided biopsy. Overall, a trend of higher diagnostic yield was seen in cases with frameless image-guided stereotactic biopsy. Thus, this small series confirms that frameless neuronavigator-guided stereotactic procedures represent the lesion sufficiently in order to make histopathologic diagnosis.

Sampling and Analysis Plan Update for Groundwater Monitoring 1100-EM-1 Operable Unit

International Nuclear Information System (INIS)

DR Newcomer

1999-01-01

This document updates the sampling and analysis plan (Department of Energy/Richland Operations--95-50) to reflect current groundwater monitoring at the 1100-EM-1Operable Unit. Items requiring updating included sampling and analysis protocol, quality assurance and quality control, groundwater level measurement procedure, and data management. The plan covers groundwater monitoring, as specified in the 1993 Record of Decision, during the 5-year review period from 1995 through 1999. Following the 5-year review period, groundwater-monitoring data will be reviewed by Environmental Protection Agency to evaluate the progress of natural attenuation of trichloroethylene. Monitored natural attenuation and institutional controls for groundwater use at the inactive Horn Rapids Landfill was the selected remedy specified in the Record of Decision

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

International Nuclear Information System (INIS)

2009-01-01

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

General Staining and Segmentation Procedures for High Content Imaging and Analysis.

Science.gov (United States)

Chambers, Kevin M; Mandavilli, Bhaskar S; Dolman, Nick J; Janes, Michael S

2018-01-01

Automated quantitative fluorescence microscopy, also known as high content imaging (HCI), is a rapidly growing analytical approach in cell biology. Because automated image analysis relies heavily on robust demarcation of cells and subcellular regions, reliable methods for labeling cells is a critical component of the HCI workflow. Labeling of cells for image segmentation is typically performed with fluorescent probes that bind DNA for nuclear-based cell demarcation or with those which react with proteins for image analysis based on whole cell staining. These reagents, along with instrument and software settings, play an important role in the successful segmentation of cells in a population for automated and quantitative image analysis. In this chapter, we describe standard procedures for labeling and image segmentation in both live and fixed cell samples. The chapter will also provide troubleshooting guidelines for some of the common problems associated with these aspects of HCI.

75 FR 32295 - Expedited Approval of Alternative Test Procedures for the Analysis of Contaminants Under the Safe...

Science.gov (United States)

2010-06-08

... Approval of Alternative Test Procedures for the Analysis of Contaminants Under the Safe Drinking Water Act... methods for use in measuring the levels of contaminants in drinking water and determining compliance with... required to measure contaminants in drinking water samples. In addition, EPA Regions as well as States and...

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

40 CFR 86.140-94 - Exhaust sample analysis.

Science.gov (United States)

2010-07-01

... pressure during zero and span (and background bag reading) must be exactly the same as that used during... test. Background samples are collected in sample bags and analyzed as in paragraphs (b)(4) (i) or (ii... procedure results in negative NMHCwm values (as may occur with high methane fractions), any negative NMHCwm...

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

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.

A DATABASE FOR TRACKING TOXICOGENOMIC SAMPLES AND PROCEDURES WITH GENOMIC, PROTEOMIC AND METABONOMIC COMPONENTS

Science.gov (United States)

A Database for Tracking Toxicogenomic Samples and Procedures with Genomic, Proteomic and Metabonomic Components Wenjun Bao1, Jennifer Fostel2, Michael D. Waters2, B. Alex Merrick2, Drew Ekman3, Mitchell Kostich4, Judith Schmid1, David Dix1Office of Research and Developmen...

Sample preparation for liquid chromatographic analysis of phytochemicals in biological fluids.

Science.gov (United States)

Oh, Ju-Hee; Lee, Young-Joo

2014-01-01

Natural products have been used traditionally for the treatment and prevention of diseases for thousands of years and are nowadays consumed as dietary supplements and herbal medicine. To ensure the safe and effective use of these herbal products, information about bioavailability of active compounds in plasma or target tissues should be provided via validated analytical methods combined with appropriate sampling methods. To provide comprehensive and abridged information about sample preparation methods for the quantification of phytochemicals in biological samples using liquid chromatography analysis. Sample pre-treatment procedures used in analytical methods for in vivo pharmacokinetic studies of natural compounds or herbal medicines were reviewed. These were categorised according to the biological matrices (plasma, bile, urine, faeces and tissues) and sample clean-up processes (protein precipitation, liquid-liquid extraction and solid-phase extraction). Although various kinds of sample pre-treatment methods have been developed, liquid-liquid extraction is still widely used and solid-phase extraction is becoming increasingly popular because of its efficiency for extensive clean up of complex matrix samples. However, protein precipitation is still favoured due to its simplicity. Sample treatment for phytochemical analysis in biological fluids is an indispensable and critical step to obtain high quality results. This step could dominate the overall analytical process because both the duration of the process as well as the reliability of the data depend in large part on its efficiency. Thus, special attention should be given to the choice of a proper sample treatment method that targets analytes and their biomatrix. Copyright © 2013 John Wiley & Sons, Ltd.

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

Science.gov (United States)

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

2009-10-01

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

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

International Nuclear Information System (INIS)

Noyori, Amanda

2017-01-01

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

A combined method for DNA analysis and radiocarbon dating from a single sample.

Science.gov (United States)

Korlević, Petra; Talamo, Sahra; Meyer, Matthias

2018-03-07

Current protocols for ancient DNA and radiocarbon analysis of ancient bones and teeth call for multiple destructive samplings of a given specimen, thereby increasing the extent of undesirable damage to precious archaeological material. Here we present a method that makes it possible to obtain both ancient DNA sequences and radiocarbon dates from the same sample material. This is achieved by releasing DNA from the bone matrix through incubation with either EDTA or phosphate buffer prior to complete demineralization and collagen extraction utilizing the acid-base-acid-gelatinization and ultrafiltration procedure established in most radiocarbon dating laboratories. Using a set of 12 bones of different ages and preservation conditions we demonstrate that on average 89% of the DNA can be released from sample powder with minimal, or 38% without any, detectable collagen loss. We also detect no skews in radiocarbon dates compared to untreated samples. Given the different material demands for radiocarbon dating (500 mg of bone/dentine) and DNA analysis (10-100 mg), combined DNA and collagen extraction not only streamlines the sampling process but also drastically increases the amount of DNA that can be recovered from limited sample material.

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

Fundamental quantification procedure for total reflection X-ray fluorescence spectra analysis and elements determination

International Nuclear Information System (INIS)

Wegrzynek, D.; Holynska, B.

1997-01-01

A method for the determination of the concentrations of elements in particulate-like samples measured in total reflection geometry is proposed. In the proposed method the fundamental parameters are utilized for calculating the sensitivities of elements and an internal standard is used to account for the unknown mass per unit area of a sample and geometrical constant of the spectrometer. The modification of the primary excitation spectrum on its way to a sample has been taken into consideration. The concentrations of the elements to be determined are calculated simultaneously with the spectra deconvolution procedure. In the process of quantitative analysis the intensities of all X-ray peaks corresponding to K and L-series lines present in the analyzed spectrum are taken into account. (Author)

Establishing a routine procedure for extraction of water from vegetation samples

International Nuclear Information System (INIS)

Varlam, Carmen; Stefanescu, Ioan; Faurescu, Ionut; Vagner, Irina; Faurescu, Denisa

2008-01-01

Full text: The Cryogenic Pilot is an experimental project within the nuclear energy national research program, which has the aim of developing technologies for tritium and deuterium separation by cryogenic distillation. The process, used in this installation, is based on a combined method for liquid-phase catalytic exchange (LPCE) and cryogenic distillation. There are two ways that Cryogenic Pilot can interact with the environment: by atmospheric release and by sewage. In order to establish the base line of tritium concentration in the environment around the nuclear facilities we investigated the preparation procedure for different type of samples: soil, hay, apple, grass, milk, meat and water. For azeotropic distillation of all types of samples two solvents were used, toluene and cyclohexane, and all measurements for determination of environmental tritium concentration were carry out using liquid scintillation counting (LSC), with ultra-low level liquid scintillation spectrometer Quantulus 1220 specially designed for environmental samples and low radioactivity. Sample scintillation cocktail ratio was 8:12 ml and liquid scintillation cocktail was UltimaGold LLT. The background determined for control samples prepared ranged between 0.926 Cpm and 1.002 Cpm and counting efficiency between 25.3% and 26.1%. The counting time was 1000 minutes (50 minutes/20 cycles) for each sample, and minimum detectable activity according to ISO 9698 was 8.9 TU, and 9.05 TU, respectively, with a confidence coefficient of 3. (authors)

Optimization of a Pre-MEKC Separation SPE Procedure for Steroid Molecules in Human Urine Samples

Directory of Open Access Journals (Sweden)

Ilona Olędzka

2013-11-01

Full Text Available Many steroid hormones can be considered as potential biomarkers and their determination in body fluids can create opportunities for the rapid diagnosis of many diseases and disorders of the human body. Most existing methods for the determination of steroids are usually time- and labor-consuming and quite costly. Therefore, the aim of analytical laboratories is to develop a new, relatively low-cost and rapid implementation methodology for their determination in biological samples. Due to the fact that there is little literature data on concentrations of steroid hormones in urine samples, we have made attempts at the electrophoretic determination of these compounds. For this purpose, an extraction procedure for the optimized separation and simultaneous determination of seven steroid hormones in urine samples has been investigated. The isolation of analytes from biological samples was performed by liquid-liquid extraction (LLE with dichloromethane and compared to solid phase extraction (SPE with C18 and hydrophilic-lipophilic balance (HLB columns. To separate all the analytes a micellar electrokinetic capillary chromatography (MECK technique was employed. For full separation of all the analytes a running buffer (pH 9.2, composed of 10 mM sodium tetraborate decahydrate (borax, 50 mM sodium dodecyl sulfate (SDS, and 10% methanol was selected. The methodology developed in this work for the determination of steroid hormones meets all the requirements of analytical methods. The applicability of the method has been confirmed for the analysis of urine samples collected from volunteers—both men and women (students, amateur bodybuilders, using and not applying steroid doping. The data obtained during this work can be successfully used for further research on the determination of steroid hormones in urine samples.

Safeguards Network Analysis Procedure (SNAP): overview

International Nuclear Information System (INIS)

Chapman, L.D; Engi, D.

1979-08-01

Nuclear safeguards systems provide physical protection and control of nuclear materials. The Safeguards Network Analysis Procedure (SNAP) provides a convenient and standard analysis methodology for the evaluation of physical protection system effectiveness. This is achieved through a standard set of symbols which characterize the various elements of safeguards systems and an analysis program to execute simulation models built using the SNAP symbology. The outputs provided by the SNAP simulation program supplements the safeguards analyst's evaluative capabilities and supports the evaluation of existing sites as well as alternative design possibilities. This paper describes the SNAP modeling technique and provides an example illustrating its use

Standard methods for sampling and sample preparation for gamma spectroscopy

International Nuclear Information System (INIS)

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

1993-01-01

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

Current Human Reliability Analysis Methods Applied to Computerized Procedures

Energy Technology Data Exchange (ETDEWEB)

Ronald L. Boring

2012-06-01

Computerized procedures (CPs) are an emerging technology within nuclear power plant control rooms. While CPs have been implemented internationally in advanced control rooms, to date no US nuclear power plant has implemented CPs in its main control room (Fink et al., 2009). Yet, CPs are a reality of new plant builds and are an area of considerable interest to existing plants, which see advantages in terms of enhanced ease of use and easier records management by omitting the need for updating hardcopy procedures. The overall intent of this paper is to provide a characterization of human reliability analysis (HRA) issues for computerized procedures. It is beyond the scope of this document to propose a new HRA approach or to recommend specific methods or refinements to those methods. Rather, this paper serves as a review of current HRA as it may be used for the analysis and review of computerized procedures.

Adrenal venous sampling: the learning curve of a single interventionalist with 282 consecutive procedures.

Science.gov (United States)

Jakobsson, Hugo; Farmaki, Katerina; Sakinis, Augustinas; Ehn, Olof; Johannsson, Gudmundur; Ragnarsson, Oskar

2018-01-01

Primary aldosteronism (PA) is a common cause of secondary hypertension. Adrenal venous sampling (AVS) is the gold standard for assessing laterality of PA, which is of paramount importance to decide adequate treatment. AVS is a technically complicated procedure with success rates ranging between 30% and 96%. The aim of this study was to investigate the success rate of AVS over time, performed by a single interventionalist. This was a retrospective study based on consecutive AVS procedures performed by a single operator between September 2005 and June 2016. Data on serum concentrations of aldosterone and cortisol from right and left adrenal vein, inferior vena cava, and peripheral vein were collected and selectivity index (SI) calculated. Successful AVS was defined as SI > 5. In total, 282 AVS procedures were performed on 269 patients, 168 men (62%) and 101 women (38%), with a mean age of 55±11 years (range, 26-78 years). Out of 282 AVS procedures, 259 were successful, giving an overall success rate of 92%. The most common reason for failure was inability to localize the right adrenal vein (n=16; 76%). The success rates were 63%, 82%, and 94% during the first, second, and third years, respectively. During the last 8 years the success rate was 95%, and on average 27 procedures were performed annually. Satisfactory AVS success rate was achieved after approximately 36 procedures and satisfactory success rate was maintained by performing approximately 27 procedures annually. AVS should be limited to few operators that perform sufficiently large number of procedures to achieve, and maintain, satisfactory AVS success rate.

Procedures for field chemical analyses of water samples

International Nuclear Information System (INIS)

Korte, N.; Ealey, D.

1983-12-01

A successful water-quality monitoring program requires a clear understanding of appropriate measurement procedures in order to obtain reliable field data. It is imperative that the responsible personnel have a thorough knowledge of the limitations of the techniques being used. Unfortunately, there is a belief that field analyses are simple and straightforward. Yet, significant controversy as well as misuse of common measurement techniques abounds. This document describes procedures for field measurements of pH, carbonate and bicarbonate, specific conductance, dissolved oxygen, nitrate, Eh, and uranium. Each procedure section includes an extensive discussion regarding the limitations of the method as well as brief discussions of calibration procedures and available equipment. A key feature of these procedures is the consideration given to the ultimate use of the data. For example, if the data are to be used for geochemical modeling, more precautions are needed. In contrast, routine monitoring conducted merely to recognize gross changes can be accomplished with less effort. Finally, quality assurance documentation for each measurement is addressed in detail. Particular attention is given to recording sufficient information such that decisions concerning the quality of the data can be easily made. Application of the procedures and recommendations presented in this document should result in a uniform and credible water-quality monitoring program. 22 references, 4 figures, 3 tables

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

Headspace solid-phase microextraction procedures for gas chromatographic analysis of biological fluids and materials.

Science.gov (United States)

Mills, G A; Walker, V

2000-12-01

Solid-phase microextraction (SPME) is a new solventless sample preparation technique that is finding wide usage. This review provides updated information on headspace SPME with gas chromatographic separation for the extraction and measurement of volatile and semivolatile analytes in biological fluids and materials. Firstly the background to the technique is given in terms of apparatus, fibres used, extraction conditions and derivatisation procedures. Then the different matrices, urine, blood, faeces, breast milk, hair, breath and saliva are considered separately. For each, methods appropriate for the analysis of drugs and metabolites, solvents and chemicals, anaesthetics, pesticides, organometallics and endogenous compounds are reviewed and the main experimental conditions outlined with specific examples. Then finally, the future potential of SPME for the analysis of biological samples in terms of the development of new devices and fibre chemistries and its coupling with high-performance liquid chromatography is discussed.

Dimethyl adipimidate/Thin film Sample processing (DTS); A simple, low-cost, and versatile nucleic acid extraction assay for downstream analysis.

Science.gov (United States)

Shin, Yong; Lim, Swee Yin; Lee, Tae Yoon; Park, Mi Kyoung

2015-09-15

Sample processing, especially that involving nucleic acid extraction, is a prerequisite step for the isolation of high quantities of relatively pure DNA for downstream analyses in many life science and biomedical engineering studies. However, existing methods still have major problems, including labor-intensive time-consuming methods and high costs, as well as requirements for a centrifuge and the complex fabrication of filters and membranes. Here, we first report a versatile Dimethyl adipimidate/Thin film based Sample processing (DTS) procedure without the limitations of existing methods. This procedure is useful for the extraction of DNA from a variety of sources, including 6 eukaryotic cells, 6 bacteria cells, and 2 body fluids in a single step. Specifically, the DTS procedure does not require a centrifuge and has improved time efficiency (30 min), affordability, and sensitivity in downstream analysis. We validated the DTS procedure for the extraction of DNA from human body fluids, as well as confirmed that the quality and quantity of the extracted DNA were sufficient to allow robust detection of genetic and epigenetic biomarkers in downstream analysis.

Results of the analysis of the intercomparison samples of the depleted uranium dioxide SR-20

International Nuclear Information System (INIS)

Aigner, H.; Deron, S.; Kuhn, E.; Ronesch, K.; Zoigner, A.

Samples of a homogeneous powder of depleted uranium dioxide, SR-20, were distributed to 32 laboratories in January 1980 for intercomparison of the precisions and accuracies of wet chemical assay. 11 laboratories reported their results (ANNEX 1). 5 laboratories applied titration procedures, 4 of them applied methods derived from the Davies and Gray procedure (1), 2 laboratories used controlled potential coulometry, 2 laboratories used precipitation procedures, 1 laboratory used fluorimetry and 1 laboratory used activation analysis. An analysis of variance yields for each laboratory the estimates of the measurement errors, the dissolution or treatment errors and the random calibration errors. The measurement errors vary between 0.01% and 1.7% relative. The differences to the reference value vary between -9.1% and +0.92% uranium, but 9 laboratories agree within +-1%U with the reference value. The mean bias of these 9 laboratories is equal to +0.04%U. The standard deviation of the biases of these 9 laboratories is equal to 0.36%.U

Sample handling of clinical specimens for ultratrace element analysis

International Nuclear Information System (INIS)

Cornelis, R.

1987-01-01

Some simple logistics to an improved sample handling of clinical specimens are presented. This comprises clean room conditions, clean laboratory ware, ultra-pure reagents and good analytical practice. Sample handling procedures for blood, urine, soft tissues and pharmaceuticals are briefly discussed. (author) 26 refs

Procedural-support music therapy in the healthcare setting: a cost-effectiveness analysis.

Science.gov (United States)

DeLoach Walworth, Darcy

2005-08-01

This comparative analysis examined the cost-effectiveness of music therapy as a procedural support in the pediatric healthcare setting. Many healthcare organizations are actively attempting to reduce the amount of sedation for pediatric patients undergoing various procedures. Patients receiving music therapy-assisted computerized tomography scans ( n = 57), echocardiograms ( n = 92), and other procedures ( n = 17) were included in the analysis. Results of music therapy-assisted procedures indicate successful elimination of patient sedation, reduction in procedural times, and decrease in the number of staff members present for procedures. Implications for nurses and music therapists in the healthcare setting are discussed.

Protein precipitation: an expedient procedure for the routine analysis of the plasma metabolites of [123I]IBZM

International Nuclear Information System (INIS)

Zea-Ponce, Yolanda; Laruelle, Marc

1999-01-01

Plasma metabolite analysis of the single photon emission computed tomography (SPECT) D 2 /D 3 receptor radiotracer (S)(-)-N-[(1-ethyl-2-pyrrolidinyl)methyl]-2-hydroxy-3-[ 123 I] iodo-6-methoxyb enzamide ([ 123 I]IBZM) is needed for the equilibrium analysis of the SPECT data, in brain imaging studies involving bolus plus constant infusion paradigm. The purpose of these experiments was to find an appropriate procedure to expedite this analysis during routine determinations. The procedure was applied to the plasma analysis of 22 human subjects. Each plasma sample was subjected to acetonitrile protein precipitation. After separation of the pellet, the acetonitrile fraction contained 91%±2% (n=88) of the mixture of labeled metabolites and parent compound. The recovery coefficient of unmetabolized [ 123 I]IBZM determined with an standard plasma sample was 95%±2% (n=22). The percent parent compound present in the extracted fraction, measured by high performance liquid chromatography, was 16%±9% (n=85) and the percent metabolites was 84%±9% (n=85). Free fraction determination (f 1 , fraction of radiotracer unbound to protein), was 4%±0.8% (n=22). Free fraction of parent was 15%±8% (n=85). The results indicate that acetonitrile protein precipitation is an adequate method for the analysis of the [ 123 I]IBZM plasma metabolites

Influence of the derivatization procedure on the results of the gaschromatographic fatty acid analysis of human milk and infant formulae.

Science.gov (United States)

Kohn, G; van der Ploeg, P; Möbius, M; Sawatzki, G

1996-09-01

Many different analytical procedures for fatty acid analysis of infant formulae and human milk are described. The objective was to study possible pitfalls in the use of different acid-catalyzed procedures compared to a base-catalyzed procedure based on sodium-methoxide in methanol. The influence of the different methods on the relative fatty acid composition (wt% of total fatty acids) and the total fatty acid recovery rate (expressed as % of total lipids) was studied in two experimental LCP-containing formulae and a human milk sample. MeOH/HCl-procedures were found to result in an incomplete transesterification of triglycerides, if an additional nonpolar solvent like toluene or hexane is not added and a water-free preparation is not guaranteed. In infant formulae the low transesterification of triglycerides (up to only 37%) could result in an 100%-overestimation of the relative amount of LCP, if these fatty acids primarily derive from phospholipids. This is the case in infant formulae containing egg lipids as raw materials. In formula containing fish oils and in human milk the efficacy of esterification results in incorrect absolute amounts of fatty acids, but has no remarkable effect on the relative fatty acid distribution. This is due to the fact that in these samples LCP are primarily bound to triglycerides. Furthermore, in formulae based on butterfat the derivatization procedure should be designed in such a way that losses of short-chain fatty acids due to evaporation steps can be avoided. The procedure based on sodium methoxide was found to result in a satisfactory (about 90%) conversion of formula lipids and a reliable content of all individual fatty acids. Due to a possibly high amount of free fatty acids in human milk, which are not methylated by sodium-methoxide, caution is expressed about the use of this reagent for fatty acid analysis of mothers milk. It is concluded that accurate fatty acid analysis of infant formulae and human milk requires a careful

The analysis of Th in the Korean total diet sample by RNAA

International Nuclear Information System (INIS)

Chung, Yong Sam; Moon, Jong Hwa; Kang, Sang Hoon; Park, Kwang Won

1999-01-01

In order to estimate the degree of intake of 232 Th through daily diet, a korean total diet sample was collected and made after the investigation of the amount of consumption of daily diet which is dependent on the ages of 20's to 50's. For Th analysis, the RNAA method was applied and NIST SRM 1575, Pine Needle was used as quality control materials. The result of the SRM analysis was compared with a certified value. The relative error was 5%. The determination of the Th in the korean total diet sample was carried out under the same analytical condition and procedure with SRM. As a result of the korean total diet sample, the concentration of Th was in 3.4 ± 0.2 ppb and the amount of daily intake of Th by the diet is found to be 0.67 g per day. Radioactivity by Th intake was estimated to be about 2.7 mBq per person per day and annual dose equivalent was revealed as 0.73 μSv per person

Systematic sampling with errors in sample locations

DEFF Research Database (Denmark)

Ziegel, Johanna; Baddeley, Adrian; Dorph-Petersen, Karl-Anton

2010-01-01

analysis using point process methods. We then analyze three different models for the error process, calculate exact expressions for the variances, and derive asymptotic variances. Errors in the placement of sample points can lead to substantial inflation of the variance, dampening of zitterbewegung......Systematic sampling of points in continuous space is widely used in microscopy and spatial surveys. Classical theory provides asymptotic expressions for the variance of estimators based on systematic sampling as the grid spacing decreases. However, the classical theory assumes that the sample grid...... is exactly periodic; real physical sampling procedures may introduce errors in the placement of the sample points. This paper studies the effect of errors in sample positioning on the variance of estimators in the case of one-dimensional systematic sampling. First we sketch a general approach to variance...

A Quantitative Review of Functional Analysis Procedures in Public School Settings

Science.gov (United States)

Solnick, Mark D.; Ardoin, Scott P.

2010-01-01

Functional behavioral assessments can consist of indirect, descriptive and experimental procedures, such as a functional analysis. Although the research contains numerous examples demonstrating the effectiveness of functional analysis procedures, experimental conditions are often difficult to implement in classroom settings and analog conditions…

Micro-scaled high-throughput digestion of plant tissue samples for multi-elemental analysis

Directory of Open Access Journals (Sweden)

Husted Søren

2009-09-01

Full Text Available Abstract Background Quantitative multi-elemental analysis by inductively coupled plasma (ICP spectrometry depends on a complete digestion of solid samples. However, fast and thorough sample digestion is a challenging analytical task which constitutes a bottleneck in modern multi-elemental analysis. Additional obstacles may be that sample quantities are limited and elemental concentrations low. In such cases, digestion in small volumes with minimum dilution and contamination is required in order to obtain high accuracy data. Results We have developed a micro-scaled microwave digestion procedure and optimized it for accurate elemental profiling of plant materials (1-20 mg dry weight. A commercially available 64-position rotor with 5 ml disposable glass vials, originally designed for microwave-based parallel organic synthesis, was used as a platform for the digestion. The novel micro-scaled method was successfully validated by the use of various certified reference materials (CRM with matrices rich in starch, lipid or protein. When the micro-scaled digestion procedure was applied on single rice grains or small batches of Arabidopsis seeds (1 mg, corresponding to approximately 50 seeds, the obtained elemental profiles closely matched those obtained by conventional analysis using digestion in large volume vessels. Accumulated elemental contents derived from separate analyses of rice grain fractions (aleurone, embryo and endosperm closely matched the total content obtained by analysis of the whole rice grain. Conclusion A high-throughput micro-scaled method has been developed which enables digestion of small quantities of plant samples for subsequent elemental profiling by ICP-spectrometry. The method constitutes a valuable tool for screening of mutants and transformants. In addition, the method facilitates studies of the distribution of essential trace elements between and within plant organs which is relevant for, e.g., breeding programmes aiming at

Infrared thermometry and the crop water stress index. II. Sampling procedures and interpretation

International Nuclear Information System (INIS)

Gardner, B.R.; Nielsen, D.C.; Shock, C.C.

1992-01-01

Infrared thermometry can be a valuable research and production tool for detecting and quantifying water stress in plants, as shown by a large volume of published research. Users of infrared thermometers (IRT) should be aware of the many equipment, environmental, and plant factors influencing canopy temperature measured by an IRT. The purpose of this paper is to describe factors influencing measured plant temperature, outline sampling procedures that will produce reliable Crop Water Stress Index (CWSI) values, and offer interpretations of CWSI and plant temperatures relative to crop production and other water stress parameters by reviewing previously conducted research. Factors that are considered are IRT condition, configuration, and position; psychrometer location; wind speed; solar radiation; time of day; leaf area and orientation; and appropriate non-water-stressed baseline equation. Standard sampling and CWSI calculation procedures are proposed. Use of CWSI with crops varying in type of response to water stress is described. Previously conducted research on plant temperatures or CWSI is tabulated by crop and water stress parameters measured. The paper provides valuable information to assist interested users of IRTs in making reliable water stress measurements. (author)

Infrared thermometry and the crop water stress index. II. Sampling procedures and interpretation

Energy Technology Data Exchange (ETDEWEB)

Gardner, B. R. [BP Research, Cleveland, OH (United States); Nielsen, D. C.; Shock, C. C.

1992-10-15

Infrared thermometry can be a valuable research and production tool for detecting and quantifying water stress in plants, as shown by a large volume of published research. Users of infrared thermometers (IRT) should be aware of the many equipment, environmental, and plant factors influencing canopy temperature measured by an IRT. The purpose of this paper is to describe factors influencing measured plant temperature, outline sampling procedures that will produce reliable Crop Water Stress Index (CWSI) values, and offer interpretations of CWSI and plant temperatures relative to crop production and other water stress parameters by reviewing previously conducted research. Factors that are considered are IRT condition, configuration, and position; psychrometer location; wind speed; solar radiation; time of day; leaf area and orientation; and appropriate non-water-stressed baseline equation. Standard sampling and CWSI calculation procedures are proposed. Use of CWSI with crops varying in type of response to water stress is described. Previously conducted research on plant temperatures or CWSI is tabulated by crop and water stress parameters measured. The paper provides valuable information to assist interested users of IRTs in making reliable water stress measurements. (author)

Analysis of biological slurry samples by total x-ray fluorescence after in situ microwave digestion

International Nuclear Information System (INIS)

Lue-Meru, M.P.; Capote, T.; Greaves, E.

2000-01-01

Biological slurry samples were analyzed by total reflection x-ray fluorescence (TXRF) after an in situ microwave digestion procedure on the quartz reflector. This method lead to the removal of the matrix by the digestion and permits the enrichment of the analites by using sample amounts higher than those normally used in TXRF for the thin layer requirement since the organic matrix is removed. In consequence, the pre-concentration of sample is performed and the detection capability is increased by a quasi direct method. The samples analyzed were the international IAEA blood standard, the SRM bovine liver 1577-a standard and fresh onion tissues. Slurries were prepared in three ways: a.- weighing a sample amount on the reflector and adding suprapure nitric acid and internal standard followed by microwave digestion, b.-weighing a sample amount and water with an appropriate concentration of the internal standard in an Eppendorf vial, taking then an aliquot to the quartz reflector for microwave digestion with suprapure nitric acid, c.- weighing a sample amount of fresh tissue, homogenising with high speed homegenator to obtain a slurry sample which can be diluted in an ependorf vial with water an the internal standard. Then an aliquot is taken to the reflector for microwave digestion with suprapure nitric acid. Further details of sample preparation procedures will be discussed during presentation. The analysis was carried out in a Canberra spectrometer using the Kalpha lines of the Ag and Mo tubes. The elements Ca, K, Fe, Cu, Zn, Se, Mn, Rb, Br, Sr were determined. The effect of the preparation procedure was evaluated by the accuracy and precision of the results for each element and the percent of recovery. (author)

Radiation and environmental data analysis computer (REDAC) hardware, software band analysis procedures

International Nuclear Information System (INIS)

Hendricks, T.J.

1985-01-01

The REDAC was conceived originally as a tape verifier for the Radiation and Environmental Data Acquisition Recorder (REDAR). From that simple beginning in 1971, the REDAC has evolved into a family of systems used for complete analysis of data obtained by the REDAR and other acquisition systems. Portable or mobile REDACs are deployed to support checkout and analysis tasks in the field. Laboratory systems are additionally used for software development, physics investigations, data base management and graphics. System configurations range from man-portable systems to a large laboratory-based system which supports time-shared analysis and development tasks. Custom operating software allows the analyst to process data either interactively or by batch procedures. Analysis packages are provided for numerous necessary functions. All these analysis procedures can be performed even on the smallest man-portable REDAC. Examples of the multi-isotope stripping and radiation isopleth mapping are presented. Techniques utilized for these operations are also presented

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...

Rapid DNA analysis for automated processing and interpretation of low DNA content samples.

Science.gov (United States)

Turingan, Rosemary S; Vasantgadkar, Sameer; Palombo, Luke; Hogan, Catherine; Jiang, Hua; Tan, Eugene; Selden, Richard F

2016-01-01

Short tandem repeat (STR) analysis of casework samples with low DNA content include those resulting from the transfer of epithelial cells from the skin to an object (e.g., cells on a water bottle, or brim of a cap), blood spatter stains, and small bone and tissue fragments. Low DNA content (LDC) samples are important in a wide range of settings, including disaster response teams to assist in victim identification and family reunification, military operations to identify friend or foe, criminal forensics to identify suspects and exonerate the innocent, and medical examiner and coroner offices to identify missing persons. Processing LDC samples requires experienced laboratory personnel, isolated workstations, and sophisticated equipment, requires transport time, and involves complex procedures. We present a rapid DNA analysis system designed specifically to generate STR profiles from LDC samples in field-forward settings by non-technical operators. By performing STR in the field, close to the site of collection, rapid DNA analysis has the potential to increase throughput and to provide actionable information in real time. A Low DNA Content BioChipSet (LDC BCS) was developed and manufactured by injection molding. It was designed to function in the fully integrated Accelerated Nuclear DNA Equipment (ANDE) instrument previously designed for analysis of buccal swab and other high DNA content samples (Investigative Genet. 4(1):1-15, 2013). The LDC BCS performs efficient DNA purification followed by microfluidic ultrafiltration of the purified DNA, maximizing the quantity of DNA available for subsequent amplification and electrophoretic separation and detection of amplified fragments. The system demonstrates accuracy, precision, resolution, signal strength, and peak height ratios appropriate for casework analysis. The LDC rapid DNA analysis system is effective for the generation of STR profiles from a wide range of sample types. The technology broadens the range of sample

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.

Study on the determination of palladium in biological samples by the method of neutron activation analysis

International Nuclear Information System (INIS)

Cavalcante, Cassio Queiroz

2007-01-01

Palladium is one of platinum group elements present in the nature at very low concentrations. However with the use of this element in the automobile catalyzers Pd became a new pollutant. Besides, Pd has been studied in the preparation of new antitumour drugs. Consequently, there is a need to determine Pd concentrations in biological and environmental samples. This study presents palladium results obtained in the analysis of biological samples and reference materials using instrumental thermal and epithermal neutron activation analysis (INAA and ENAA). The solvent extraction and solid phase extraction separation methods were also applied before ENAA. The samples analyzed in this study were, reference material BCR 723 - Palladium, Platinum and Rhodium in road dust, CCQM-P63 automotive catalyst material of the Proficiency Test and bovine tissue samples containing palladium prepared in the laboratory. Samples and palladium synthetic standard were irradiated at the IEA-R1 nuclear research reactor under thermal neutron flux of about 4 x 10 12 n cm-2 s-1, during a period of 4 and 16 h for INAA and ENAA, respectively. The induced gamma activity of 109 Pd to the sample and standard was measured using a hyper pure Ge detector coupled to a gamma ray spectrometer. The palladium concentration was calculated by comparative method. The gamma ray energy of 109 Pd radioisotope measured was of 88.0 keV, located in a spectrum region of low energy where occurs the interference of X rays, 'Bremsstrahlung' radiations, as well as Compton effect of 24 Na. The pre-separation of palladium from interfering elements by solvent extraction was performed using dimethylglyoxime complexant and chloroform as diluent. In the case of the pre separation procedure using solid reversed phase column, the palladium was retained using N,N-diethyl-N'-benzoyl thiourea complexant and eluted using ethanol. Aliquots of the resulting solutions from the pre-separations, free of interfering elements, were

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

Energy Technology Data Exchange (ETDEWEB)

Brune, D; Sjoeberg, H E

1964-07-15

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

Analysis of PAH in soil samples

International Nuclear Information System (INIS)

Haeufel, J.; Weisweiler, W.

1994-01-01

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

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

International Nuclear Information System (INIS)

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

1997-10-01

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

Experience with conventional inelastic analysis procedures in very high temperature applications

International Nuclear Information System (INIS)

Mallett, R.H.; Thompson, J.M.; Swindeman, R.W.

1991-01-01

Conventional incremental plasticity and creep analysis procedures for inelastic analysis are applied to hot flue gas cleanup system components. These flue gas systems operate at temperatures where plasticity and creep are very much intertwined while the two phenomena are treated separately in the conventional inelastic analysis procedure. Data for RA333 material are represented in forms appropriate for the conventional inelastic analysis procedures. Behavior is predicted for typical operating cycles. Creep-fatigue damage is estimated based upon usage fractions. Excessive creep damage is predicted; the major contributions occur during high stress short term intervals caused by rapid temperature changes. In this paper these results are presented for discussion of the results and their interpretation in terms of creep-fatigue damage for very high temperature applications

Nevada Applied Ecology Group procedures handbook for environmental transuranics

International Nuclear Information System (INIS)

White, M.G.; Dunaway, P.B.

1976-10-01

The activities of the Nevada Applied Ecology Group (NAEG) integrated research studies of environmental plutonium and other transuranics at the Nevada Test Site have required many standardized field and laboratory procedures. These include sampling techniques, collection and preparation, radiochemical and wet chemistry analysis, data bank storage and reporting, and statistical considerations for environmental samples of soil, vegetation, resuspended particles, animals, and other biological material. This document, printed in two volumes, includes most of the Nevada Applied Ecology Group standard procedures, with explanations as to the specific applications involved in the environmental studies. Where there is more than one document concerning a procedure, it has been included to indicate special studies or applications more complex than the routine standard sampling procedures utilized

Nevada Applied Ecology Group procedures handbook for environmental transuranics

International Nuclear Information System (INIS)

White, M.G.; Dunaway, P.B.

1976-10-01

The activities of the Nevada Applied Ecology Group (NAEG) integrated research studies of environmental plutonium and other transuranics at the Nevada Test Site have required many standardized field and laboratory procedures. These include sampling techniques, collection and preparation, radiochemical and wet chemistry analysis, data bank storage and reporting, and statistical considerations for environmental samples of soil, vegetation, resuspended particles, animals, and others. This document, printed in two volumes, includes most of the Nevada Applied Ecology Group standard procedures, with explanations as to the specific applications involved in the environmental studies. Where there is more than one document concerning a procedure, it has been included to indicate special studies or applications perhaps more complex than the routine standard sampling procedures utilized

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)

Mercury and gold concentrations of highly polluted environmental samples determined using prompt gamma-ray analysis and instrument neutron activation analysis

Science.gov (United States)

Osawa, Takahito; Hatsukawa, Yuichi; Appel, Peter W. U.; Matsue, Hideaki

2011-04-01

The authors have established a method of determining mercury and gold in severely polluted environmental samples using prompt gamma-ray analysis (PGA) and instrumental neutron activation analysis (INAA). Since large amounts of mercury are constantly being released into the environment by small-scale gold mining in many developing countries, the mercury concentration in tailings and water has to be determined to mitigate environmental pollution. Cold-vapor atomic absorption analysis, the most pervasive method of mercury analysis, is not suitable because tailings and water around mining facilities have extremely high mercury concentrations. On the other hand, PGA can determine high mercury concentrations in polluted samples as it has an appropriate level of sensitivity. Moreover, gold concentrations can be determined sequentially by using INAA after PGA. In conclusion, the analytical procedure established in this work using PGA and INAA is the best way to evaluate the degree of pollution and the tailing resource value. This method will significantly contribute to mitigating problems in the global environment.

Mercury and gold concentrations of highly polluted environmental samples determined using prompt gamma-ray analysis and instrument neutron activation analysis

International Nuclear Information System (INIS)

Osawa, Takahito; Hatsukawa, Yuichi; Appel, Peter W.U.; Matsue, Hideaki

2011-01-01

The authors have established a method of determining mercury and gold in severely polluted environmental samples using prompt gamma-ray analysis (PGA) and instrumental neutron activation analysis (INAA). Since large amounts of mercury are constantly being released into the environment by small-scale gold mining in many developing countries, the mercury concentration in tailings and water has to be determined to mitigate environmental pollution. Cold-vapor atomic absorption analysis, the most pervasive method of mercury analysis, is not suitable because tailings and water around mining facilities have extremely high mercury concentrations. On the other hand, PGA can determine high mercury concentrations in polluted samples as it has an appropriate level of sensitivity. Moreover, gold concentrations can be determined sequentially by using INAA after PGA. In conclusion, the analytical procedure established in this work using PGA and INAA is the best way to evaluate the degree of pollution and the tailing resource value. This method will significantly contribute to mitigating problems in the global environment.

Atmospheric Deposition: Sampling Procedures, Analytical Methods, and Main Recent Findings from the Scientific Literature

Directory of Open Access Journals (Sweden)

M. Amodio

2014-01-01

Full Text Available The atmosphere is a carrier on which some natural and anthropogenic organic and inorganic chemicals are transported, and the wet and dry deposition events are the most important processes that remove those chemicals, depositing it on soil and water. A wide variety of different collectors were tested to evaluate site-specificity, seasonality and daily variability of settleable particle concentrations. Deposition fluxes of POPs showed spatial and seasonal variations, diagnostic ratios of PAHs on deposited particles, allowed the discrimination between pyrolytic or petrogenic sources. Congener pattern analysis and bulk deposition fluxes in rural sites confirmed long-range atmospheric transport of PCDDs/Fs. More and more sophisticated and newly designed deposition samplers have being used for characterization of deposited mercury, demonstrating the importance of rain scavenging and the relatively higher magnitude of Hg deposition from Chinese anthropogenic sources. Recently biological monitors demonstrated that PAH concentrations in lichens were comparable with concentrations measured in a conventional active sampler in an outdoor environment. In this review the authors explore the methodological approaches used for the assessment of atmospheric deposition, from the analysis of the sampling methods, the analytical procedures for chemical characterization of pollutants and the main results from the scientific literature.

The computer system for the express-analysis of the irradiation samples

International Nuclear Information System (INIS)

Vzorov, I.K.; Kalmykov, A.V.; Korenev, S.A.; Minashkin, V.F.; Sikolenko, V.V.

1999-01-01

The computer system for the express-analysis (SEA) of the irradiation samples is described. The system is working together with the pulse high current electrons and ions source. It allows us to correct irradiation regime in real time. The SEA system automatically measures volt-ampere and volt-farad characteristics, sample resistance by 'four-probe' method, sample capacitor parameters. Its parameters are: in the volt-ampere measuring regime - U max = 200 V, minimal voltage step U sh =0.05 V, voltage accuracy 0.25%; in the capacity measuring regime - capacity measurement diapason 0 - 1600 pF, working frequencies diapason 1 -150 kHz, capacity accuracy 0.5%, voltage shifting diapason 1 - 200 V, minimal step of voltage shifting U sh 0.05 V. The SEA management is performed by IBM/AT computer. The control and measuring apparatus was realized in CAMAC standard. The programmed set consists of the first display procedures, control, treatment and information exit. (author)

Meta-analysis of the technical performance of an imaging procedure: guidelines and statistical methodology.

Science.gov (United States)

Huang, Erich P; Wang, Xiao-Feng; Choudhury, Kingshuk Roy; McShane, Lisa M; Gönen, Mithat; Ye, Jingjing; Buckler, Andrew J; Kinahan, Paul E; Reeves, Anthony P; Jackson, Edward F; Guimaraes, Alexander R; Zahlmann, Gudrun

2015-02-01

Medical imaging serves many roles in patient care and the drug approval process, including assessing treatment response and guiding treatment decisions. These roles often involve a quantitative imaging biomarker, an objectively measured characteristic of the underlying anatomic structure or biochemical process derived from medical images. Before a quantitative imaging biomarker is accepted for use in such roles, the imaging procedure to acquire it must undergo evaluation of its technical performance, which entails assessment of performance metrics such as repeatability and reproducibility of the quantitative imaging biomarker. Ideally, this evaluation will involve quantitative summaries of results from multiple studies to overcome limitations due to the typically small sample sizes of technical performance studies and/or to include a broader range of clinical settings and patient populations. This paper is a review of meta-analysis procedures for such an evaluation, including identification of suitable studies, statistical methodology to evaluate and summarize the performance metrics, and complete and transparent reporting of the results. This review addresses challenges typical of meta-analyses of technical performance, particularly small study sizes, which often causes violations of assumptions underlying standard meta-analysis techniques. Alternative approaches to address these difficulties are also presented; simulation studies indicate that they outperform standard techniques when some studies are small. The meta-analysis procedures presented are also applied to actual [18F]-fluorodeoxyglucose positron emission tomography (FDG-PET) test-retest repeatability data for illustrative purposes. © The Author(s) 2014 Reprints and permissions: sagepub.co.uk/journalsPermissions.nav.

A novel solid phase extraction procedure on Amberlite XAD-1180 for speciation of Cr(III), Cr(VI) and total chromium in environmental and pharmaceutical samples

International Nuclear Information System (INIS)

Narin, Ibrahim; Kars, Ayse; Soylak, Mustafa

2008-01-01

Due to the toxicity of chromium, species depend on their chemical properties and bioavailabilities, speciation of chromium is very important in environmental samples. A speciation procedure for chromium(III), chromium(VI) and total chromium in environmental samples is presented in this work, prior to flame atomic absorption spectrometric determination of chromium. The procedure is based on the adsorption of Cr(III)-diphenylcarbazone complex on Amberlite XAD-1180 resin. After oxidation of Cr(III), the developed solid phase extraction system was applied to determinate the total chromium. Cr(III) was calculated as the difference between the total Cr content and the Cr(VI) content. The analytical conditions for the quantitative recoveries of Cr(VI) on Amberlite XAD-1180 resin were investigated. The effects of some alkaline, earth alkaline, metal ions and also some anions were also examined. Preconcentration factor was found to be 75. The detection limits (LOD) based on three times sigma of the blank (N: 21) for Cr(VI) and total chromium were 7.7 and 8.6 μg/L, respectively. Satisfactory results for the analysis of total chromium in the stream sediment (GBW7310) certified reference material for the validation of the presented method was obtained. The procedure was applied to food, water and pharmaceutical samples successfully

A simple cleanup method for the isolation of nitrate from natural water samples for O isotopes analysis

International Nuclear Information System (INIS)

Haberhauer, G.; Blochberger, K.

1999-09-01

The analysis of O-isotopic composition of nitrate has many potential applications in studies of environmental processes. O-isotope nitrate analysis require sample free of other oxygen-containing compounds. More than 100 % of non-NO 3 - oxygen relative to NO 3 - oxygen can still be found in forest soil water samples after cleanup if improper cleanup strategies, e.g., adsorption onto activated carbon, are used. Such non-NO 3 - oxygen compounds will bias O-isotropic data. Therefore, an efficient cleanup method was developed to isolate nitrate from natural water samples. In a multistep cleanup procedure using adsorption onto water-insoluble poly(vinylpyrrolidone), removal of almost all other oxygen-containing compounds, such as fulvic acids, and isolation of nitrate was achieved. The method supplied samples free of non-NO 3 - oxygen which can be directly combusted to CO 2 for subsequent O-isotope analysis. (author)

Sampling and analysis validates acceptable knowledge on LANL transuranic, heterogeneous, debris waste, or ''Cutting the Gordian knot that binds WIPP''

International Nuclear Information System (INIS)

Kosiewicz, S.T.; Triay, I.R.; Souza, L.A.

1999-01-01

Through sampling and toxicity characteristic leaching procedure (TCLP) analyses, LANL and the DOE validated that a LANL transuranic (TRU) waste (TA-55-43, Lot No. 01) was not a Resource Recovery and Conservation Act (RCRA) hazardous waste. This paper describes the sampling and analysis project as well as the statistical assessment of the analytical results. The analyses were conducted according to the requirements and procedures in the sampling and analysis plan approved by the New Mexico Environmental Department. The plan used a statistical approach that was consistent with the stratified, random sampling requirements of SW-846. LANL adhered to the plan during sampling and chemical analysis of randomly selected items of the five major types of materials in this heterogeneous, radioactive, debris waste. To generate portions of the plan, LANL analyzed a number of non-radioactive items that were representative of the mix of items present in the waste stream. Data from these cold surrogates were used to generate means and variances needed to optimize the design. Based on statistical arguments alone, only two samples from the entire waste stream were deemed necessary, however a decision was made to analyze at least two samples of each of the five major waste types. To obtain these samples, nine TRU waste drums were opened. Sixty-six radioactively contaminated and four non-radioactive grab samples were collected. Portions of the samples were composited for chemical analyses. In addition, a radioactively contaminated sample of rust-colored powder of interest to the New Mexico Environment Department (NMED) was collected and qualitatively identified as rust

Cost analysis of robotic versus laparoscopic general surgery procedures.

Science.gov (United States)

Higgins, Rana M; Frelich, Matthew J; Bosler, Matthew E; Gould, Jon C

2017-01-01

Robotic surgical systems have been used at a rapidly increasing rate in general surgery. Many of these procedures have been performed laparoscopically for years. In a surgical encounter, a significant portion of the total costs is associated with consumable supplies. Our hospital system has invested in a software program that can track the costs of consumable surgical supplies. We sought to determine the differences in cost of consumables with elective laparoscopic and robotic procedures for our health care organization. De-identified procedural cost and equipment utilization data were collected from the Surgical Profitability Compass Procedure Cost Manager System (The Advisory Board Company, Washington, DC) for our health care system for laparoscopic and robotic cholecystectomy, fundoplication, and inguinal hernia between the years 2013 and 2015. Outcomes were length of stay, case duration, and supply cost. Statistical analysis was performed using a t-test for continuous variables, and statistical significance was defined as p robotic procedures. Length of stay did not differ for fundoplication or cholecystectomy. Length of stay was greater for robotic inguinal hernia repair. Case duration was similar for cholecystectomy (84.3 robotic and 75.5 min laparoscopic, p = 0.08), but significantly longer for robotic fundoplication (197.2 robotic and 162.1 min laparoscopic, p = 0.01) and inguinal hernia repair (124.0 robotic and 84.4 min laparoscopic, p = ≪0.01). We found a significantly increased cost of general surgery procedures for our health care system when cases commonly performed laparoscopically are instead performed robotically. Our analysis is limited by the fact that we only included costs associated with consumable surgical supplies. The initial acquisition cost (over $1 million for robotic surgical system), depreciation, and service contract for the robotic and laparoscopic systems were not included in this analysis.

Building America House Performance Analysis Procedures

Energy Technology Data Exchange (ETDEWEB)

Hendron, R.; Farrar-Nagy, S.; Anderson, R.; Judkoff, R.

2001-10-29

As the Building America Program has grown to include a large and diverse cross section of the home building industry, accurate and consistent analysis techniques have become more important to help all program partners as they perform design tradeoffs and calculate energy savings for prototype houses built as part of the program. This document illustrates some of the analysis concepts proven effective and reliable for analyzing the transient energy usage of advanced energy systems as well as entire houses. The analysis procedure described here provides a starting point for calculating energy savings of a prototype house relative to two base cases: builder standard practice and regional standard practice. Also provides building simulation analysis to calculate annual energy savings based on side-by-side short-term field testing of a prototype house.

Comparative analysis of lockout programs and procedures applied to industrial machines

Energy Technology Data Exchange (ETDEWEB)

Chinniah, Y.; Champoux, M.; Burlet-Vienney, D.; Daigle, R. [Institut de recherche Robert-Sauve en sante et en securite du travail, Montreal, PQ (Canada)

2008-09-15

In 2005, approximately 20 workers in Quebec were killed by dangerous machines. Approximately 13,000 accidents in the province were linked to the use of machines. The resulting cost associated with these accidents was estimated to be $70 million to the Quebec Occupational Health and Safety Commission (CSST) in compensation and salary replacement. According to article 185 of the Quebec Occupational Health and Safety Regulation (RSST), workers intervening in hazardous zones of machines and processes during maintenance, repairs, and unjamming activities must apply lockout procedures. Lockout is defined as the placement of a lock or tag on an energy-isolating device in accordance with an established procedure, indicating that the energy-isolating device is not to be operated until removal of the lock or tag in accordance with an established procedure. This report presented a comparative analysis of lockout programs and procedures applied to industrial machines. The study attempted to answer several questions regarding the concept of lockout and its definition in the literature; the differences between legal lockout requirements among provinces and countries; different standards on lockout; the contents of lockout programs as described by different documents; and the compliance of lockout programs in a sample of industries in Quebec in terms of Canadian standard on lockout, the CSA Z460-05 (2005). The report discussed the research objectives, methodology, and results of the study. It was concluded that the concept of lockout has different meanings or definitions in the literature, especially in regulations. However, definitions of lockout which are found in standards have certain similarities. 50 refs., 52 tabs., 2 appendices.

The principles, procedures and pitfalls in identifying archaeological and historical wood samples.

Science.gov (United States)

Cartwright, Caroline R

2015-07-01

The science of wood anatomy has evolved in recent decades to add archaeological and historical wood to its repertoire of documenting and characterizing modern and fossil woods. The increasing use of online wood anatomy databases and atlases has fostered the adoption of an international consensus regarding terminology, largely through the work of the International Association of Wood Anatomists (IAWA). This review presents an overview for the general reader of the current state of principles and procedures involved in the study of the wood anatomy of archaeological and historical specimens, some of which may be preserved through charring, waterlogging, desiccation or mineral replacement. By means of selected case studies, the review evaluates to what extent varying preservation of wood anatomical characteristics limits the level of identification to taxon. It assesses the role played by increasingly accessible scanning electron microscopes and complex optical microscopes, and whether these, on the one hand, provide exceptional opportunities for high-quality imaging and analysis of difficult samples, but, on the other hand, might be misleading the novice into thinking that advanced technology can be a substitute for specialized botanical training in wood anatomy. © The Author 2015. Published by Oxford University Press on behalf of the Annals of Botany Company. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Optimization of procedures for mercury-203 instrumental neutron activation analysis in human urine

Energy Technology Data Exchange (ETDEWEB)

Blotcky, A J; Claassen, J P [Nebraska Univ., Omaha, NE (United States). Medical Center; Fung, Y K [Nebraska Univ., Lincoln, NE (United States). Dept. of Chemistry; Meade, A G; Rack, E P [Nebraska Univ., Lincoln, NE (United States)

1995-08-01

Mercury, a known neurotoxin, has been implicated in etiology and pathogenesis of such disease states as Alzheimer`s and Parkinson`s diseases. There is concern that the exposure to mercury vapor released from dental amalgam restorations is a potential health hazard. Measurement of mercury concentrations in blood or urine may be useful in diagnosis of mercury poisoning and in assessing the extent exposure. This study describes the optimization of pre-neutron activation analysis procedures such as sampling, selection of irradiation and counting vials and acid digestion in order to minimize mercury loss via volatilization and/or permeation through containers. Therefore, the determination of mercury can be complicated by these potential losses. In the optimized procedure 20mL of urine was spiked with three different concentrations of mercury, digested with concentrated nitric acid, and placed in polypropylene vials for irradiation and counting. Analysis was performed by subtracting the Se-75 photopeak contribution to the 279 keV Hg-203 photopeak and applying the method of standard additions. Urinary mercury concentrations in normal human subjects were determined to be of the order of 10ng/mL. (author). 22 refs., 1 fig., 5 tabs.

Optimization of procedures for mercury-203 instrumental neutron activation analysis in human urine

International Nuclear Information System (INIS)

Blotcky, A.J.; Claassen, J.P.

1995-01-01

Mercury, a known neurotoxin, has been implicated in etiology and pathogenesis of such disease states as Alzheimer's and Parkinson's diseases. There is concern that the exposure to mercury vapor released from dental amalgam restorations is a potential health hazard. Measurement of mercury concentrations in blood or urine may be useful in diagnosis of mercury poisoning and in assessing the extent exposure. This study describes the optimization of pre-neutron activation analysis procedures such as sampling, selection of irradiation and counting vials and acid digestion in order to minimize mercury loss via volatilization and/or permeation through containers. Therefore, the determination of mercury can be complicated by these potential losses. In the optimized procedure 20mL of urine was spiked with three different concentrations of mercury, digested with concentrated nitric acid, and placed in polypropylene vials for irradiation and counting. Analysis was performed by subtracting the Se-75 photopeak contribution to the 279 keV Hg-203 photopeak and applying the method of standard additions. Urinary mercury concentrations in normal human subjects were determined to be of the order of 10ng/mL. (author). 22 refs., 1 fig., 5 tabs

Sample-size effects in fast-neutron gamma-ray production measurements: solid-cylinder samples

International Nuclear Information System (INIS)

Smith, D.L.

1975-09-01

The effects of geometry, absorption and multiple scattering in (n,Xγ) reaction measurements with solid-cylinder samples are investigated. Both analytical and Monte-Carlo methods are employed in the analysis. Geometric effects are shown to be relatively insignificant except in definition of the scattering angles. However, absorption and multiple-scattering effects are quite important; accurate microscopic differential cross sections can be extracted from experimental data only after a careful determination of corrections for these processes. The results of measurements performed using several natural iron samples (covering a wide range of sizes) confirm validity of the correction procedures described herein. It is concluded that these procedures are reliable whenever sufficiently accurate neutron and photon cross section and angular distribution information is available for the analysis. (13 figures, 5 tables) (auth)

Sample preparation: a critical step in the analysis of cholesterol oxidation products.

Science.gov (United States)

Georgiou, Christiana A; Constantinou, Michalis S; Kapnissi-Christodoulou, Constantina P

2014-02-15

In recent years, cholesterol oxidation products (COPs) have drawn scientific interest, particularly due to their implications on human health. A big number of these compounds have been demonstrated to be cytotoxic, mutagenic, and carcinogenic. The main source of COPs is through diet, and particularly from the consumption of cholesterol-rich foods. This raises questions about the safety of consumers, and it suggests the necessity for the development of a sensitive and a reliable analytical method in order to identify and quantify these components in food samples. Sample preparation is a necessary step in the analysis of COPs in order to eliminate interferences and increase sensitivity. Numerous publications have, over the years, reported the use of different methods for the extraction and purification of COPs. However, no method has, so far, been established as a routine method for the analysis of COPs in foods. Therefore, it was considered important to overview different sample preparation procedures and evaluate the different preparative parameters, such as time of saponification, the type of organic solvents for fat extraction, the stationary phase in solid phase extraction, etc., according to recovery, precision and simplicity. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-11-30

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

Determination of Initial Conditions for the Safety Analysis by Random Sampling of Operating Parameters

International Nuclear Information System (INIS)

Jeong, Hae-Yong; Park, Moon-Ghu

2015-01-01

In most existing evaluation methodologies, which follow a conservative approach, the most conservative initial conditions are searched for each transient scenario through tremendous assessment for wide operating windows or limiting conditions for operation (LCO) allowed by the operating guidelines. In this procedure, a user effect could be involved and a remarkable time and human resources are consumed. In the present study, we investigated a more effective statistical method for the selection of the most conservative initial condition by the use of random sampling of operating parameters affecting the initial conditions. A method for the determination of initial conditions based on random sampling of plant design parameters is proposed. This method is expected to be applied for the selection of the most conservative initial plant conditions in the safety analysis using a conservative evaluation methodology. In the method, it is suggested that the initial conditions of reactor coolant flow rate, pressurizer level, pressurizer pressure, and SG level are adjusted by controlling the pump rated flow, setpoints of PLCS, PPCS, and FWCS, respectively. The proposed technique is expected to contribute to eliminate the human factors introduced in the conventional safety analysis procedure and also to reduce the human resources invested in the safety evaluation of nuclear power plants

Procedure for statistical analysis of one-parameter discrepant experimental data

International Nuclear Information System (INIS)

Badikov, Sergey A.; Chechev, Valery P.

2012-01-01

A new, Mandel–Paule-type procedure for statistical processing of one-parameter discrepant experimental data is described. The procedure enables one to estimate a contribution of unrecognized experimental errors into the total experimental uncertainty as well as to include it in analysis. A definition of discrepant experimental data for an arbitrary number of measurements is introduced as an accompanying result. In the case of negligible unrecognized experimental errors, the procedure simply reduces to the calculation of the weighted average and its internal uncertainty. The procedure was applied to the statistical analysis of half-life experimental data; Mean half-lives for 20 actinides were calculated and results were compared to the ENSDF and DDEP evaluations. On the whole, the calculated half-lives are consistent with the ENSDF and DDEP evaluations. However, the uncertainties calculated in this work essentially exceed the ENSDF and DDEP evaluations for discrepant experimental data. This effect can be explained by adequately taking into account unrecognized experimental errors. - Highlights: ► A new statistical procedure for processing one-parametric discrepant experimental data has been presented. ► Procedure estimates a contribution of unrecognized errors in the total experimental uncertainty. ► Procedure was applied for processing half-life discrepant experimental data. ► Results of the calculations are compared to the ENSDF and DDEP evaluations.

Determination of thiobencarb in water samples by gas chromatography using a homogeneous liquid-liquid microextraction via flotation assistance procedure

Directory of Open Access Journals (Sweden)

H.A. Mashayekhi

2013-09-01

Full Text Available Homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA coupled with gas chromatography-flame ionization detection (GC-FID was applied for the extraction and determination of thiobencarb in water samples. In this study, a special extraction cell was designed to facilitate collection of the low-density solvent extraction. No centrifugation was required in this procedure. The water sample solution was added into the extraction cell which contained an appropriate mixture of toluene (as an extraction solvent and acetone (as a homogeneous solvent. By using air flotation, the organic solvent was collected at the conical part of the designed cell. The effect of the different parameters on the efficiency of extraction such as type and volume of extraction and homogeneous solvents, ionic strength and extraction time were studied and optimized. Under the optimal conditions, linearity of the method was in the range of 1.0-200 µg L-1. The relative standard deviations in the real samples varied from 7.8-11.7 % (n = 3. The proposed method was successfully applied to analysis of thiobencarb in the water samples and satisfactory results were obtained.DOI: http://dx.doi.org/10.4314/bcse.v27i3.4

Formalizing the Austrian Procedure Catalogue: A 4-step methodological analysis approach.

Science.gov (United States)

Neururer, Sabrina Barbara; Lasierra, Nelia; Peiffer, Karl Peter; Fensel, Dieter

2016-04-01

Due to the lack of an internationally accepted and adopted standard for coding health interventions, Austria has established its own country-specific procedure classification system - the Austrian Procedure Catalogue (APC). Even though the APC is an elaborate coding standard for medical procedures, it has shortcomings that limit its usability. In order to enhance usability and usefulness, especially for research purposes and e-health applications, we developed an ontologized version of the APC. In this paper we present a novel four-step approach for the ontology engineering process, which enables accurate extraction of relevant concepts for medical ontologies from written text. The proposed approach for formalizing the APC consists of the following four steps: (1) comparative pre-analysis, (2) definition analysis, (3) typological analysis, and (4) ontology implementation. The first step contained a comparison of the APC to other well-established or elaborate health intervention coding systems in order to identify strengths and weaknesses of the APC. In the second step, a list of definitions of medical terminology used in the APC was obtained. This list of definitions was used as input for Step 3, in which we identified the most important concepts to describe medical procedures using the qualitative typological analysis approach. The definition analysis as well as the typological analysis are well-known and effective methods used in social sciences, but not commonly employed in the computer science or ontology engineering domain. Finally, this list of concepts was used in Step 4 to formalize the APC. The pre-analysis highlighted the major shortcomings of the APC, such as the lack of formal definition, leading to implicitly available, but not directly accessible information (hidden data), or the poor procedural type classification. After performing the definition and subsequent typological analyses, we were able to identify the following main characteristics of

Soil sample collection and analysis for the Fugitive Dust Characterization Study

Science.gov (United States)

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

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

On the development of automatic sample preparation devices

International Nuclear Information System (INIS)

Oesselmann, J.

1987-01-01

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

Procedures for conducting common cause failure analysis in probabilistic safety assessment

International Nuclear Information System (INIS)

1992-05-01

The principal objective of this report is to supplement the procedure developed in Mosleh et al. (1988, 1989) by providing more explicit guidance for a practical approach to common cause failures (CCF) analysis. The detailed CCF analysis following that procedure would be very labour intensive and time consuming. This document identifies a number of options for performing the more labour intensive parts of the analysis in an attempt to achieve a balance between the need for detail, the purpose of the analysis and the resources available. The document is intended to be compatible with the Agency's Procedures for Conducting Probabilistic Safety Assessments for Nuclear Power Plants (IAEA, 1992), but can be regarded as a stand-alone report to be used in conjunction with NUREG/CR-4780 (Mosleh et al., 1988, 1989) to provide additional detail, and discussion of key technical issues

Drawing up of a procedure for vanadium determination in mussels using the neutron activation analysis method

International Nuclear Information System (INIS)

Seo, Daniele; Vasconcellos, Marina B.A.; Saiki, Mitiko; Catharino, Marilia G.M.; Moreira, Edson G.; Sousa, Eduinetty C.P.M. de; Pereira, Camilo D.S.

2009-01-01

This work establishes an adequate procedure for obtaining reliable results for determination of vanadium in mussels, leg by leg by the neutron activation analysis (NAA), viewing the posterior application on the bio monitoring the coastal pollution, particularly near the petroleum terminals.For the evaluation of result quality concerning to the quality of those results, the work analysed the reference material certification NIST SRM 1566b Oyster Tissue. The precision of the results were also analysed using repetitions of mussel samples collected at the coastal of northern Sao Paulo state, Brazil. The NAA procedure consisted of 200 mg of sample and a synthetic standard of vanadium during a period of 8 s and under a thermal neutron flux of 6.6 x 10 12 n cm -2 s -1 at the pneumatic station 4 of the IEA-R1 nuclear reactor of IPEN-CNEN/SP. After a 3 min decay, the measurements of the gamma activities of the sample and the standard were done using a Ge hyper pure semi-conductor detector, connected to gamma ray multichannel analyser. The vanadium were determined by the measurement of the gamma activity of the 52 V through the 1434.08 keV peak, and half-life time of 3.75 min. The concentration of V were calculated by the comparative method. The obtained results indicated the viability of the NAA procedure established for the determination of vanadium in mussels

Optimizing sample pretreatment for compound-specific stable carbon isotopic analysis of amino sugars in marine sediment

Science.gov (United States)

Zhu, R.; Lin, Y.-S.; Lipp, J. S.; Meador, T. B.; Hinrichs, K.-U.

2014-09-01

Amino sugars are quantitatively significant constituents of soil and marine sediment, but their sources and turnover in environmental samples remain poorly understood. The stable carbon isotopic composition of amino sugars can provide information on the lifestyles of their source organisms and can be monitored during incubations with labeled substrates to estimate the turnover rates of microbial populations. However, until now, such investigation has been carried out only with soil samples, partly because of the much lower abundance of amino sugars in marine environments. We therefore optimized a procedure for compound-specific isotopic analysis of amino sugars in marine sediment, employing gas chromatography-isotope ratio mass spectrometry. The whole procedure consisted of hydrolysis, neutralization, enrichment, and derivatization of amino sugars. Except for the derivatization step, the protocol introduced negligible isotopic fractionation, and the minimum requirement of amino sugar for isotopic analysis was 20 ng, i.e., equivalent to ~8 ng of amino sugar carbon. Compound-specific stable carbon isotopic analysis of amino sugars obtained from marine sediment extracts indicated that glucosamine and galactosamine were mainly derived from organic detritus, whereas muramic acid showed isotopic imprints from indigenous bacterial activities. The δ13C analysis of amino sugars provides a valuable addition to the biomarker-based characterization of microbial metabolism in the deep marine biosphere, which so far has been lipid oriented and biased towards the detection of archaeal signals.

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

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.

Quantitative analysis of detailed lignin monomer composition by pyrolysis-gas chromatography combined with preliminary acetylation of the samples.

Science.gov (United States)

Sonoda, T; Ona, T; Yokoi, H; Ishida, Y; Ohtani, H; Tsuge, S

2001-11-15

Detailed quantitative analysis of lignin monomer composition comprising p-coumaryl, coniferyl, and sinapyl alcohol and p-coumaraldehyde, coniferaldehyde, and sinapaldehyde in plant has not been studied from every point mainly because of artifact formation during the lignin isolation procedure, partial loss of the lignin components inherent in the chemical degradative methods, and difficulty in the explanation of the complex spectra generally observed for the lignin components. Here we propose a new method to quantify lignin monomer composition in detail by pyrolysis-gas chromatography (Py-GC) using acetylated lignin samples. The lignin acetylation procedure would contribute to prevent secondary formation of cinnamaldehydes from the corresponding alcohol forms during pyrolysis, which are otherwise unavoidable in conventional Py-GC process to some extent. On the basis of the characteristic peaks on the pyrograms of the acetylated sample, lignin monomer compositions in various dehydrogenative polymers (DHP) as lignin model compounds were determined, taking even minor components such as cinnamaldehydes into consideration. The observed compositions by Py-GC were in good agreement with the supplied lignin monomer contents on DHP synthesis. The new Py-GC method combined with sample preacetylation allowed us an accurate quantitative analysis of detailed lignin monomer composition using a microgram order of extractive-free plant samples.

Trace aluminium determination and sampling problems of archeological bone employing destructive neutron activation analysis

International Nuclear Information System (INIS)

Blotcky, A.J.; Rack, E.P.; Recker, R.R.; Leffler, J.A.; Teitelbaum, S.

1978-01-01

A destructive neutron activation analysis procedure was developed for determining trace aluminium content in bone. The method is based on a carefully planned sample preparation, irradiation at a neutron flux for 3.1x10 11 nxcm -2 xs -1 for 5 minutes, and chemical separation based on ion exchange. It was found that bone samples soaked in aluminium containing soil gave highly elevated aluminium values as a result of the aluminium adsorption into the bone matrix. The maximum aluminium content values for prehistoric bones are larger than those of modern bones and comparable to aluminium levels present in bone from renal patients. (T.G.)

Recommended procedures for performance testing of radiobioassay laboratories: Volume 2, In vitro samples

International Nuclear Information System (INIS)

Fenrick, H.W.; MacLellan, J.A.

1988-11-01

Draft American National Standards Institute (ANSI) Standard N13.30 (Performance Criteria for Radiobioassay) was developed for the US Department of Energy and the US Nuclear Regulatory Commission to help ensure that bioassay laboratories provide accurate and consistent results. The draft standard specifies the criteria for defining the procedures necessary to establish a bioassay performance-testing laboratory and program. The bioassay testing laboratory will conduct tests to evaluate the performance of service laboratories. Pacific Northwest Laboratory helped develop testing procedures as part of an effort to evaluate the performance criteria by testing the existing measurement capabilities of various bioassay laboratories. This report recommends guidelines for the preparation, handling, storage, distribution, shipping, and documentation of in vitro test samples (artificial urine and fecal matter) for indirect bioassay. The data base and recommended records system for documenting radiobioassay performance at the service laboratories are also presented. 8 refs., 3 tabs

Comparative analysis of diagnostic accuracy of different brain biopsy procedures

OpenAIRE

Jain Deepali; Sharma Mehar; Sarkar Chitra; Gupta Deepak; Singh Manmohan; Mahapatra A

2006-01-01

Background: Image-guided procedures such as computed tomography (CT) guided, neuronavigator-guided and ultrasound-guided methods can assist neurosurgeons in localizing the intraparenchymal lesion of the brain. However, despite improvements in the imaging techniques, an accurate diagnosis of intrinsic lesion requires tissue sampling and histological verification. Aims: The present study was carried out to examine the reliability of the diagnoses made on tumor sample obtained via different s...

Prospects for the introduction of Wide Area Monitoring Using Environmental Sampling

International Nuclear Information System (INIS)

Wogman, N.A.

2013-01-01

Nuclear proliferation signatures released to the environment must be collected and distinguished from primordial and man-made backgrounds in soils, sediments, air, and surface and underground water. The delay time between the nuclear proliferation emissions and the date of the Wide-Area Environmental Sampling (WAES) analysis will determine which radionuclides would be analyzed based upon their half-lives. Various sampling and analysis technologies have been considered here for application to a WAES. Sampling procedures and equipment discussed are aimed at aquatic, airborne particulate, gas, vegetation, sediment and/or soil, and fauna media. Specific procedures must be selected based upon the application scenario; for example, sampling in the northern latitudes under freezing conditions, sampling at the equator under tropical rain-forest conditions, sampling in the mid-latitudes under desert conditions, and sampling in the marine environment require different equipment and procedures. The paper is followed by the slides of the presentation

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

International Nuclear Information System (INIS)

Takahashi, Masato; Magara, Masaaki; Sakurai, Satoshi

2002-01-01

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

40 CFR 257.23 - Ground-water sampling and analysis requirements.

Science.gov (United States)

2010-07-01

...: (1) Sample collection; (2) Sample preservation and shipment; (3) Analytical procedures; (4) Chain of... theory test, then the data should be transformed or a distribution-free theory test should be used. If... chart and its associated parameter values shall be protective of human health and the environment. The...

Application of human error theory in case analysis of wrong procedures.

Science.gov (United States)

Duthie, Elizabeth A

2010-06-01

The goal of this study was to contribute to the emerging body of literature about the role of human behaviors and cognitive processes in the commission of wrong procedures. Case analysis of 5 wrong procedures in operative and nonoperative settings using James Reason's human error theory was performed. The case analysis showed that cognitive underspecification, cognitive flips, automode processing, and skill-based errors were contributory to wrong procedures. Wrong-site procedures accounted for the preponderance of the cases. Front-line supervisory staff used corrective actions that focused on the performance of the individual without taking into account cognitive factors. System fixes using human cognition concepts have a greater chance of achieving sustainable safety outcomes than those that are based on the traditional approach of counseling, education, and disciplinary action for staff.

Effect of microbiological testing on subsequent mid-infrared milk component analysis of the same milk sample.

Science.gov (United States)

Wojciechowski, Karen L; Melilli, Caterina; Barbano, David M

2014-09-01

Our objectives were to determine if mixing and sampling of a raw milk sample at 4°C for determination of total bacteria count (TBC) and if incubation at 14°C for 18h and sampling for a preliminary incubation (PI) count influenced the accuracy of subsequent fat, protein, or lactose measurement by mid-infrared (IR) analysis of milk from the same sample container due to either nonrepresentative sampling or the presence of microbial metabolites produced by microbial growth in the milk from the incubation. Milks of 4 fat levels (2.2, 3, 4, and 5%) reflected the range of fat levels encountered in producer milks. If the portion of milk removed from a cold sample was not representative, then the effect on a milk component test would likely be larger as fat content increases. Within the milks at each fat level, 3 treatments were used: (1) 20 vials of the same milk sampled for testing TBC using a BactoScan FC and then used for a milk component test; (2) 20 vials for testing TBC plus PI count followed by component test; and (3) 20 vials to run for IR component test without a prior micro sampling and testing. This was repeated in 3 different weeks using a different batch of milk each week. No large effect on the accuracy of component milk testing [IR fat B (carbon hydrogen stretch) and fat A (carbonyl stretch)] due to the cold milk sample handling and mixing procedures used for TBC was detected, confirming the fact that the physical removal of milk from the vial by the BactoScan FC (Foss Electric, Hillerød, Denmark) was a representative portion of the milk. However, the representativeness of any other sampling procedure (manual or automated) of a cold milk sample before running milk component testing on the same container of milk should be demonstrated and verified periodically as a matter of routine laboratory quality assurance. Running TBC with a BactoScan FC first and then IR milk analysis after had a minimal effect on milk component tests by IR when milk bacteria counts

Determination of radium-226 in environmental samples

International Nuclear Information System (INIS)

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

1980-01-01

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

Selection of blood sampling times for determination of 51Cr-EDTA clearance in a screeening procedure

International Nuclear Information System (INIS)

Gullquist, R.; Askergren, A.; Brandt, R.; Silk, B.; Strandell, T.; Huddinge University Hospital

1983-01-01

In a group of 44 construction workers various blood sampling protocols were compared with regard to variability of the 51 Cr-EDTA clearance on repeated determinations. A comparison was also made among the different blood sampling protocols with a reference method using Simpson's formula in the area calculation. A double slope method lasting for two and a half hours was finally choosen and suggested as a screening procedure in industrial environment with blood sampling at 5, 15, 90, 120, 135 and 150 minutes after injection and with the patient resting in a semirecumbent position. (orig.) [de

Comparison of diagnostic efficacy between CLE, tissue sampling, and CLE combined with tissue sampling for undetermined pancreaticobiliary strictures: a meta-analysis.

Science.gov (United States)

Gao, Ya-Dong; Qu, Ya-Wei; Liu, Hai-Feng

2018-04-01

The accurate diagnosis of undetermined pancreaticobiliary strictures remains challenging. Current ERCP-guided tissue sampling methods are of low sensitivity. Confocal laser endomicroscopy (CLE) is a new procedure and allows real optical biopsies that may improve the diagnosis of undetermined pancreaticobiliary strictures. The aim of this meta-analysis was to determine the diagnostic yield of CLE, tissue sampling, and CLE combined with tissue sampling for undetermined pancreaticobiliary strictures. Pubmed, Embase, and the Cochrane Library database were reviewed for relevant studies. Pooled estimates of sensitivity and specificity with 95% confidence intervals (CIs) were calculated using the random-effects meta-analysis model. The summary receiver-operating characteristic (SROC) curve was constructed, and the area under the receiver operating characteristic curve (AUC) was calculated. Twelve studies involving 591 patients were enrolled in our analysis. The overall sensitivity and the specificity estimate of CLE for discriminating benign and malignant pancreaticobiliary strictures were 87% (95%CI, 83-91%) and 76% (95%CI, 70-81%), respectively. The AUC to assess the diagnostic efficacy was 0.8705. For tissue sampling, the overall sensitivity and the specificity estimate were 64% (95%CI, 57-70%) and 94% (95%CI, 90-97%), respectively. The AUC to assess the diagnostic efficacy was 0.8040. A combination of both methods increased the sensitivity (93%; 95%CI, 88-96%) with a specificity of 82% (95%CI, 74-89%). The AUC to assess the diagnostic efficacy was 0.9377. There was no publication bias by Deeks' Funnel Plot with p = .936. Compared with tissue sampling, CLE may increase the sensitivity for the diagnosis of malignant pancreaticobiliary strictures. A combination of both can effectively diagnose malignant pancreaticobiliary strictures.

ORNL: PWR-BDHT analysis procedure, a preliminary overview

International Nuclear Information System (INIS)

Cliff, S.B.

1978-01-01

The computer programs currently used in the analysis of the ORNL-PWR Blowdown Heat Transfer Separate-Effects Program are overviewed. The current linkages and relationships among the programs are given along with general comments about the future directions of some of these programs. The overview is strictly from the computer science point of view with only minimal information concerning the engineering aspects of the analysis procedure

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

A smart Monte Carlo procedure for production costing and uncertainty analysis

International Nuclear Information System (INIS)

Parker, C.; Stremel, J.

1996-01-01

Electric utilities using chronological production costing models to decide whether to buy or sell power over the next week or next few weeks need to determine potential profits or losses under a number of uncertainties. A large amount of money can be at stake--often $100,000 a day or more--and one party of the sale must always take on the risk. In the case of fixed price ($/MWh) contracts, the seller accepts the risk. In the case of cost plus contracts, the buyer must accept the risk. So, modeling uncertainty and understanding the risk accurately can improve the competitive edge of the user. This paper investigates an efficient procedure for representing risks and costs from capacity outages. Typically, production costing models use an algorithm based on some form of random number generator to select resources as available or on outage. These algorithms allow experiments to be repeated and gains and losses to be observed in a short time. The authors perform several experiments to examine the capability of three unit outage selection methods and measures their results. Specifically, a brute force Monte Carlo procedure, a Monte Carlo procedure with Latin Hypercube sampling, and a Smart Monte Carlo procedure with cost stratification and directed sampling are examined

Sieve-based device for MALDI sample preparation. I. Influence of sample deposition conditions in oligonucleotide analysis to achieve significant increases in both sensitivity and resolution.

Science.gov (United States)

Molin, Laura; Cristoni, Simone; Crotti, Sara; Bernardi, Luigi Rossi; Seraglia, Roberta; Traldi, Pietro

2008-11-01

Spraying of oligonucleotide-matrix solutions through a stainless steel (ss) sieve (38 microm, 450 mesh) leads to the formation, on the matrix-assisted laser desorption/ionization (MALDI) sample holder, of uniformly distributed microcrystals, well separated from each other. When the resulting sample holder surface is irradiated by laser, abundant molecular species form, with a clear increase in both intensity and resolution with respect to values obtained by 'Dried Droplet', 'Double Layer', and 'Sandwich' deposition methods. In addition, unlike the usual situation, the sample is perfectly homogeneous, and identical spectra are obtained by irradiating different areas. On one hand, the data indicate that this method is highly effective for oligonucleotide MALDI analysis, and on the other, that it can be validly employed for fully automated MALDI procedures.

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, ...